TI 980 TriboIndenter User Manual

TI 980 TriboIndenter User Manual• TI 980 TriboIndenter Base System• nanoDMA Option• 3D OmniProbe/MultiRange NanoProbe Option

Original Instructions

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This user manual as well as the software described in it, is furnished under license and may only be used or copied in

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TABLE OF CONTENTS

TI 980 TriboIndenter System ....................................................................................... 7General Hardware ........................................................................................... 9

System Requirements ........................................................................................................9X, Y, & Z-Axis Stages .........................................................................................................10

Sample Stage .............................................................................................................11Granite Frame ..................................................................................................................13Acoustic Enclosure ...........................................................................................................13Optical Camera System ....................................................................................................14Vibration Isolation System ...............................................................................................16

Active Vibration Isolation System .............................................................................16TriboScanner Piezo Scanner .............................................................................................18

Installing the TriboScanner .......................................................................................21Transducer Assembly .......................................................................................................23

Nanoindentation Probe Mounting ............................................................................26Installing the Transducer ..........................................................................................31

Hysitron Control Unit .......................................................................................................32Safety Considerations ...............................................................................................32Ventilation .................................................................................................................33Back Panel Overview .................................................................................................34Specifications ............................................................................................................35

Instrument Connections ...................................................................................................35Dual Low Load Transducer Compatibility .................................................................36

Data Acquisition Computer ..............................................................................................37Powering the Instrument On and Off ...............................................................................38Storage of Components ...................................................................................................39

General Software ........................................................................................... 41Action Bar .........................................................................................................................42

Zero Button & Transducer Status ..............................................................................43Workspace Pull-Down Menu ....................................................................................43System Progress Panel ..............................................................................................44Back & Forward Shortcut Buttons .............................................................................45Pause TriboScan Button ............................................................................................45Mode Pull-Down Menu .............................................................................................45Current Optic & Probe Indicator ...............................................................................46Emergency Stop Button ............................................................................................46

Sample Navigation Tab ....................................................................................................48Video .........................................................................................................................48Stage Controls ...........................................................................................................50Sample Boundaries ...................................................................................................52

Load Function Tab ............................................................................................................54Indentation Sub Tab ..................................................................................................55Load Function Generator ..........................................................................................62XPM Sub Tab .............................................................................................................66Scratch Sub Tab .........................................................................................................69ScanningWear Sub Tab .............................................................................................76

Analysis Tab ......................................................................................................................79Quasi Sub Tab ...........................................................................................................80XPM Sub Tab .............................................................................................................90Scratch Sub Tab .........................................................................................................92

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Image Sub Tab ...........................................................................................................95Plot Scaling .......................................................................................................................95Imaging Tab ......................................................................................................................97Automation Tab .............................................................................................................110

Methods Sub Tab ....................................................................................................111Piezo Automation Sub Tab ......................................................................................119

Calibration Tab ...............................................................................................................124System Calibrations Sub Tab ...................................................................................124Stage Calibration Sub Tab .......................................................................................129Tip Calibration Sub Tab ...........................................................................................132Machine Compliance Sub Tab .................................................................................133In-situ Sub Tab ........................................................................................................134Auto Calibration Sub Tab ........................................................................................135

Preferences Tab .............................................................................................................136Table Sub Tab ..........................................................................................................136Piezo Sub Tab ..........................................................................................................138

Hysitron Customer Support Site & The About Tab ........................................................140TI Series System Calibrations ................................................................................... 141

Calibrations ................................................................................................. 142Loading a Transducer Constants File ..............................................................................142Tare Value Verification ...................................................................................................144ADC Calibration ..............................................................................................................145Indentation Axis Calibration ...........................................................................................146

Performing the Indentation Axis Calibration ..........................................................147Lateral Axis Calibration ..................................................................................................151

Notes on Lateral Axis Range ...................................................................................153Transducer Breakpoint ............................................................................................153Imaging Position ......................................................................................................154Optimizing the Imaging Position Parameter ...........................................................154

Optical Zoom Calibration ...............................................................................................155XY Stage Move Limits Calibration ...................................................................................156Optic-Probe Tip Offset Calibration .................................................................................157

Automatic Optic-Probe Tip Offset Calibration ........................................................157Traditional Optic-Probe Tip Offset Calibration .......................................................162

TriboScanner Piezo Scanner Calibration ........................................................................167Probe Calibration ...........................................................................................................171

Procedure for Probe Calibration .............................................................................174Machine Compliance Calibration ...................................................................................181

Auto Calibration Sub Tab ............................................................................. 185TI Series Testing ...................................................................................................... 195

Testing ......................................................................................................... 196Testing Overview ............................................................................................................196Sample Mounting ...........................................................................................................197

Dual Head Mode .....................................................................................................198Creating Sample Boundaries ...................................................................................199Quick Approach .......................................................................................................202

Choosing a Test Type .....................................................................................................204Perform a Test From the Optical Focus ..........................................................................204Tuning Feedback Gains ..................................................................................................208Testing Troubleshooting ................................................................................................212

in-situ SPM Imaging Procedure .................................................................... 214Scanning Wear Testing ...................................................................................................215Testing From the in-situ Imaging Position ......................................................................217

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Piezo Automation Procedure ..................................................................................219Automated Method Testing ......................................................................... 224

Combi Utility ..................................................................................................................226TI Series Analysis ..................................................................................................... 231

Analysis ....................................................................................................... 232Single Indentation Test Analysis ....................................................................................232

Plot Multiple Curves ................................................................................................236Partial Unload Analysis ...........................................................................................237

XPM Accelerated Property Mapping Analysis ................................................................238Nanoscratch Analysis .....................................................................................................240

in-situ SPM Imaging Analysis ....................................................................... 2453D Plot Window .............................................................................................................251

nanoDMA ............................................................................................................... 257nanoDMA Hardware .................................................................................... 261

Instrument Connections .................................................................................................261Installation of Components .....................................................................................262Lock-In Amplifier Configuration ..............................................................................263

nanoDMA Operation ................................................................................... 264nanoDMA Calibrations ...................................................................................................265

Verify the Transducer Constants .............................................................................265Probe Area Function ...............................................................................................266Indentation Axis Calibration ....................................................................................266DDLA Lock-in Amplifier Calibration .........................................................................267Dynamic Calibration ................................................................................................268

nanoDMA III Testing .......................................................................................................271nanoDMA side tab ..................................................................................................273Dynamic (Frequency or Load) Sweep Generator window ......................................277

Dynamic Test Types ........................................................................................................280Variable Frequency .................................................................................................281Variable Load ..........................................................................................................282CMX .........................................................................................................................283Reference Creep .....................................................................................................286

nanoDMA Testing Suggestions .......................................................................................288nanoDMA Data Analysis .................................................................................................288

nanoDMA Data Analysis Details ..............................................................................294nanoDMA Data Analysis Procedure ........................................................................297

Modulus Mapping ..........................................................................................................299Acquisition Software ...............................................................................................300Analysis ...................................................................................................................304Testing Procedure ...................................................................................................304

xProbe Transducer .................................................................................................. 309xProbe Transducer ....................................................................................... 310

Probe ..............................................................................................................................310Hardware Installation .....................................................................................................311

xProbe Transducer Details ......................................................................................311xProbe Transducer Specifications ...........................................................................312

xProbe Transducer Operation ...................................................................... 313xProbe Transducer Calibrations .....................................................................................314

Verify the Transducer Constants .............................................................................314Transducer Indentation Axis Calibration .................................................................314Lateral Axis Calibration ...........................................................................................314Optic-Probe Tip Offset Calibration ..........................................................................314

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Probe Area Function ...............................................................................................315xProbe Transducer Testing & Analysis ...........................................................................315

Gain Settings ...........................................................................................................3153D OmniProbe/MultiRange NanoProbe .................................................................. 317

3D OmniProbe/MRNP Hardware ................................................................. 318Instrument Connections .................................................................................................319Hardware Installation .....................................................................................................321

3D OmniProbe/MRNP Nanoindentation Probe Mounting .....................................321Installing the 3D OmniProbe/MRNP Transducer Head ...........................................323

3D OmniProbe/MRNP Operation ................................................................. 3243D OmniProbe/MRNP Calibrations ................................................................................324

Verify the Transducer Constants .............................................................................325Tare Value Verification ............................................................................................3273D OmniProbe/MRNP Indentation Axis Calibration ...............................................328nanoDMA-HL Calibration ........................................................................................330

Sample Mounting ...........................................................................................................3303D OmniProbe/MultiRange NanoProbe Testing ............................................................331

XY Approach Offset .................................................................................................332System Test tab .......................................................................................................332Indentation Testing .................................................................................................333in-situ SPM Imaging ................................................................................................333Automated Testing Methods ..................................................................................334Indentation Analysis ................................................................................................334

Probe Cleaning Procedure & Selection Guide .......................................................... 337Cleaning Hysitron Probes ............................................................................. 338Probe Selection Guide .................................................................................. 340

Berkovich Probes ............................................................................................................34090 Degree Probes (Cube Corner) ...................................................................................342Cono-spherical Probes ...................................................................................................342

Imaging Cono-Spherical (radii < 10 µm) ..................................................................343Non-Imaging Cono-Spherical Probes (radii > 10 µm) ..............................................344

Specialty Probes .............................................................................................................344Vickers Probes .........................................................................................................344Knoop Probes ..........................................................................................................345Flat Ended Probes ...................................................................................................345Wedge Probes .........................................................................................................345Fluid Cell Probes ......................................................................................................345Temperature Control Stage Probes ........................................................................346nanoECR Probes ......................................................................................................346

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TI 980 TriboIndenter System

SECTION 1 TI 980 TRIBOINDENTER SYSTEM

• Hardware and system components for the TI 980 TriboIndenter system• Installation of common hardware components for the TI 980 TriboIndenter

system• Software overview for the TI 980 TriboIndenter

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Congratulations on your purchase of a Hysitron TI 980 TriboIndenter nanomechanical testing instrument. Hysitron

testing instruments, options and user support have been designed with the user in mind so you can be confident that

you are using the most technologically advanced, quality instrument with the highest level of user support available.

This user manual has been constructed to be accessible for any user experience level covering topics from the basics

of nanomechanical testing with a Hysitron system to the more advanced complex automation or analysis routines.

This user manual also contains the calibration procedures necessary for maintaining the precision and accuracy of the

instrument as well as instructions for performing testing and analysis.

In order to bring attention to important items that may cause damage to the equipment or information that may ease a

process, this user manual contains two icons that will be displayed in the margin near the relevant information.

! Danger, Warning, or Caution - Damage to instrument or persons possible.

Information - Suggestions to assist with instrument use.

Special attention should be given to any warning information presented in the user manual as damage to the

instrument or persons can result from improper use.

Your TI 980 TriboIndenter system is equipped with the latest TriboScan operational and analysis software from

Hysitron. TriboScan is organized into a tab, sub tab, and side tab structure to simplify the navigation process.

• Tabs, sub tabs, side tabs, and buttons are italicized• Menu options, directories, and filenames are bold

Following each step in a procedure is important to minimize the possibility of equipment damage and to obtain

quality data. For this reason, all procedures are numbered to distinguish procedures from general user manual

information.

If a problem or question should arise which is not addressed in this user manual, please contact the Hysitron service

department or your local service representative before proceeding.

Hysitron9625 West 76th StreetEden Prairie, MN [email protected]://support.hysitron.com

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CHAPTER 1 GENERAL HARDWARE

The hardware components used with Hysitron nanomechanical testing systems are fragile and should be handled with

extreme care. Because of the sensitivity associated with nanoresolution testing, it is necessary to ensure that the

hardware components are properly calibrated as discussed in this user manual.

Although this user manual will emphasize the importance of properly installing and calibrating the hardware

components, it is equally important that the equipment be properly handled and stored when not in use. Components

such as the transducer or piezo scanner should always be stored in the originally supplied case supported by the die

cut foam. Other components that were not supplied with a case are generally less sensitive and should be stored in a

low-humidity location where the components will not be subjected to any physical shock or excessive vibration.

This user manual will discuss the TI 980 TriboIndenter system (base) and two of the most common options for the

TI 980 TriboIndenter (nanoDMA and 3D OmniProbe/MultiRange NanoProbe). Because of the similar routines

between testing modes, this user manual is written in sections with each section covering topics specific to the

respective testing mode or option. Each option builds upon the TI 980 TriboIndenter base so the user must be familiar

with the base system before proceeding to the options. Other options (not discussed in this user manual) will be

supplied with an additional user manual.

! Perform all hardware installation procedures and calibrations required for your TI 980 TriboIndenter system as specified in the calibration section prior to operation.

It is also important to note that some features may be discussed in a section that may not be explicitly defined for your

TI 980 TriboIndenter system.

Auxiliary hardware components (monitor, light source, computer, etc...) should be powered according to their

manufacture's instructions.

1.1 SYSTEM REQUIREMENTSThe total weight of all components (excluding computer and monitor) is approximately 300 kg (660 lbs) for the

TI 980 TriboIndenter system. The total space required for the standard base and enclosure is 86 cm (34 in)

wide 80 cm (32 in) deep 170 cm (67 in) tall. The TI 980 system shall be installed with the rear of the system

against a wall to avoid access to the wiring and components located in back of the equipment. Access behind the

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equipment should only occur after lockout tagout procedures are performed. The equipment feet must be lowered at

permanent position to avoid run away from non-locking transportation casters.

A separate desk at least 1 m (40 in) 1 m (40 in) should be used for the computer station and auxiliary electronics.

Allowable floor vibration specifications are outlined in the Installation Site Guidelines, which is available from

Hysitron upon request. The room should be in a quiet region of a building, preferably on the ground floor. Locations

near objects such as air conditioning, noisy motors (vacuum pumps), elevator shafts, windows with direct sunlight,

air or heating ducts, fans, or other high voltage equipment should be avoided as these noise sources can adversely

affect the performance of the instrument.

The system will run on line voltage from 100 VAC to 240 VAC (50/60 Hz). 7.0 A maximum current, single phase.

The system should be operated at a temperature between 5˚C and 40˚C with a maximum relative humidity of 80% at

31˚C and 50% at 40˚C. The maximum altitude of operation is 2000 m

The system does not require any additional building connections. Some instruments are equipped with an air line

connection that is intended to supply the testing environment with an inert gas, however, this is optional based on the

users desired testing regime.

! Never attempt to connect the system to a voltage supply other than what the instrument has been designed to be used with.

Unsure if the location planned for the Hysitron instrument will be suitable? Contact a Hysitron service engineer to discuss your installation locations and help you select an ideal position.

1.2 X, Y, & Z-AXIS STAGESThe Hysitron TI 980 TriboIndenter instruments are equipped with an automated X, Y, and Z-axis staging system. The

automated stages are operated with the supplied stage control unit (located within the instrument electronics rack) and

are operated through the instrument computer system. The stage control unit contains the micro-stepping drives for

the X, Y, and Z-axis stage motors. There are three outputs and two inputs on the back panel of the stage control unit.

Outputs • X-axis stage control• Y-axis stage control• Z-axis stage control

Inputs • From computer serial port/USB port• Emergency stop signal from the Hysitron control unit

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The X and Y-axis of the TI 980 TriboIndenter system are encoded to a resolution of 100 nm (500 nm for systems

prior to 2013) to allow for precise, repeatable positioning of the nanoindentation probe. Because the X and Y-axis are

encoded, the stages can be moved manually with the knobs on each respective stage and the position displayed in the

TriboScan software will update. The Z-axis is not encoded and any manual movement of the Z-axis requires that the

stage be homed (through TriboScan commands) before continuing.

Table 1.A TI 980 TriboIndenter system

automated stage specifications

! There is an Emergency Stop button located on the front of the stage control unit. This button can be used to stop the stage movement if the user suspects the probe (or other component) will contact an item resulting in damage. Use of the Emergency Stop button causes a break in USB communication with the computer and will require the user to restart TriboScan. There is also a software emergency stop that will be discussed in the Action Bar section of the Software section of this user manual.

The TI 980 TriboIndenter system may be equipped with a Newport ESP 301 stage control unit or a Hysitron stage

control unit. Both control units operate identically with regard to software and testing routines.

The power button for the Newport ESP 301 stage control unit is located on the rear of the stage control unit near the AC power input.

1.2.1 SAMPLE STAGEThe default sample stage shipped with the Hysitron TI 980 TriboIndenter system uses magnetic attraction, clips, or

vacuum (house vacuum connection required) for securing samples. A strong neodymium magnet has been machined

TI 980 TriboIndenter

X and Y-Axis

Travel Distance 300 mm 150 mm

Microstepping Resolution 50 nm

Encoder Resolution 100 nm (500 nm piror to 2013)

Maximum Translation Speed 30 mm/sec

Z-Axis

Travel Distance 50 mm

Microstepping Resolution 3.1 nm

Maximum Translation Speed 2.0 mm/sec

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into the underside of the sample stage at each sample location (identified in Figure 1.1). There are also vacuum

channels machined in different sizes depending on sample size with a small hex plug screw in each channel that must

be removed before use and replaced when no longer in use. The sample stage is designed to bolt onto the X/Y axis

stage with the large thumb screw.

The TI 980 sample stage has two rectangular sample moutons that adhere to the stage with magnetic attraction and

are intended for the standard samples (to help with sample repeatability placement). Standard samples are included

unmounted and should be adhered with cyanoacrylate-based adhesive (super glue).

Figure 1.1 TI 980 TriboIndenter magnetic

sample stage

! When installing the stage, do not allow the stage to come into contact with transducer. This will cause serious damage to the transducer and/or scanner.

The magnetic sample stage uses very strong magnets to ensure that the steel SPM sample pucks are held securely. To prevent the sample from snapping to the stage, possibly breaking the bond between the SPM sample puck and the sample, it is recommended to set the sample on a corner of the stage (far from the magnets) and slide the sample into place.

Other options such as the temperature stage or nanoECR will hold samples differently. Some (typically non-standard)

probes may contain magnetic components and therefore cannot be used with the magnetic sample stage. For more

information on additional sample mounting options contact a Hysitron service engineer.

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1.3 GRANITE FRAMEHysitron instruments are built upon a carefully designed granite frame. A granite frame with a two-point bridge is

used for Hysitron instruments in order to:

• Supply a ridged skeleton for components to be built• Contribute to thermal stability of the instrument• Reduce environmental noise• Reduce resonant frequencies

The Z-axis stage is mounted on the granite bridge and the transducer of the instrument is secured to this stage with

specially designed brackets allowing for accurate placement in the Z-axis. The optical camera system is secured to

the Z-axis near the transducer to allow for accurate placement between the optical view and the testing location.

Figure 1.2 illustrates the granite frame (given in light grey) and the associated attached components of the system

(given in dark grey) for the TI 980 TriboIndenter system.

Figure 1.2 TI 980 TriboIndenter granite

frame

1.4 ACOUSTIC ENCLOSUREHysitron instruments are equipped with an acoustic enclosure designed to minimize the amount of acoustic noise,

block air currents and act as a thermal buffer to reduce drift. A front-facing door provides interior access while side

and front windows allow the user to view the position of the stages and transducer assembly to assist with coarse

positioning.

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Figure 1.3 TI 980 TriboIndenter acoustic

enclosure

In addition to the standard acoustic enclosures given in Figure 1.3 if the system is configured for nanoECR a copper

wire mesh material is embedded into the fiberglass to reduce the effects of electro-magnetic interference.

1.5 OPTICAL CAMERA SYSTEMThe top-down optical camera used with the TI 980 TriboIndenter systems is identified in red in Figure 1.4. The color

CCD camera is located in the middle of the Z-axis stage and interfaces with the computer through the USB 3.0 port.

There is a standard 20x (interchangeable) objective lens at the lower end, which sends the magnified image to the

camera resulting in an apparent magnification from 20x up to 220x (with the standard configuration). The all-digital

magnification is software controlled, which requires no moving parts or additional electronic control units and is

operated through the computer USB 3.0 port.

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Figure 1.4 TI 980 TriboIndenter USB 3.0

optical camera system

The TI 980 TriboIndenter optical camera system has several settings that are configured at the factory from the

National Instruments Measurement & Automation Explorer. This configuration software will be installed on the

TI 980 TriboIndenter system if any settings need future adjustment.

The optics assembly requires an external fiber optic illumination unit that is operated with a power and intensity

switch. The TI 980 TriboIndenter system is supplied with an LED unit that has no user-serviceable components.

The LED fiber optic illumination unit also has a finite lifespan. The lifespan of the unit can be increased by operating at lower intensity levels.

Within TriboScan, the user has the ability to zoom the optical camera system from 1x to 10x (as discussed in the

Software section of this user manual). The TriboScan zoom settings correspond to different actual magnification

values given in Table 1.B.

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Table 1.B TI 980 TriboIndenter IEEE 1394

CCD camera zoom specifications

1.6 VIBRATION ISOLATION SYSTEMDue to the sensitive nature of nanomechanical testing, all Hysitron systems are equipped with either a passive

(standard) or active (upgrade) vibration isolation system.

The specifications and tuning required for the vibration isolation system(s) is outlined in the following section(s).

1.6.1 ACTIVE VIBRATION ISOLATION SYSTEMThe active vibration isolation system used with Hysitron systems is the HerzanTM AVI-200 S/LP. The Herzan AVI-200

S/LP system consists of a control unit and two rails (Figure 1.5) that are located under each side of the granite base

inside the acoustic enclosure. Enclosed within each rail are four piezo-electric accelerometers that continuously sense

changes through an internal feedback loop. Four electro-dynamic transducers send offsetting or correcting forces to

damp the vibrations sensed by the accelerometers in the lower frequency ranges (0-200 Hz). At higher frequencies,

the mass of the granite base and the spring system in the rails passively damp vibrations.

TriboScan Zoom Setting

Camera Digital

Magnification

Fixed Optical Magnification (objective lens)

Total Magnification

Horizontal Size (μm)

Vertical Size (μm)

1 0.5x 20x 10x 626 548

2 0.7x 20x 14x 444 388

3 1.0x 20x 20x 316 278

4 1.4x 20x 28x 222 188

5 2.0x 20x 40x 156 136

6 2.8x 20x 56x 112 96

7 4.0x 20x 80x 76 66

8 5.6x 20x 112x 56 48

9 8.0x 20x 160x 40 32

10 11.0x 20x 220x 28 22

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Figure 1.5 Active vibration isolation control unit (left) and vibration isolation

units (right)

In order for the active vibration isolation system to operate properly, the control unit must be powered on and the

switch must be toggled to Enabled mode (a green AND orange LED will be illuminated). If the orange LED is

blinking, there has been a large jolt to the system that the isolation system was incapable of offsetting or the controller

has just been powered on. The orange light will blink for a few seconds while the system resets and then regains the

vibration isolation capabilities.

There are a set of red LED lights that will illuminate when a vibration has been sensed by the system and attempts are

made to isolate the vibration. If any of the red LED lights remain illuminated the vibration isolation system may need

to be reset or there may be an issue with the vibration isolation system.

More information regarding the Herzan AVI-200 S/LP active vibration isolation system can be found at: http://www.herzan.com/

Table 1.C Specifications of the active vibration isolation system

Frequency Range 1.0 - 200 Hz active; > 200 Hz passive

Transmissibility See plot in Figure 1.6

System noise < 50 ng per root Hz from 0.1 - 300 Hz

Static compliance 1.75 µm/N vertical; 3.5 µm/N horizontal

Correction forces 16 N vertical; 8 N Horizontal

Power requirements 90 - 250 VAC, 50-60 Hz, 9 W

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Figure 1.6 Transmissibility plot for Herzan

AVI-200 S/LP active vibration isolation system

1.7 TRIBOSCANNER PIEZO SCANNER

The TI 980 TriboIndenter will be supplied with two TriboScanner piezo scanners to allow for dual head operation (standard transducer). The TriboScanner piezo scanners are similar but will have different calibration files that must be loaded from the Calibration tab In-situ sub tab.

The TriboScanner piezo scanner is used by the TI 980 TriboIndenter system when operating in three-plate capacitive

indentation or dynamic mode (the TriboScanner piezo scanner is removed for MultiRange NanoProbe [MRNP] or

3D OmniProbe operation). The TriboScanner piezo scanner (Figure 1.7) is designed to provide fine scale positioning

of the nanoindentation probe before and after performing a test. The precision provided by the three-axis piezo

scanner is much higher than that of the X, Y, and Z-axis stage, which is why the final approach of the probe to the

sample is performed with the TriboScanner piezo scanner.

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Figure 1.7 TriboScanner

The TriboScanner piezo scanner is used for performing in-situ SPM imaging of the sample surface before and/or after

indentation or scratch tests are performed. This allows for very precise (+/-20 nm) positioning of the tests, as well as

post-test imaging to investigate qualitative and quantitative information about the test area. The in-situ images can be

used to determine failure modes (adhesion, cracking, pile-up, etc...) as well as determine sizes of deformation for

different types of analyses.

The TriboScanner piezo scanner is stationary during any nanoindentation or nanoscratch test. All actuation during a

test is performed with the transducer. All in-situ imaging and non-stage positioning offsets are performed with the

TriboScanner piezo scanner.

On the top of the TriboScanner piezo scanner are two 15-pin connectors and a lead with a 21-pin connector. The lead

with the 21-pin connector is used to connect the TriboScanner piezo scanner to the associated electronic control unit.

The 15-pin connectors are used to connect the transducer to the associated electronic control unit.

! The TriboScanner piezo scanner is an extremely delicate piece of equipment. Any blunt or shear force introduced to the interior piezo tube can cause extreme damage. The user must handle the scanner with extreme care.

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! During any transport of the TriboScanner piezo scanner, the transducer must be removed. Failure to do so can result in extreme damage. When not mounted to the instrument or for transport, store the TriboScanner in the originally supplied case.

! When removing the TriboScanner piezo scanner from the system, first remove the transducer, before unscrewing the three point contact dovetail mount. Be sure to only lay the scanner down on a flat surface with the large dovetail facing downward.

The TriboScanner allows for imaging of a sample and precise placement of tests through the use of a tandem

piezoelectric ceramic tube (Figure 1.8). Piezoelectric ceramics rapidly change shape when high voltages are applied.

The dimensions will increase in one direction and decrease in another while maintaining a constant volume. A tube

configuration is used due to its inherently rigid construction.

Figure 1.8 TriboScanner piezo ceramic tube

construction

The top half of the TriboScanner piezo scanner tube is composed of four separate quarter cylinders. Each quarter of

the tube controls motion in a different direction: +X, +Y, -X, and -Y. The bottom half of the TriboScanner piezo

scanner tube is constructed of a single piece of piezo ceramic. When each separate portion of the top half of the

TriboScanner piezo scanner tube is energized, the ceramic of that portion lengthens along the axis of the scanner

while the walls become thinner. This causes the tube to bend towards the side. When the lower tube is energized, it

lengthens to provide motion along the Z-axis. By manipulating the voltages sent to all five portions of the tube, 3D

motion can be achieved.

Ideally, the piezo ceramic should deform as a linear function of the voltage applied, however, in real-world

applications, piezo behavior is not ideal. With all piezo ceramic material there will be some amount of hysteresis and

creep. Hysteresis occurs when the mechanical response of the ceramic lags behind what is expected for the applied

voltage. Hysteretic effects will be magnified when the piezo is cycled through increasing and decreasing voltages.

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Creep is caused when the voltage to the piezo is suddenly and dramatically adjusted. The piezo continues to deform

slightly after the initial change. This often results in piezo overshoot and ring for a short period of time until the

desired deformation is achieved. Examples of ideal piezo ceramic behavior, hysteresis and creep are given in

Figure 1.9.

Figure 1.9 Ideal behavior, hysteresis, and

creep of piezo electric material

For more accurate placement of indentation tests, it is recommended, when possible, to perform tests from the in-situ SPM imaging position. Performing tests from imaging can be done quicker than tests performed from the optics position because the indentation probe is already on the sample. Additionally, performing tests from imaging will result in greater accuracy than performing tests from optical positions as the stage movements will be much smaller.

Table 1.D Specifications of the

TriboScanner

1.7.1 INSTALLING THE TRIBOSCANNERThe TriboScanner piezo scanner fits onto the Z-axis of the system using a dovetail attachment. The scanner is

installed from the top and slides down over a small pin that stops the scanner at the correct height. Gravity will hold

the scanner in place, however, before testing, the scanner must be tightened into place with the 1/16” hex screw

located on the side of the Z-axis stage (a 1/16” hex driver is included with all systems). The location of the hex screw

is highlighted with a [ ] symbol in Figure 1.10.

Please note, Figure 1.10 has removed the dovetail mount (shown in green) from the Z-axis of the system to better

illustrate the location of the locking hex screw, DO NOT remove the dovetail mount from the system under normal

conditions.

Maximum Z-Axis Range > 3 µm

Maximum X/Y-Axis Range > 60 µm

Piezo Scanner Type Tandem Tube

Operating Voltage -185 V to +185 V per electrode

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Figure 1.10 Installation of the TriboScanner

on a TI 980 TriboIndenter

Figure 1.10 shows a TI 980 TribOIndenter with a 3D OmniProbe transducer in slot 1 and a standard transducer with

TriboScanner piezo scanner in slot 2. The location of the 1/16” locking hex screw is identified in Figure 1.10. The

locking hex screw should only be loosened and not removed from the system.

With the scanner (or other transducer head) locked in place, it is electrically connected to the system through the

junction (located on the rear of the granite base). From the junction the piezo scanner cable passes on to the Hysitron

control unit in the instrument electronics rack.

The sockets on top of the TriboScanner are used to connect the transducer to the Hysitron control unit electronics.

The cable leading from the transducer plugs into the socket on the right. The cable from the Hysitron control unit

loops over the granite bridge and plugs in to the left socket. The two sockets are used as a pass-through and are

provided as a safety measure for the piezo scanner to prevent cable tension from damaging the system.

The transducer cables may be connected directly, but damage could occur to the scanner if it were removed with the transducer mounted and still connected.

Following the initial installation, the TriboScanner is rarely removed from the instrument. Reasons to remove the TriboScanner include: - If repair is required for a broken piezo scanner element

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- If a MRNP/3D OmniProbe is installed onto the system - If a temperature control stage heat shield is installed

! The piezo scanner is very fragile and can easily break from mishandling. Avoid applying any shock or unnecessary forces to the piezo ceramic material.

1.8 TRANSDUCER ASSEMBLYThe core of every Hysitron system is the patented three-plate capacitive force/displacement transducer developed by

Hysitron (Figure 1.11). The three-plate capacitive design provides high sensitivity, a large dynamic range and a linear

force or displacement output signal. The low mass (~200 mg) of the transducer center plate minimizes the

instrument's sensitivity to external vibrations, and allows for light load (less than 25 μN) nanoindentation tests to be

performed.

Figure 1.11 Standard 1D and 2D transducer

assemblies

The 1D (normal force only) transducer assembly consists of the force/displacement sensor, drive circuit board, and

hardware used to mount the transducer to the TriboScanner. The 2D (both normal and lateral force) transducer

assembly has the components of the three-plate capacitive 1D plus two additional transducer sensors mounted on

opposite sides of the first at a 90° angle. A cross-sectional schematic of the three-plate capacitive (1D) transducer

assembly shown in Figure 1.12.

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Figure 1.12 Cross sectional schematic of

standard (1D) transducer assembly

DISPLACEMENT MEASUREMENTThe center plate (with probe attached) can move between the outer plates. To determine the displacement a high

frequency oscillating voltage is applied across the outer plates. The voltage varies linearly between the outer plates

and the center plate will pick up this voltage. The voltage amplitude at the center plate is used to determine the

position between the outer plates. The drive circuit board within the transducer converts the voltage amplitude to a

DC signal called the Transducer Output Voltage. When the center plate is exactly in the center of the outer plate the

Transducer Output Voltage is zero, however, as the center plate moves towards the lower plate (as during an

indentation test) the Transducer Output Voltage becomes more negative (Figure 1.13). By measuring the voltage

amplitude and calibrating the relationship between the voltage amplitude and center plate position the displacement

during a test can be obtained.

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Figure 1.13 Transducer displacement

measurement diagram

FORCE MEASUREMENTThe force is applied to the transducer electrostatically. To apply a force, a large DC bias (up to 600 V) is applied to the

bottom plate of the capacitor (drive plate). This will create an electrostatic attraction between the center plate and the

bottom plate pulling the center plate down. The force can be calculated from the magnitude of the voltage applied

(based on the calibration of the transducer at the Hysitron factory).

Figure 1.14 Transducer force measurement

diagram

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More information regarding the transducer calibration values can be found in the Calibration section of this user

manual.

The maximum normal force available from the standard transducer is approximately 10 mN although models with

maximum normal load forces of approximately 30 mN are available.

Table 1.E Specifications of the Transducer

Assembly

1.8.1 NANOINDENTATION PROBE MOUNTINGMounting the Hysitron probe to the transducer is a very delicate process. Because of this, care should be taken not to

over tighten the probe or apply any s when mounting the probe. The procedure for mounting the probe is outlined

below.

! DO NOT power off the performech control unit (if TriboScan is running) when removing the transducer or scanner. Doing so will result in the DSP losing the USB connection and will require TriboScan to be restarted.

! It is recommended to Pause TriboScan (from the Action Bar) before adjusting or removing the piezo scanner or transducer.

Indentation Axis Lateral Axis

Maximum Force 10 mN or 30 mN 2 mN

Maximum Indentation Displacement 5 µm 500 nm

Maximum Lateral Displacement NA 15 µm

Thermal Drift < 0.05 nm/sec < 0.05 nm/sec

Load Noise Floor

performech/Digital Control 100 nN 3.5 µN

performech II 20 nN 3.5 µN

Load Resolution

performech/Digital Control 1 nN 3 µN

performech II 1 nN 50 nN

Displacement Resolution

performech/Digital Control 0.04 nm 4 nm

performech II 0.006 nm 0.02 nm

Displacement Noise Floor

performech/Digital Control 0.2 nm 2 nm

performech II 0.1 nm 2 nm

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Hysitron is willing to work with customers to provide custom nanoindentation probes to fit particular testing needs. Contact a Hysitron representative to discuss your testing needs or for information regarding stock and custom probe geometries.

1. If TriboScan is running, Pause TriboScan from the Action Bar before removing the transducer. DO NOT power off the Hysitron control unit. If TriboScan is not running, the Hysitron control unit should be powered off before remov-ing or installing the transducer.

2. If the transducer is currently installed in the instrument, remove the transducer from the TriboScanner by loosening (but not completely removing) the 0.035" hex screw with the supplied 0.035" torque hex driver (Figure 1.15).

Figure 1.15 Location of 0.035” hex screw

3. Place the transducer on its side.

Figure 1.16 Transducer ready for probe

installation

! Never place the transducer on a surface with the probe facing down. The probe will contact the surface resulting in a damaged transducer and/or probe. Always place the transducer on its side.

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! Never place the transducer in the storage container with a probe installed. Any contact with the probe when it is installed in the transducer will likely damage the transducer and/or probe.

4. Carefully remove the probe from its protective sheath holding the probe in the left hand if the user is right-handed (Figure 1.17).

Figure 1.17 Removing the nanoindentation

protective sheath

5. The probe inserts into the probe tool, point first (Figure 1.18). The probe tool should be held upright at all times. The probe is only held in the tool by gravity and friction so extra care should be exercised to prevent the probe from falling out of the tool.

Figure 1.18 Probe installation tool with

probe

Figure 1.19 Probe tool and probe geometry

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! Use caution when inserting the probe into the probe tool as any contact between the tip of the probe and the installation tool could chip or break the point.

6. Place the threaded end of the probe onto the threads of the transducer at a slight incline angle and then tilt the tool horizontally (perpendicular to the trans-ducer sensor) to prevent the probe from falling out of the tool (Figure 1.20).

Figure 1.20 Installation of nanoindentation

probe

7. Gently turn the probe counterclockwise until a slight click is felt when the lag of the threads fall into place. This is to avoid cross-threading the probe onto the sensor.

! Be careful not to cross-thread the probe on the transducer screw. The probe should turn easily. If the probe turns tightly, or becomes stuck, contact Hysitron customer service for advice to avoid damage to the probe or transducer.

! Lateral force Z-axis transducers are mounted between two X-axis transducers making them very delicate and more susceptible to forces applied by the user while installing the probe. Take extra care not to apply any lateral force on the indentation probe with lateral force transducers.

8. Gently turn the probe clockwise until the spring of the probe tool begins to deflect slightly. Stop turning when the probe tool begins to deflect, continu-ing to turn the probe tool after it has begun to deflect can cause damage to the transducer sensors.

9. Pull the probe tool straight away from the transducer taking extra care not to contact the tip of the probe with the tool.

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Figure 1.21 Removing the probe tool from the installed nanoindentation

probe

10. Follow steps 1 through 9 in reverse order to remove the probe from the trans-ducer.

After the nanoindentation probe has been mounted, the transducer can be installed onto the TriboScanner piezo

scanner (as outlined in the following section) via the dovetail mount and secured by tightening the 0.035" hex locking

screw on the transducer.

! Always perform the probe mounting procedure with the transducer laying on its side on a solid surface.

! Never allow the probe tool to hang freely from the transducer. The user should always support the mass of the tool or damage to the finely calibrated springs within the transducer may result.

To prevent damage to the probes, and keep the geometries easily organized while not being used, it is recommended

to always store the probes in the original protective sheath. It is also recommended to store the probes with the

original probe calibration sheet (Figure 1.22) that is supplied with each probe for future reference.

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Figure 1.22 Example probe calibration sheet

1.8.2 INSTALLING THE TRANSDUCERIf TriboScan is running, DO NOT power off the Hysitron control unit while removing or reinstalling the transducer.

With TriboScan running, the software should be Paused (suspended) to remove or adjust the transducer and then

Unpaused (resumed) when the transducer has been reinstalled. Powering off the Hysitron control unit may require a

restart of the TriboScan software.

Locate the 0.035” locking hex screw on the dovetail of the transducer. This locking hex screw on the side of the

transducer (Figure 1.15) must be loosened with the included 0.035" torque hex driver.

Figure 1.23 Location of 0.035” hex screw

With the locking hex screw loosened, the transducer easily slides onto the dovetail of the TriboScanner piezo scanner.

The cable leading out of the transducer should always be on the front side of the TriboScanner piezo scanner, and the

transducer should slide on the dovetail from left to right as looking from the front of the system. After the transducer

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has been positioned fully onto the dovetail, the 0.035" locking hex screw needs to be tightened using the torque hex

driver. Use of the torque screwdriver ensures that the locking hex screw is not over tightened.

The cable from the transducer connects into the top-right socket of the TriboScanner and the transducer electronics

cable coming from the back panel of the instrument connects into the top-left socket.

Installation of the TriboScanner, probe and transducer should always be performed in the following order: 1. Install the TriboScanner on the Z-axis of the Hysitron system 2. Install the nanoindentation probe onto the transducer 3. Install the transducer onto the TriboScanner Generally, under normal operation, the TriboScanner will rarely need to be removed from the system.

1.9 HYSITRON CONTROL UNITThe TI 980 TriboIndenter system utilizes the newest generation of DSP based Hysitron control unit available - the

performech II. For the purposes of this user manual the term Hysitron control unit will be used to encompass

performech II, performech, and digital control unit (control units used on other Hysitron TI series systems).

The TI 980 TriboIndenter system is equipped with a performech II. Software operation and analysis shares many similarities with the performech and digital control unit so for this user manual the term Hysitron control unit will be used to encompass control units used for all Hysitron TI series systems.

Figure 1.24 Hysitron performech II back

panel

1.9.1 SAFETY CONSIDERATIONSConnect an appropriate AC power cord to the AC input connection on the back of the Hysitron control unit and then

into an available grounded (earth grounded) power outlet. The Hysitron control unit accepts line voltages from

100 VAC to 240 VAC, 50/60 Hz, 1.9 Amp maximum, single phase. Do not position the equipment so that it is

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difficult to disconnect the AC power cord. When mounting in a rack and plugging into a rack power source be sure

the main rack power cord or power switch remains accessible for disconnection.

The Hysitron control unit uses two 250 V, 2.5 Amp, Type “T” (time lag) fuses located in the main power inlet. To

inspect or replace the fuses, disconnect the power cord from the back of the control unit and pull out the fuse tray.

! If the equipment is operated in a manner not specified by this user manual, the protection provided by the equipment may be impaired.

LOCK OUT TAG OUT (LOTO) PROCEDURE FOR THE TI 980 TRIBOINDENTERThe lock out tag out procedure is to turn off all system components and disconnect the power from the wall outlet.

With the components powered off and system disconnected from the wall outlet the power source can be locked out

or tagged out using the procedure of your facility. Access behind the equipment should only occur after lockout

tagout procedures are performed.

ELECTRONICS RACKThe performech II control unit must be mounted in the Hysitron supplied electronics rack.

! The performech II control unit must be mounted in the Hysitron supplied electronics rack.

1.9.2 VENTILATIONThe Hysitron control unit requires adequate ventilation to operate normally. There are two cooling fans located on the

rear of the Hysitron control unit and one small cooling fan for each DSP or DAQ board located within the Hysitron

control unit.

Excess heat is expelled out of the vents located on the top or front of the Hysitron control unit. Because of this, it is

important that no equipment is placed on top or in front of the Hysitron control unit that obstructs these vents. It is

also important that adequate space is given between the top or front of the control unit and other electronics.

If the vents of the Hysitron control unit are obstructed, as the heat builds up, the user may start to notice peculiar

operation of the software as the various power supplies begin to operate out of the normal range. Eventually, the

5 VDC power supply may fail, which powers all DSP and DAQ boards so instrument operation will terminate. If this

occurs, clear the obstructed vents, allow adequate time for the control unit to cool then attempt to restart the system.

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! Do not obstruct the vents on the top of the Hysitron control unit or the ventilation fans on the rear of the control unit. Obstructing these vents may cause the unit to overheat can cause damage to the internal components.

1.9.3 BACK PANEL OVERVIEWThe Hysitron control unit is designed to combine many external components into one easy-to-operate, computer

driven control unit. The Hysitron control unit is equipped with a number of input/output BNC connections that are

used for additional options/upgrades. Options and upgrades that utilize these auxiliary connections will be addressed

in the respective user manuals.

The Hysitron control unit includes two transducer connections (each with a 15-pin and a 25-pin connection).

TI 980 TriboIndenter systems should have the standard transducer for slot 1 connected to Transducer 1 Low Load

with the 15-pin connection and the standard transducer for slot 2 connected to Transducer 2 Low Load with the 15-

pin connection. The 25-pin connection is used only for TI 980 TriboIndenter systems with the 3D OmniProbe/MRNP

transducer and it will only be connected to Transducer 2 High Load (no Transducer 1 connection is active for the

3D OmniProbe/MRNP transducer). There is one orange LED near each of the transducer connections. When the

orange LED is illuminated high-voltage is being supplied to the transducer.

The instrument piezo scanner connects to the junction box within the enclosure and then out to the Piezo connector on

the Hysitron control unit.

The Emergency Stop BNC should be connected to the stage control unit being used with the TI 980 TriboIndenter

system.

There are five green LED lights on the rear of the Hysitron control unit. The five lights represent different voltages

being supplied by the internal power supply. All five green lights should be illuminated when the Hysitron control

unit is operational.

There are three red LED lights on the rear of the Hysitron control unit. The top red light is illuminated if no USB

connection is detected between the control unit and the computer. The bottom red light is an emergency stop

indicator. If the system is being used with an ESP 6000 stage control unit, a lit LED represents normal operation and

an unlit LED represents emergency stop. If the system is being used with an ESP 300/301 stage control unit, a lit LED

represents an emergency stop and an unlit LED represents normal operation.

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1.9.4 SPECIFICATIONSThe specifications for the Hysitron control unit are given in Table 1.F

Table 1.F Hysitron control unit

specifications

1.10 INSTRUMENT CONNECTIONSThe connections for a TI 980 TriboIndenter system are given in Figure 1.25. All components should be powered off

prior to connecting or disconnecting any cables.

Electrical Requirements

Voltage 100-240 VAC

Frequency 50/60 Hz

Current (all configurations) 1.9 Amp (max)

Fuses (two located at appliance inlet) 2.5 A, 250 V, Type “T”, 5x20 mm

Environmental Conditions (for safe operation of the Hysitron control unit)

Temperature 5˚C - 40˚C

Maximum Relative Humidity 80% at 31˚C, 50% at 40˚C

Altitude Up to 2000 m

Symbols Related to Safety

Warning: Disconnect power input before removing the cover.

Only qualified personnel should make adjustments to the instrument.

Caution: High voltage connection.

Ground: Indicates the terminal is connected to protective earth ground and chassis ground.

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Figure 1.25 performech II

TI 980 TriboIndenter connection diagram

1.10.1 DUAL LOW LOAD TRANSDUCER COMPATIBILITYThe TI 980 TriboIndenter system includes the dual low load transducer option. This option allows the user to have

two piezo scanners and two low load transducers installed on the system at the same time. If your system is equipped

with the dual low load transducer option there will be additional wiring and junctions inside the TI 980 TriboIndenter

enclosure as well as one additional connection from the performech II to the instrument back panel.

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Figure 1.26 performech II dual low load

option connection

1.11 DATA ACQUISITION COMPUTERHysitron instruments have been designed to be software controlled with the data acquisition computer supplied with

the instrument. A new Hysitron system data acquisition computer, as of the time this manual was written, will meet or

exceed the following specifications.

• Microsoft™ Windows® 10 Professional • Intel® i5 • 1 TB hard drive• 4 GB RAM• DVD-R/RW drive• Onboard LAN• 19” LCD flat panel monitor

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COMPUTER FEATURESA list of standard computer cards and features for the various Hysitron systems as well as cards required for

additional options is listed below

Table 1.G Computer requirements for

TI 980 TriboIndenter systems

Additional PCI cards may be required for systems running legacy stage control units, optical camera systems, or GPIB devices (lock-in amplifier, nanoECR SourceMeter, etc...).

Any computer cards, operating system requirements or hardware that is required for the system will be professionally

installed and tested for compatibility at Hysitron and should only be serviced by qualified Hysitron personnel. Future

options and upgrades may require additional computer cards or PCI expansion devices to accomodate quantity or size

of PCI cards.

1.12 POWERING THE INSTRUMENT ON AND OFFThere is no specific order for powering on the Hysitron control unit, computer or other auxiliary components.

All auxiliary electronics associated with the Hysitron system, including the Hysitron control unit MUST be powered

on prior to starting TriboScan to allow the hardware components to properly initialize.

When powering off the components, first close the TriboScan software then power off all auxiliary components

including the Hysitron control unit and computer.

Depending upon how the user intends to use the instrument, it can either be left on for extended periods of time or

shut down and restarted as needed.

Do not turn off the Hysitron control unit at any point without first shutting off the TriboScan software. Doing so will disrupt the DSP USB connection and the software will not be able reconnect without restarting TriboScan.

TI 980 TriboIndenter Systems

USB 2.0 Unlocked and accessible to all users

USB 3.0 Required

1280 x 1024 Screen Resolution Highly Recommended

Microsoft Windows Windows 10; 64 bit

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The optical camera system is supplied with a fiber optic light source that contains a high-power bulb. Powering this unit off during automated testing or when unneeded will extend the life of the bulb.

1.13 STORAGE OF COMPONENTSIt is important that the equipment be properly handled and stored when not in use. Many times it is safest and easiest

to leave the piezo scanner and transducer installed in the system between uses. However, when the piezo scanner and/

or transducer are removed they should always be stored in the originally supplied case supported by the die cut foam.

! Components should be stored separately. The nanoindentation probe should be removed from the transducer and the transducer should be removed from the piezo scanner before storing.

Probes should be stored in the original protective sheath within the original case and attached to the original probe

data sheet.

Other components that were not supplied with a case are generally less sensitive but should be handled with care. All

components should be stored in a low-humidity location away from excessive shock or vibration.

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General Software

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CHAPTER 2 GENERAL SOFTWARE

This chapter will cover the general operation (components common to all configurations) of the Hysitron system

including:

• Software operation common to all system configurations• Calibrations common to all system configurations• Indentation testing and analysis (a testing mode available on all Hysitron

systems)• Automated testing methods

Start TriboScan by selecting the TriboScan icon from the Windows desktop or by selecting the TriboScan.exe

program from C: Program Files Hysitron TriboScan. When TriboScan starts, if there are multiple features

available on the system, the user may be prompted with a Transducer Select window. If only one feature is installed

on the system TriboScan will auto-select the installed option.

For more information on the other features available for upgrade on your system contact your local Hysitron sales engineer.

Although TriboScan has been designed to be fully-automated and incorporate the data collection and analysis for

many of the available instrument upgrades and options there may be additional stand-alone software packages for

some options. Additionally, there may be communication port settings as well as other system settings that must be

entered or verified before the instrument or feature will operate normally.

In addition to the testing and analysis included with TriboScan, the following Hysitron programs are available from

within the TriboScan software suite (if equipped):

• TriboTC• TriboView• Modulus Mapping• TriboImage

This section of the user manual is intended as an overview for most software operations within the TriboScan

software. Additional calibrations, testing, or analysis routines can be found in the respective sections of this user

manual.

TriboScan, and any associated Hysitron software, is installed in the C: Program Files Hysitron directory or

C: Hysitron directory. Important files such as saved load functions, workspaces, and calibration files can all be

found within these directories.

Action Bar

To start the TriboScan software package, double click the TriboScan icon on the desktop or select the corresponding

choice from within the Start Menu Programs TriboScan. When the software is started the X, Y, and Z axis

stages will initialize and move to the home position. If various features are installed on the system, the software may

prompt the user regarding which mode he/she would like to run the software. After the initialization of the software is

complete, the Sample Navigation tab will be the active window.

TriboScan version 9 and higher is operated by tabs within the TriboScan software. The function of each of these tabs,

as well as an explanation of the available parameters and features, is given in this section. The tab scheme was created

as an intuitive filter method to allow the user to easily find complex features by starting from basic fields.

Problems starting TriboScan? Confirm that the all electronic components are powered on prior to starting TriboScan.

Before any testing is begun, the user must be comfortable with the material presented throughout this user manual. Procedures must be followed as outlined in this manual or at the instruction of a Hysitron representative to prevent instrument damage and obtain desirable testing results.

2.1 ACTION BARThe Action Bar contains many of the commonly used global features of the TriboScan software and displays the

system status and current testing mode. The Action Bar contains:

• Zero button and transducer status parameters• Workspace pull-down menu• System Progress panel (only visible while testing)• Back & Forward shortcut buttons• Pause TriboScan button• Mode pull-down menu• Current optics and probe indicator• Emergency Stop button

Figure 2.1 TriboScan Action Bar

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Action Bar

2.1.1 ZERO BUTTON & TRANSDUCER STATUS The Hysitron DSP-based control unit monitors and displays the transducer status at all times. For TI series systems,

the transducer status parameters are given only for user information and are completely software controlled requiring

no user interaction. There are four transducer status parameters and one Zero button given on the Action Bar:

Z Displacement (nm) The Z Displacement status parameter displays the current displacement of the nanoindentation probe in the indentation axis direction. The Z Displacement status parameter will automatically be zeroed by the software prior to performing any test. However, the user can zero this value at anytime by selecting the Zero button.

X Displacement (μm) The X Displacement status parameter displays the current displacement of the nanoindentation probe in the lateral axis direction. The X Displacement status parameter is automatically zeroed during the Lateral Axis Calibration and is not affected by the Zero button.

The X Displacement status parameter will only be displayed after the system has been toggled to Scratch mode and then will remain visible until the software is restarted.

Actuation (μN) The Actuation status parameter displays the current measured force being applied by the transducer indentation axis. This measured force includes any bias that is applied to the transducer. The Actuation status parameter is not affected by the Zero button.

Sample (μN) The Sample status parameter displays the current indentation axis force being applied by the system to a sample for performing an in-situ image or a nanoindentation test. The Sample status parameter is automatically zeroed by the software prior to performing a test or approaching a surface. However, the user can zero this value at anytime by selecting the Zero button.

Zero Button The Zero button can be used to bring the Z Displacement and Sample parameters to the zero position. For TI series systems, use of this button is unnecessary as the software will automatically zero the proper parameters prior to approaching a sample for imaging or testing.

2.1.2 WORKSPACE PULL-DOWN MENUDuring regular TriboScan operation, the majority of the user defined software settings are saved in a Workspace. A

Workspace is a software-created preference folder that contains settings, sample safety zones, automated method

routines, data, in-situ image files, etc... A saved Workspace can be reopened at any time to recall saved testing

parameters which helps to increase instrument productivity.

The Workspace pull-down menu is accessed from the TriboScan Action Bar by clicking the small down facing arrow

[ ] in the upper left corner:

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Action Bar

Open Workspace… The Open Workspace... menu item opens an existing workspace for the user to work within or modify.

Save Workspace The Save Workspace menu saves the current workspace.

Save Workspace as… The Save Workspace as... saves the current workspace under a new name.

New Workspace The New Workspace menu starts a new workspace for the user to save parameters, sample safety zones, automated method routines, position groups, patterns, data, etc…

Delete Workspace The Delete Workspace menu item opens a window that allows the user to delete old workspace files. The currently open workspace cannot be deleted.

Saving the workspace is required prior to starting an automated testing method, however, it is a good practice to save the workspace after adding/removing samples or making other modifications to the workspace. In the event of a power failure or software crash, the saved workspace can be loaded and the samples boundaries will not need to be recreated.

The Last Contact Height parameters are cleared any time the software is restarted or a workspace is re-opened. A quick approach must be performed on all samples that will be tested after opening a pre-saved workspace.

2.1.3 SYSTEM PROGRESS PANELThe System Progress Panel button (Figure 2.2) is only visible when a test is being performed, the system is

performing an in-situ image, or an automated method. The System Progress Panel button is intended to alert the user

that the system is working and, although different tabs or windows can be accessed, the system will be limited in its

current ability until the activity has finished.

Figure 2.2 System Progress Panel

Clicking on the System Progress Panel button (when available) will bring TriboScan back to the active tab or

progress window.

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Action Bar

2.1.4 BACK & FORWARD SHORTCUT BUTTONSThe Back and Forward shortcut buttons operate similar to many of today’s popular internet browsers. The Back and

Forward shortcut buttons are intended to allow the user to easily navigate common and frequently used tabs by

allowing simple, chronological navigation.

2.1.5 PAUSE TRIBOSCAN BUTTONWhen TriboScan is active, it utilizes a considerable amount of computer resources. If other programs are launched or

used while TriboScan is active, they may perform very slowly, with adverse effects, or not at all. Although it is not

encouraged, there will be times when other programs need to be operated alongside TriboScan.

To increase the performance of other programs, it is possible to temporarily suspend or Pause TriboScan. When

TriboScan is paused, all background TriboScan processes are suspended, and other computer programs can operate as

normal. TriboScan can be suspended by clicking the red hand button on the Action Bar. The Pause TriboScan feature

will not function while performing an in-situ image, performing a test, running an automated method or the automatic

stages are in motion.

Pausing TriboScan removes the high voltage power applied to the transducer and piezo scanner. Because of this, it is

required to use the Pause TriboScan feature whenever the transducer or piezo scanner will be removed from the

system or adjusted while TriboScan is running.

Pausing the TriboScan software whenever it is not in use will greatly increase the performance of the computer causing auxiliary programs to run much more smoothly and efficiently.

2.1.6 MODE PULL-DOWN MENUThe Mode pull-down menu determines what type of test the system is capable of performing at any given time.

Depending upon how the instrument is licensed there will always be the option for Indentation and Scratch and there

may be the option for nanoDMA [for instruments equipped with nanoDMA II], Modulus Mapping [for instruments

equipped with nanoDMA III and Modulus Mapping], nanoECR, etc...

Even systems without a lateral force transducer will have the ability to select the Scratch mode. However, no nanoscratch testing can be performed without the proper hardware.

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Action Bar

When performing a test while in-situ imaging a sample surface the Mode can not be changed (the probe must first be

withdrawn). Only the test type defined in the Mode pull-down menu can be performed while imaging the sample.

2.1.7 CURRENT OPTIC & PROBE INDICATORIt is important for the user to always know where the probe and optical camera are located with respect to the sample

locations. The Current Optic and Probe Indicator on the Action Bar represents the current X/Y axis location of the

probe and optics at any given time. As the X/Y axis is maneuvered around the Current Optic and Probe Indicator will

update to represent which samples are beneath the respective components. The Current Optic and Probe Indicator is

not related to the Z axis height of the samples and will only register X/Y axis sample locations.

2.1.8 EMERGENCY STOP BUTTONHysitron systems with automated stages are equipped with an emergency stop feature. There is a hardware

emergency stop located on the stage control unit in the electronics rack. Activating the hardware emergency stop will

cause a hard-stop of the stage motors and will require the software be restarted for the stages to be re-initialized.

The software emergency stop is located at the far right of the Action Bar in TriboScan. Clicking the Emergency Stop

button will halt all motion in the X, Y, and Z axis. When the software emergency stop is activated (depressed), a

button labeled Enable Motors will appear over the top of the Emergency Stop button. The motors must be enabled by

selecting the Enable Motors button before the user can continue to operate the software. If the user initiated the

emergency stop by clicking the Emergency Stop button, the stages can be re-enabled and there is no need to re-home

the Z axis.

The Emergency Stop will also be generated if an excessive force is applied to the nanoindentation probe. If an

unexpected, excessive force is applied to the nanoindentation probe (such as a probe crash into an incorrectly defined

sample space) an Emergency Stop will be generated by the software and the following procedure should be followed:

1. FOLLOW THE ON SCREEN DIRECTIONS. The directions given on the software pop-up are very thorough and will guide the user through the steps required to correct the issue.

2. Open the enclosure front access door and turn the yellow knob on top of the Z axis (labeled UP ß UP ß UP…) in the UP direction (clockwise as viewed from above) until the probe is visibly clear of the crash site.

3. Click the Enable Motors button that has appeared over the Emergency Stop but-ton.

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Action Bar

4. Home the Z axis (Calibration tab Stage Calibration sub tab Setup Home Z Axis).

5. Continue testing.

If the software generated Emergency Stop continues, the sample boundary may have been created out of focus. This

will cause the system to assume the wrong approach height for the sample and thus cause a probe crash. Another

common cause for the generation of an Emergency Stop is when the user attempts a quick approach without first

completing an Optics-Probe Tip Offset Calibration for the current optics/transducer/probe assembly.

! The emergency stop will only activate for excessive force being applied to the nanoindentation probe. Forces applied to the transducer housing or TriboScanner are not detected and will cause serious damage. Take special care to ensure samples are spaced far enough apart and that the transducer housing and TriboScanner do not contact any foreign object.

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Sample Navigation Tab

2.2 SAMPLE NAVIGATION TABThe primary tab (and default open tab upon startup) of the TriboScan software package is the Sample Navigation tab.

The Sample Navigation tab consists of three main areas:

• Video• Sample Boundaries• Stage Controls

Figure 2.3 Sample Navigation tab

2.2.1 VIDEOThe current optic view will be displayed in the Video area of the Sample Navigation tab. The dimensions of the X and

Y axis area displayed within the Video area are given above the optical image. The optical camera system is

calibrated to allow users to left-click and drag a measuring line that displays segment length and angle from +X axis

(given in the lower left of the Video area). The user may also right-click on a feature of interest and the X and Y axis

stages will move the area of interest in the center of the video window (following the necessary optical and stage

calibrations discussed later in this user manual).

The automated right-click stage moves uses the speed (as currently selected with the black cursor) in the Stage Controls area. If the cursor is located entirely along either the X or Y axis the opposite axis will not be active and the stages may not properly move or produce a Set Speeds = 0 error.

There are two check-boxes in the video area:

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Reticle (cross-hair) The Reticle check-box will toggle on and off the blue indicator lines showing the center point and the distance.

Scale Bar The Scale Bar check-box will toggle on and off the green scale bar in the lower left of the image. The scale bar dimensions will change as the zoom factor is changed.

There is one pull-down menu in the video area:

Zoom Factor The zoom factor value represents an arbitrary magnification of the video signal. The video signal is first sent through a standard 10x or 20x objective lens and then further magnified by the digital zoom which operates from 0.5x up to 11x for Zoom Factorsettings from 1x up to 10x, respectively. This results in an actual magnification of 5x/10x up to 110x/220x with software Zoom Factor settings of 1x up to 10x, respectively.

There are two buttons in the video area:

Save Optical Image The Save Optical Image button will save the current video view as a *.jpg image.

The video controls exclusively for the TI series IEEE 1394 color camera are given below the Video area by selecting

the Adjust Optics button:

Red, Green and Blue Level

The red, green and blue levels are used by the IEEE 1394 color camera (using the additive color model) to produce a full-spectrum of colors for the sample. The red, green and blue levels are typically set from the National Instruments Measurement and Automation Explorer. However, further adjustments can be made within TriboScan to achieve the best possible images for any given sample.

The contrast of the image can also be adjusted by using the manual Light Intensity knob located on the fiber optic light source.

Interpolation Interpolation is an estimation routine used by the digital top-down optics systems (typically at higher magnifications) to create a cleaner, more desirable image. The Interpolation pull-down menu offers three options:

• Zero Order (no interpolation)• Bilinear (default setting; averages nearest pixel left, right, up and down)• Quadratic (averages nearest two pixels left, right, up and down)

Other settings are available within the Adjust Optics button and are normally set within the National Instruments

Measurement & Automation Explorer (and will not typically require any adjustment within TriboScan):

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• Auto Exposure• Brightness• Gain• Gamma• Shutter Speed• Sharpness• Hue• Saturation• White Balance UB• White Balance VR

2.2.2 STAGE CONTROLSThe Stage Controls area allows the user to move the X, Y, and Z axis. The Stage Controls area allows for control of

the stage by clicking the move pad. Predefined movement can also be entered in the boxes below the move pad.

MOVING THE STAGESWhen moving the stages, the user can choose from four user-definable speed ranges Coarse, Medium, Fine, and Ultra

Fine. The speed and direction is selected by clicking a location in the move pad. The speed of the move increases as

the clicking location moves toward the outside of the move pad. The direction of the stage movement increases and

decreases as the clicking location moves closer to and further from the corresponding axis.

Figure 2.4 Move pad with color

enhancement to illustrate stage speeds

The directions listed in the Stage Controls area correspond to the following:

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+X Moves the field of view in the optics to the right, or the sample to the left

-X Moves the field of view in the optics to the left, or the sample to the right

+Y Moves the field of view in the optics backward, or the sample forward

-Y Moves the field of view in the optics forward, or the sample backward

+Z Moves the Z stage (including probe and optics) down, or closer to the stage

-Z Moves the Z stage (including probe and optics) up, or away from the stage

NANOINDENTATION PROBE POSITIONThe Nanoindentation Probe Position is given in the lower left portion of the Stage Controls area. The

Nanoindentation Probe Position records and displays the position of the probe at any given time. The user may click

on the move pad to move the stage or, alternatively, the user can enter a value in the probe position boxes and click

the Move button. The toggle to move either relative to the probe or as an absolute position is to the right of the listed

indenter position.

Figure 2.5 Nanoindentation Probe Position

If the user chooses to enter a value and click the Move button, attention should be given to the units used for moving the stages (given in the pull-down menu) to ensure the proper stage moves are being performed.

X-Y AND Z SAFETY RADIO BUTTONSThe X-Y and Z Safety is a feature built into Hysitron systems with automated stages to help prevent the likelihood of

crashing the nanoindentation probe into a defined sample surface. When a sample is defined within the TriboScan

software, the height of the sample and the height necessary for the transducer to clear the given sample (Z axis safety

height) is recorded. If the nanoindentation probe is lower than the software determined safety height and the safety is

active the software will not allow any movement in the X/Y plane.

• GREY circle next to X/Y and Z Safety DISABLED indicates safety is ON • RED circle next to X/Y and Z safety DISABLED indicates safety is OFF

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In some cases, the user will be required to deactivate the X/Y and Z Safety when creating sample boundaries (to allow

for X/Y-axis movement below the defined Z-axis safety height) and all other times the X/Y and Z Safety should be

grey (active).

! The X/Y and Z Safety will only work on a workspace with defined sample spaces. Any undefined sample installed in the system is very dangerous and can cause damage to the transducer and piezo scanner.

STAGE POSITIONSThe Stage Positions is located on the right side of the Stage Controls area and displays an overview of the stage. After

samples have been created the stage will be updated to show an outline of the current sample spaces in blue. The

optics is represented by a pink circle and the nanoindentation probe is represented by a green diamond. Right clicking

anywhere on the stage positions window will take the optics to that position. Right clicking outside of a defined

sample safety zone will move the Z-axis to the Z fly height (tallest sample safety height). Clicking outside of the

defined sample safety zones is not recommended.

Figure 2.6 Stage positions area

2.2.3 SAMPLE BOUNDARIESThe Sample Boundaries area is used to create, edit and remove sample areas. Before any automated stage moves

occur in the X and Y axis, the Z axis must first move to the Z Fly Height (by default, defined as 4 mm above the

tallest defined sample). This will minimize the likelihood of the probe crashing into a sample.

If the tallest sample is much taller than the other samples on the stage, it may be useful to remove the sample from

both the instrument and from the software if testing will not be performed on the sample. The current value for the

Z Fly Height is given in the Sample Boundaries area of the Sample Navigation tab. A diagram of the parameters given

in the Sample Boundaries area including the Z Fly Height is given in Figure 2.7

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Figure 2.7 Sample Boundaries parameters

The process for creating a sample boundary will be discussed in the Testing section of this user manual.

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Load Function Tab

2.3 LOAD FUNCTION TABThe Load Function tab contains the tools necessary for creating or editing the nanomechanical tests that will be run

by the instrument. Depending on the options and upgrades the instrument has been equipped with, additional sub tabs

may be available from the Load Function tab, each of which would be discussed in the option or upgrade respective

user manual.

The Load Function tab contains the following sub tabs:

Indentation The Indentation sub tab (Figure 2.8) is used to create nanoindentation load functions. The Indentation sub tab is standard on all instruments.

XPM The XPM sub tab is used to create XPM (accelerated property mapping) load functions. The XPM testing routine is an option upgrade available on any system using a performech II.

Scratch The Scratch sub tab is used to create nanoscratch load functions. The Scratch sub tab is standard on all instruments, however, lateral force (2D) transducer hardware is required for use.

Scanning Wear The Scanning Wear sub tab is used to create Scanning Wear load functions. The Scanning Wear sub tab is standard on all TI-series systems.

nanoDMA The nanoDMA sub tab is used to create nanoDMA II load functions. The nanoDMA sub tab is optional and will be available only on instruments that are equipped with nanoDMA II. nanoDMA III uses a side tab on the Indentation sub tab and the nanoDMA sub tab will not be available for nanoDMA III systems.

Temperature Control The Temperature Control sub tab is used to access the TriboTC program and configure the Hysitron temperature control stage (if equipped). The Temperature Control sub tab is optional and will be available only on instruments equipped with a temperature control stage.

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Figure 2.8 Indentation sub tab

2.3.1 INDENTATION SUB TABThe nanoindentation load function editor (accessed from Load Function tab Indentation sub tab) is used to create

all three-plate capacitive nanoindentation tests. The load function can be saved at any time by clicking File Save.

Likewise, a previously saved load function can be opened by clicking File Open. TriboScan is pre-loaded with

some basic load functions located at C: Program Files Hysitron TriboScan Load Functions.

Save time by modifying pre-made load functions to meet your testing needs. TriboScan comes loaded with several standard nanoindentation load functions. Open any of these load functions and modify the segment times, loads and number of segments instead of creating load functions from a blank window.

STANDARD LOAD FUNCTION MENUThe Standard Load Function menu (Figure 2.9) allows easy access to some of the most commonly used load

functions including a basic nanoindentation trapezoid (load segment, hold segment, and unload segment) test.

The Standard Load Function menu is only intended as a shortcut to some of the most commonly used load functions. Users can continue to create, edit, or modify load functions as discussed in later sections of this user manual.

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Load Function Tab

Figure 2.9 Standard Load Function menu

USER MODE MENUThe User Mode menu (Figure 2.10) is intended as a way to simplify the creation, editing, or modifying of the load

function.

When the User Mode is set to Standard the user will have a limited amount of parameters to modify (the most

commonly tuned parameters), which should simplify the load function creation, editing, and modification process.

The Advanced mode will give the user access to all parameters and can be more complicated for users who are

unfamiliar with the capabilities of the nanoindentation system. This user manual is written while in Advanced mode

so all parameters will be discussed.

Figure 2.10 User Mode menu

This user manual is written with the User Mode set to Advanced so that all parameters will be discussed. If parameters discussed in this user manual are not present in the instrument software the user should verify the User Mode is set to Advanced.

AUTOMATIC SAVE MENU

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The Automatic Save menu item allows the user to define a path and base file name for the tests that will be performed.

With the Automatic Save feature activated (with a check, similar to Figure 2.11) when a test has been performed it

will automatically be saved to the given directory with the given base file name and a test number (i.e., test_000,

test_001, test_002, etc...). This feature prevents the user from having to name each individual file following a test and

will speed the individual test process.

Figure 2.11 Automatic Save menu

The normal force vs. time plot will be updated after any change has been made in the parameters below the load

function plot. When a segment is selected by a single left-click, the segment will turn red and the parameters below

the plot will adjust to reflect the properties of that particular segment.

If the system is equipped with and being operated in Dual Head mode, the created load function will be saved and performed as whichever Transducer Slot (low load [three-plate capacitive] or high load [MRNP/3D OmniProbe]) is selected.

There are several buttons on the Indentation sub tab as shown in Figure 2.8. These buttons are the same for open-loop

and feedback control testing. The buttons are described below:

Add Segment Clicking the Add Segment button will add a ten second, constant load or displacement segment immediately to the right of the currently selected segment. The user can select a segment by clicking on the segment in the normal force or displacement vs. time plot.

Remove Segment Clicking the Remove Segment button will remove the currently selected segment. The first and last segment of a load function can not be removed. There must always be, at minimum, two segments and the beginning and ending force for the entire function must be 0.0 μN. The software will not allow the user to remove a segment that violates these rules.

Graph to Clipboard Clicking the Graph to Clipboard button copies the currently displayed normal force or displacement vs. time plot to the computer clipboard so that it may be pasted into any other available program.

Load Func. Gen. Clicking the Load Func. Gen. button will launch the load function creator software which allows the user to create complex partial unload functions. The Load Function Generator is discussed in the following Load Function Generator section.

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Load Function Tab

Air Indent Clicking the Air Indent button will perform the defined load function at the current position in the air (if the system is not in contact with a sample surface). The Air Indent button is disabled when the probe is in contact with a sample.

Perform Indent Clicking the Perform Indent button will perform the defined load function at the position centered in the Video area of the Sample Navigation tab or at the center of the current in-situ imaging area (if the probe is in contact with the sample surface). This position must lie within a defined sample safety zone.

Tune Displ. PID (displacement control only) The Tune Displ. PID button opens the PID Tuningwindow that allows the user to adjust the proportional, integral, and derivative gains while viewing a real-time step-response function of the transducer.

In the lower center section of the Indentation sub tab there is a Control Feedback pull-down menu. The user can

select different feedback controlled options from this pull-down menu shown in Figure 2.12. Open Loop (no fb),

Load, and Displacement control testing are standard on all systems. Because of the numerous similarities between the

testing modes, all three test types will be discussed in the following sections togeter.

Figure 2.12 Control Feedback pull-down

menu

By selecting the different types of nanoindentation tests from the Control Feedback pull-down menu (Open Loop,

Load, or Displacement control) the load function parameters will change. A description of the load function

parameters follows:

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Load Function Tab

Figure 2.13 Control Feedback parameters

Proportional Gain (displacement control only) Displacement control tests are inherently more difficult in forcing the test results to follow the desired testing load function. The Proportional Gain looks at where the actual result is in relation to the desired result at any given time (present error). Increasing the Proportional Gain may result in a quicker response but increased too much may cause oscillations. Default value is 1.00.

Integral Gain (load and displacement control only) This field allows the user to define the Integral Gain. This gain has the biggest effect on how well the test follows the load function. The Integral Gain looks at where the actual result was in relation to the desired result (past error) and uses this information to make corrections and bring the actual result closer to the desired result. Increasing the Integral Gain forces the actual result to follow the desired result more closely, however, too much Integral Gain may cause instabilities in the system and too little will result in a sluggish response time. Default value is 0.20 for load control and 1.00 for displacement control both load and displacement control testing.

Derivative Gain (displacement control only) Displacement control tests are inherently more difficult in forcing the test results to follow the desired testing load function. The Derivative Gain looks at where the actual result is going to be in relation to the desired result at any given time (prediction of future error based on current rate of change). The Derivative Gain works to limit the amount of overshoot; however, increasing the Derivative Gain by too much may result in a slower response. Default value is 0.00.

Adaptive Gain (displacement control only) Displacement control tests are inherently more difficult in forcing the test results to follow the desired testing load function. The Adaptive

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Load Function Tab

Gain is a feed-forward control that can quickly adapt to changes in the test to regain stability. Decreasing the Adaptive Gain may result in a slower response for complex load functions and an increased Adaptive Gain may will force complex load functions to follow the desired result more closely. Default value is 0.50.

Figure 2.14 Illustration of PID gain operation

Begin Force/Begin Disp.

The Begin Force or Begin Displacement field is used to enter the force or displacement for the selected segment to begin. The software will require that the user define the same value as the ending force or displacement for the previous segment (or zero for the first segment of the load function).

End Force/End Disp. The End Force or End Displacement field is used to enter the force or displacement for the selected segment to end. The software will require that the user define the same value as the beginning force or displacement for the following segment (or zero for the last segment of the load function).

Segment Time The Segment Time field allows the user to define a length of time for the selected segment. The loading rate will be automatically calculated.

Loading Rate The Loading Rate field allows the user to define a loading rate for the selected segment. The segment time will automatically be calculated.

Begin Time The Begin Time is the time that the selected load function segment will begin. This field is automatically populated and cannot be edited.

End Time The End Time is the time that the selected load function segment will end. This field is automatically populated and cannot be edited.

# to Average The # to Average field allows the user to define how to average the collected data. One corresponds to no averaging (raw data). Two corresponds to every two data points being averaged, yielding less data but a smoother plot, and so on.

# of Segments The # of Segments displays the number of segments for the open load function. This field is automatically populated and cannot be edited.

Data Points The Data Points parameter displays the number of data points that will be collected during the currently selected load function segment. The Data Points is calculated based on the defined Data Acq. Rate and the time for the selected load function segment.

Data Acq. Rate The Data Acq. Rate parameter allows the user to define how many data points to collect per second for the duration of the test. The default value is 200 pts/sec.

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Total Number of Points

The Total Number of Points parameter displays the number of data points that will be collected for the entire test. This is calculated based on the Data Acq. Rate and the total test time.

Last Drift Rate The measured Drift Rate for the most recently performed test is automatically entered into this field. This parameter is for user information only and is not editable by the user.

Peak Force/Peak Displacement

The Peak Force or Peak Displacement field is used to enter the load function maximum force (open loop or load controlled test) or displacement (displacement controlled test) for the entire load function.

Pre-Load The Pre-Load field allows the user to define a load for the probe to hold while the system pauses to allow the piezo scanner to settle and the system drift to be measured. This value is typically set to be similar to the in-situ imaging setpoint value. The default value is 2.0 μN.

Use Imaging Setpoint The Use Imaging Setpoint will automatically use the same value for the Pre-Load as is currently used on the in-situ SPM imaging tab Setpoint value.

Lift Height (load and displacement control only) The Lift Height parameter allows the user define a height for the probe to lift off the sample following the drift correction and then start the test in the air above the sample surface. The Lift Height is usually used to ensure that the probe has not sunken into the sample surface during the drift correction and the test starts at the sample surface. The default value is 25 nm.

Approach Offset (load and displacement control only) The Approach Offset check-box and associated X and Y fields allows the user to enable and set an approach offet. An approach offset does the following:

1. When a test is initiated the system will approach the probe to the sample offset from the desired testing location (the amount determined by the X and Yfields).

2. During the Lift Height the system will enable the X and/or Y axis stages and shift the stages the desired distance to perform the test in the originally located area

The Approach Offset will not function if:• The Lift Height is set to zero• The test is performed from with the probe in-contact (during in-situ imaging

and during a piezo automation)

When using the Approach Offset option the Lift Height should be set to a large enough value to avoid the probe from contacting the sample during the offset (due to sample tilt).

Lift Integral Gain (load control only) The Lift Integral Gain parameter allows the user to adjust the gain for the lift height that occurs immediately before a test is performed. If the Lift Integral Gain is set too high, the system may become unstable during the lift height. However, if the Lift Integral Gain is set too low the probe may not lift fully from the sample surface. The default value is 0.10.

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Load Function Tab

For more information regarding the integral, proportional, derivative, adaptive, or lift integral gains, refer to the Testing section of this user manual.

Lift Time (load and displacement control only) The Lift Time parameter allows the user to define the time used to perform the lift height. The default value is 2.0 sec.

Reseek Time (load and displacement control only) The Reseek Time parameter allows the user to define the time used to bring the probe from the defined lift height to the sample surface. The default value of 2.0 sec is approximate as any changes in sample height due to recovery or drift are not factored into this Reseek Time.

Pre-Displacement (load and displacement control only) The Pre-Displacement parameter (and Realtive to... drop down menu) allows the user to set a displacement (to be performed by the transducer) prior to starting the defined load function. The Pre-Displacement function is hardcoded to use the same rate as the reseek (Lift Height vs. Reseek Time). The default value is 0.0 nm.

Drift Monitor Time The Drift Monitor Time allows the user to enter a length of time for the system to monitor the drift of the system before any test. Default value is 40 seconds.

Drift Analysis Time The Drift Analysis Time allows the user to enter a length of time for the system to measure the drift rate. The system uses a linear fit to calculate the drift rate and the calculated rate will be taken into account when the result from the test is complete and the curve is fit to measure sample properties.

Drift Target Rate The Drift Target Rate parameter allows the user to define the maximum allowable drift rate desired prior to starting a test. The system will measure the drift rate after the initial Drift Analysis Time and, if less than the Drift Target Rate, start the test. If the drift rate is greater than the Drift Target Rate the system will continue to monitor the drift until either the drift rate becomes less than the Drift Target Rate or the system reaches the defined Drift Monitor Time. The default value is 0.05 nm/sec.

Drift Settle Time The Drift Settle Time parameter is an additional system settle time that allows the user to extend the amount of time the probe waits on the sample surface, in feedback, prior to beginning the drift correction procedure. The default value is 1 sec.

Pre-Load Integral Gain

(displacement control only) The Pre-Load Integral Gain field allows the user to adjust how accurately the probe is held to the sample surface during the drift correction and piezo scanner settle time. Increasing the Pre-Load Integral Gain will force the probe to hold more accurately to the sample surface, however, if set too high the system may become unstable. If the Pre-Load Integral Gain is set too low, the probe may lose contact with the sample surface during the drift correction or piezo scanner settle time. The default value is 0.10.

2.3.2 LOAD FUNCTION GENERATORAs an additional option to the Hysitron TriboScan software, the Load Function Creator software is an application that

enables the creation of complex load functions. The two complex load function types that are available with the Load

Function Creator software are:

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• Constant Strain Rate• Partial Unload/Cyclic

The purpose of the constant strain rate load function is to apply a force so that the test imitates a constant applied

strain.

The purpose of the partial unload function is to obtain several loading/unloading curves with one test. A partial

unload function will reveal differences or similarities in hardness and/or reduced modulus with respect to depth. With

this tool, depth profiles can be performed on samples with thin films or other coatings to investigate the differences in

the film region, the bulk region, and at the boundary point between the two.

Partial unloading functions take much longer than a standard indent and during this time drift is assumed to be a

constant rate, which may or may not be correct for extended time testing such as this. Additionally, displacements are

not re-zeroed following each unloading segment and, consequently, shallow indentation data may be skewed.

To access the Load Function Generator go to the Load Function tab Indentation sub tab and click the Load Func.

Gen. button located near the bottom of the window.

CONSTANT STRAIN RATE LOAD FUNCTIONThe constant strain rate load function is created from the Load Function Generator by selecting the Constant Strain

Rate option from the pull down menu in the upper left of the window (Figure 2.15).

Figure 2.15 Constant strain rate load

function editor

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Load Function Tab

After selecting the Load Function Type, the user must modify the associated parameters for the given type of load

function and then, when finished, verify the total time for the test and click the Return button to transfer the created

load function to the Load Function tab Indentation sub tab.

The constant strain rate load function, although it appears like one smooth curve, is actual split into several small

segments (default is 100 total segments). The user enters the Max Load, Strain Rate, Preloading Time, Hold Time,

Unloading Time and Number of Segments.

The number of segments defined includes the small segments used to construct the loading strain rate, the hold

segment, and the unloading. By default, this corresponds to 98 loading segments, 1 hold segment, and 1 unloading

segment

The time for the loading portion of the constant strain rate load function is calculated by:

The time segment is calculated with:

The first of the 98 segments starts at 0.0 seconds and ends at the Preloading Time, which is by default set to

0.1 seconds. The second segment will start at 0.1 seconds and end at [0.1 seconds] + [1 Time Segment]. The third

segment starts at the end of the second then adds [2 Time Segment] and so on.

The ending load of each segment is calculated with:

PARTIAL UNLOAD FUNCTIONThe partial unload function is created from the Load Function Generator by selecting the Partial Unload option from

the pull down menu in the upper left of the window (Figure 2.16).

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Figure 2.16 Partial unload load function

editor

After selecting the Load Function Type, the user must modify the associated parameters for the given type of load

function and then, when finished, verify the total time for the test and click the Return button to transfer the created

load function to the Load Function tab Indentation sub tab.

A description of the different user-adjustable parameters is given below:

Number of Cycles The Number of Cycles parameter defines the total number of times the function will load and unload.

Peak Load/Disp The Peak Load or Peak Disp. parameter defines the maximum load or displacement of the load function that will be achieved on the final load cycle

Displacement Exponent

Changes the exponent fit of the force vs. time curve, which allows for more partial loads at higher forces (lower displacement exponent) or for more partial loads at lower forces (higher displacement exponent)

Unloading Fraction The Unloading Fraction parameter controls the percentage of unloading for each unloading segment.

Loading Time The Loading Time parameter defines the time required for each loading segment.

Hold Time The Hold Time parameter defines the time required for each holding segment. Set this to zero for a two segment load/unload function (final hold time must also be zero).

Unloading Time The Unloading Time parameter defines the time required for each unloading segment.

Final Hold Time The Final Hold Time parameter defines the time required for the final hold segment. If the Hold Time parameter is zero, then the Final Hold Time must also be zero.

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Final Unloading Time The Final Unloading Time parameter defines the time required for the final unloading segment

When the load function is satisfactorily created, click the Return button in the bottom left corner of the screen and the

created load function will automatically be placed in the Load Function tab Indentation sub tab.

The load function is performed identically to any indentation load function. Because of the additional time associated

with partial unload testing, it is recommended to perform partial unload load functions from the in-situ imaging

position (to minimize system drift) when possible.

Partial unload load functions are analyzed similar to standard indentation tests. On the Analysistab Indentation sub tab if the user right-clicks the Execute Fit button they will be prompted to enter the number of the first unloading segment. The software will automatically fit to each additional unloading segment and produce a hardness and reduced modulus versus contact depth plot.

2.3.3 XPM SUB TAB

The XPM testing routine is an option upgrade available on any system using a performech II. For upgrade information please contact your Hysitron sales engineer.

The XPM (accelerated property mapping) load function editor (accessed from Load Function tab XPM sub tab) is

used to create all XPM tests (Figure 2.17). The XPM sub tab contains a plot and map with test location indicated with

a number. The plot indicates the test that will be performed at each location on the map.

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Figure 2.17 XPM sub tab

Number of Tests in X & Y

The Number of Tests in X & Y parameters allows the user to define how many tests to perform in the X and Y axis for the XPM (accelerated property map).

• Default value is 2• Minimum value is 1• Maximum value is 667

Spacing Between Tests in X & Y

The Spacing Between Tests in X & Y parameters allows the user to define the spacing between each test.

• Default value is 1.0000 µm• Minimum value is 0.0000 µm• Maximum value is defined by maximum piezo scan size for system

Total Distance in X & Y

The Total Distance in X & Y parameters is a display-only parameter that calculates the current size of the XPM test. The default value is 1.0000 µm because of the default Number of Tests in X & Y and the Spacing Between Tests in X & Y.

Lateral Move Speed The Lateral Move Speed parameter allows the user to define how fast the piezo scanner moves between the testing locations. The value may need to be reduced from default depending on system options installed.

• Default value is 10.0000 µm• Minimum value is 0.0001 µm• Maximum value is ∞ µm

Pre-Load & Use Imaging Setpoint

The Pre-Load & Use Imaging Setpoint parameters allow the user to define the pre-load force for the test. The defined pre-load value will be used for each location in the XPM test. The Use Imaging Setpoint check box will default the pre-load to the value defined in the Imaging tab Setpoint parameter.

• Default value is 2.00 µN

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• Minimum value is 0.050 µN• Maximum value is 5000 µN

Start & End Load The Start & End Load parameters allow the user to define the maximum load for the XPM test. The user can set the start and end parameters to the same value to perform the XPM tests all at the same load or adjust the load to obtain a depth profile of the sample.

• Default value for both is 100.00 µN • Minimum value for both is 0.00 µN• Maximum value for both is limited by the maximum force defined on the

Calibration tab System Calibration sub tab

Vary Load By The Vary Load By parameter allows the user to adjust the load by a fixed amount or percentage of last force. Adjusting by percentage of last segment will result in a logarithmic adjustment in load and fixed amount would be even steps. The Vary Load By parameter will only have an effect if the Start Load & End Load are not the same value.

• Default value is Fixed Amt.

Load Time, Hold Time, Unload Time

The Load Time, Hold Time, and Unload Time parameters allow the user to define the segment times for the XPM test. Each location of an XPM test will be a three segment test with the times defined with these three parameters.

• Default value for all three is 0.1000 seconds• Minimum value is 0.0001 seconds• Maximum value is ∞ seconds

Data Acquisition Rate & Number of Data

Points

The Data Acquisition Rate parameter allows the user to tune the number of points collected during the XPM test. Due to the length of the XPM test and the amount of data collected the data acquisition rate may need to be reduced to result in manageable file sizes. The Number of Data Points is a calculated value to allow the user view and adjust the data acquisition based on the current data collected.

• Default value is 1000 pts/sec• Minimum value is 0.01 pts/sec• Maximum value is ∞ pts/sec (suggested number of data points should be less

than 209,715)

File menu The File menu contains the Save Load Function to allow the user to save the created XPM load function to open in the Load Function tab Indentation sub tab.

Perform XPM button The Perform XPM button will perform the current defined XPM test at the current in-situ imaging position or optical focus position.

XPM testing can perform tests very quickly but in order to obtain reasonable results the type of hardware installed on

the system should be considered before creating and performing a test. A good indicator of a reasonable XPM test is

the number of tests per second. The XPM sub tab displays the Total Time under the test map area. Divide the total

time by the number of tests to find the Tests/Second value. It is suggested to keep the Tests/Second less than:

• 6 tests per second for nanoDMA transducer• 1 test per second for lateral axis transducer• 2 tests per second for indentation only transducers

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2.3.4 SCRATCH SUB TABThe nanoscratch load function editor (accessed from Load Function tab Scratch sub tab) is used to create all

standard nanoscratch tests. The nanoscratch load function can be saved at any time by clicking File Save Load

Function, likewise, a previously saved file can be opened by clicking File Open Load Function. TriboScan is

pre-loaded with some basic load functions located at C: Program Files Hysitron TriboScan Load

Functions.

Save time by modifying pre-made load functions to meet your testing needs. TriboScan comes loaded with several standard quasi static nanoindentation load functions. Open any of these load functions and modify the segment times, loads and number of segments instead of creating load functions from a blank window.


functions including a constant load, ramping load, and friction measurement nanoscratch tests.




function.

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The Advanced mode will give the user access to all parameters and can be more complicated for users who are

unfamiliar with the capabilities of the nanoindentation system. This user manual is written while in Advanced mode

so all parameters will be discussed.


This user manual is written with the User Mode set to Advanced so that all parameters will be discussed. If parameters discussed in this user manual are not present in the instrument software the user should verify the User Mode is set to Advanced.

AUTOMATIC SAVE MENUThe Automatic Save menu item allows the user to define a path and base file name for the tests that will be

performed. With the Automatic Save feature activated (with a check, similar to Figure 2.11) when a test has been

performed it will automatically be saved to the given directory with the given base file name and a test number (i.e.,

test_000, test_001, test_002, etc...). This feature prevents the user from having to name each individual file following

a test and will speed the individual test process.

Figure 2.20 Automatic Save menu

The normal force vs. time plot will be updated after any change has been made in the parameters below the load

function plot. When a segment is selected by a single left-click, the segment will turn red and the parameters below

the plot will adjust to reflect the properties of that particular segment.

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If the system is equipped with and being operated in Dual Head mode, the created load function will be saved and performed as whichever Transducer Slot (low load [three-plate capacitive] or high load [MRNP/3D OmniProbe]) is selected.

There are four buttons on the Scratch sub tab as shown in Figure 2.21. These buttons are the same for open loop and

feedback control testing. The buttons are described below:

Add Segment Clicking the Add Segment button will add a ten second, constant load or displacement segment immediately to the right of the currently selected segment. The user can select a segment by clicking on the segment in the normal force/normal displacement or lateral displacement versus time plot.

Remove Segment Clicking the Remove Segment button will remove the currently selected segment. The first and last segment can not be removed. There must always be at least two segments and the beginning and ending normal force/lateral displacement for the entire function must be 0.0 μN and 0.0 μm, respectively. The software will not allow the user to remove a segment that violates these truths.

Air Scratch Clicking the Air Scratch button will perform the defined nanoscratch load function from the current position in the air (if the system is not in contact with a sample surface). The Air Scratch button is disabled when the probe is in contact with a sample.

Perform Scratch Clicking the Perform Scratch button will perform the defined test at the position centered in the Video area of the Sample Navigation tab or at the center of the current in-situ imaging point (if the probe is in contact with the sample surface). This position must lie within a defined sample safety zone.

The Scratch sub tab will have a Control Feedback pull-down menu (similar to the Indentation sub tab) that the user

can select different feedback controlled testing options.

By selecting the different types of nanoscratch testing regimes from the Control Feedback pull-down menu (Open

Loop, Load, or Displacement control) the nanoscratch load function parameters will change. A description of the

parameters follows:

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Figure 2.21 Scratch sub tab

Normal Proportional Gain

(displacement control only) Displacement control tests are inherently more difficult in forcing the test to follow the desired testing load function. The Proportional Gainlooks at where the actual result is in relation to the desired result at any given time. Increasing the Proportional Gain may result in a quicker response but increased too much may cause oscillations. The default value is 0.0.

Normal Integral Gain (load and displacement control only) This field allows the user to define the Integral Gain. This gain has the biggest effect on how well the test follows the load function. The Integral Gain looks at where the actual result was in relation to the desired result and uses this information to make corrections and bring the actual result closer to the desired result. Increasing the Integral Gain forces the actual result to follow the desired result more closely; however, too much Integral Gain may cause instabilities in the system and too little will result in a sluggish response time. The default value is 1.0.

Normal Derivative Gain

(displacement control only) Displacement control tests are inherently more difficult in forcing the test to follow the desired testing load function. The Derivative Gainlooks at where the actual result is going to be in relation to the desired result at any given time. The Derivative Gain works to limit the amount of overshoot. Increasing the Derivative Gain by too much may result in a slower response. The default value is 0.0.

Normal Adaptive Gain

(displacement control only) Displacement control tests are inherently more difficult in forcing the test to follow the desired testing load function. The Adaptive Gainpredicts where the actual result is going to be in relation to the desired result at any given time, decreasing the Adaptive Gain may result in a slower response for complex load functions and an increased Adaptive Gain will force complex load functions to follow the desired result more closely. The default value is 0.0.

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There are similar Lateral gains (available for all lateral force testing modes) that works identically to the Normal gains given above. The defaults for the Lateral Gains are:

Proportional gain: 0.5 Integral gain: 0.5 Derivative gain: 0.0 Adaptive Gain 0.0

Tilt The Tilt parameter is automatically populated with the most recent tilt measurement performed on any currently defined sample. Tilt is measured and corrected from the Analysis tab Scratch sub tab Scratch Data sub tab.

Begin Force/Begin Disp.

The Begin Force or Begin Displacement field is used to enter the force or displacement for the selected segment to begin. The software will require that the user define the same value as the ending force or displacement for the previous segment (or zero for the first segment of the load function).

End Force/End Disp. The End Force or End Displacement field is used to enter the force or displacement for the selected segment to end. The software will require that the user define the same value as the beginning force or displacement for the following segment (or zero for the last segment of the load function).

Segment Time The Segment Time field allows the user to define a length of time for the selected segment. The loading rate will be automatically calculated.

Begin Time The Begin Time is the time that the selected load function segment will begin. This field is automatically populated and cannot be edited.

End Time The End Time is the time that the selected load function segment will end. This field is automatically populated and cannot be edited.

# to Average The # to Average field allows the user to define how to average the collected data. One corresponds to no averaging (raw data). Two corresponds to every two data points being averaged, yielding less data but a smoother plot, and so on.

Data Points The Data Points parameter displays the number of data points that will be collected during the currently selected load function segment. The Data Points is calculated based on the defined Data Acq. Rate and the time for the selected load function segment.

Data Acq. Rate The Data Acq. Rate parameter allows the user to define how many data points to collect per second for the duration of the test. The default is 200 pts/sec.

Total Number of Points

The Total Number of Points parameter displays the number of data points that will be collected for the entire test. This is calculated based on the Data Acq. Rate and the total test time.

Begin Lateral Displacement

The Begin Lateral Displacement parameter is used to enter the starting lateral displacement for the selected segment. The software will require that the user define the same value as the ending lateral displacement for the previous segment (or zero for the first segment of the load function).

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End Lateral Displacement

The End Lateral Displacement parameter is used to enter the final lateral displacement for the selected segment. The software will require that the user define the same value as the beginning lateral displacement for the following segment (or zero for the last segment of the load function).

Max Displacement The Max Displacement value is used as a global lateral displacement parameter. Changing the Max Displacement value will adjust all segments within a load function (with variance between the beginning and ending lateral displacement) so that the displayed load function reaches the defined Max Displacement.

Min Displacement The Min Displacement value is used as a global lateral displacement parameter. Changing the Min Displacement value will adjust all segments within a load function (with variance between the beginning and ending lateral displacement) so that the displayed load function reaches the defined Min Displacement.


The Peak Force or Peak Displacement field is used to enter the load function maximum force (open loop or load controlled test) or displacement (displacement controlled test) for the entire load function.

Pre-Load The Pre-Load field allows the user to define a load for the probe to hold while the system pauses to allow the piezo scanner to settle and the system drift to be measured. This value is typically set to be similar to the in-situ imaging setpoint value. The default value is 2.0 μN.

Use Imaging Setpoint The Use Imaging Setpoint will automatically use the same value for the Pre-Load as is currently used on the in-situ SPM imaging tab Setpoint value.

Lift Height (load and displacement control only) The Lift Height parameter allows the user define a height for the probe to lift off the sample following the drift correction and then start the test in the air above the sample surface. The Lift Height is usually used to ensure that the probe has not sunken into the sample surface during the drift correction and the test starts at the sample surface. The default value is 25 nm.

Approach Offset (load and displacement control only) The Approach Offset check-box and associated X and Y fields allows the user to enable and set an approach offet. An approach offset does the following:

1. When a test is initiated the system will approach the probe to the sample offset from the desired testing location (the amount determined by the X and Yfields).

2. During the Lift Height the system will enable the X and/or Y axis stages and shift the stages the desired distance to perform the test in the originally located area

The Approach Offset will not function if:• The Lift Height is set to zero• The test is performed from with the probe in-contact (during in-situ imaging

and during a piezo automation)

When using the Approach Offset option the Lift Height should be set to a large enough value to avoid the probe from contacting the sample during the offset (due to sample tilt).

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Lift Integral Gain (load control only) The Lift Integral Gain parameter allows the user to adjust the gain for the lift height that occurs immediately before a test is performed. If the Lift Integral Gain is set too high, the system may become unstable during the lift height. However, if the Lift Integral Gain is set too low the probe may not lift fully from the sample surface. The default value is 0.10.

For more information regarding the integral, proportional, derivative, adaptive, or lift integral gains, refer to the Testing section of this user manual.

Lift Time (load and displacement control only) The Lift Time parameter allows the user to define the time used to perform the lift height. The default value is 2.0 sec.

Reseek Time (load and displacement control only) The Reseek Time parameter allows the user to define the time used to bring the probe from the defined lift height to the sample surface. The default value of 2.0 sec is approximate as any changes in sample height due to recovery or drift are not factored into this Reseek Time.

Pre-Displacement (load and displacement control only) The Pre-Displacement parameter (and Realtive to... drop down menu) allows the user to set a displacement (to be performed by the transducer) prior to starting the defined load function. The default value is 0.0 nm.

Drift Monitor Time The Drift Monitor Time allows the user to enter a length of time for the system to monitor the drift of the system before any test. Default value is 40 seconds.

Drift Analysis Time The Drift Analysis Time allows the user to enter a length of time for the system to measure the drift rate. The system uses a linear fit to calculate the drift rate and the calculated rate will be taken into account when the result from the test is complete and the curve is fit to measure sample properties.

Drift Target Rate The Drift Target Rate parameter allows the user to define the maximum allowable drift rate desired prior to starting a test. The system will measure the drift rate after the initial Drift Analysis Time and, if less than the Drift Target Rate, start the test. If the drift rate is greater than the Drift Target Rate the system will continue to monitor the drift until either the drift rate becomes less than the Drift Target Rate or the system reaches the defined Drift Monitor Time. The default value is 0.05 nm/sec.

Drift Settle Time The Drift Settle Time parameter is an additional system settle time that allows the user to extend the amount of time the probe waits on the sample surface, in feedback, prior to beginning the drift correction procedure. The default value is 1 sec.

Pre-Load Integral Gain

(displacement control only) The Pre-Load Integral Gain field allows the user to adjust how accurately the probe is held to the sample surface during the drift correction and piezo scanner settle time. Increasing the Pre-Load Integral Gain will force the probe to hold more accurately to the sample surface, however, if set too high the system may become unstable. If the Pre-Load Integral Gain is set too low, the probe may lose contact with the sample surface during the drift correction or piezo scanner settle time. The default value is 0.20.


The Peak Force or Peak Displacement field is used to enter the load function maximum force (open-loop or load controlled test) or displacement (displacement controlled test) for the entire load function.

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2.3.5 SCANNINGWEAR SUB TABThe scanning wear load function editor (accessed from Load Function tab ScanningWear sub tab) is used to create

all automated scanning wear tests. The scanning wear load function can be saved at any time by clicking File Save

Load Function, likewise, a previously saved file can be opened by clicking File Open Load Function.

ScanningWear testing is not available while using the MultiRange NanoProbe (MRNP) or 3D OmniProbe transducers.

Automated ScanningWear load function testing is only available with 1:1 (square) resolution settings.

Figure 2.22 ScanningWear sub tab

Scanning wear tests can be performed by holding a constant setpoint force and scanning for a defined number of

passes, by adjusting the setpoint force during a single scan, or a combination of the two modes.

The method for performing a scanning wear test is to perform a small in-situ SPM image at an elevated setpoint for a

defined number of passes. When this has completed, an in-situ SPM image is captured at a normal setpoint and

slightly larger scan size. The amount of material worn away from the increased setpoint (and/or number of passes)

can be analyzed with TriboView (further analysis information is given in the Imaging section of this user manual).

If the system is equipped with and being operated in Dual Head mode, the created load function will be saved and performed as whichever Transducer Slot (low load [three-plate capacitive] or high load [MRNP/3D OmniProbe]) is selected. Post imaging is ALWAYS performed with the low load transducer.

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! A scanning wear test can only be performed with a MRNP/3D OmniProbe system when used in conjunction with a closed loop scanning stage. Contact Hysitron if there are questions or for purchasing information regarding the closed loop scanning stage.

There are several parameters given on the ScanningWear sub tab (given in Figure 2.22). There are two headings:

Wear Test Parameters and Post Wear Imaging Parameters. The testing parameters will be defined under the Wear

Test Parameters and the imaging parameters and image storage information is defined under the Post Wear Test

Imaging Parameters. The parameters are described below:

Start Setpoint The Start Setpoint parameter is the setpoint that the wear test will start. If the user would like a constant setpoint, the Start Setpoint and End Setpoint should be the same value. Selecting the radio button next to the Start Setpoint parameter indicates this value will be calculated based on the End Setpoint and Adjust Peak Setpointparameters.

End Setpoint The End Setpoint parameter is the setpoint that the wear test will end. If the user would like a constant setpoint, the End Setpoint and Start Setpoint should be the same value. Selecting the radio button next to the End Setpoint parameter indicates this value will be calculated based on the Start Setpoint and Adjust Peak Setpointparameters.

Adjust Peak Setpoint The Adjust Peak Setpoint parameter is the amount that the setpoint will adjust for each step in the progressive wear test (the number of steps defined in the Scan Lines/Step parameter). Selecting the radio button next to the Adjust Peak Setpoint parameter indicates this value will be calculated based on the Start Setpoint and End Setpointparameters.

Scan Resolution The Scan Resolution parameter allows the user to select from the resolution for the ScanningWear testing based on the options available on the system. All systems will have 64, 128, and 256 resolutions available. Additional resolutions may be avaialble.

Scan Lines/Step The Scan Lines/Step parameter determines how the progressive wear test should divide the increasing setpoint force. The options for this parameter are dependent upon the available scan resolutions on the system.

Scan Rate The Scan Rate parameter defines the frequency to perform the scanning wear test. One cycle is defined as a forward and reverse scan (over and back).

Scan Size The Scan Size parameter defines the size to perform the scanning wear test. The maximum scan size will be limited by the range of the piezo scanner.

Integral Gain The Integral Gain parameter allows the user to adjust how well the probe follows the sample surface. This is the same parameter that appears on the Imaging tab. The default of 240 works well for most samples and is a good starting gain for most samples.

Approach Integral Gain

The Approach Integral Gain parameter allows the user to define a gain to use during the probe approach. The default of 90 works well for most samples and is a good starting gain for most samples.

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# of Passes The # of Passes parameter defines the number of times the wear area is scanned during the test. The scanning wear tests will always start at the bottom of the image and scan upward. For tests with a # of Passes more than 1, all scans will start at the bottom of the image and scan upward.

Save Image After Each Pass

The Save Image After Each Pass parameter allows the user to save *.hdf image files of the scanned area if the # of Passes is set to more than 1.

Post Image File Directory

The Post Image File Directory defines where the image captured following the scanning wear test will be saved. This information can be modified by selecting the Save As button.

Post Image Base File Name

The Post Image Base File Name defines the name of the image captured following the scanning wear test. This information can be modified by selecting the Save As button.

Save As Button The Save As button is used to modify the name and location of the images saved following a wear test.

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2.4 ANALYSIS TABThe Analysis tab contains the analysis tools and functions for analyzing most data collected with Hysitron systems.

Depending on the options and upgrades the instrument has been equipped with, additional sub tabs may be available

from the Analysis tab, each of which would be discussed in the option or upgrade user manual.

The Analysis tab contains the following sub tabs:

Indent The Quasi sub tab is composed of two additional sub tabs:• Quasi

The Quasi sub tab is standard on all Hysitron systems and contains all nanoindentation analysis.

• Multi ChannelThe Multi Channel sub tab is optional and will be available only on instruments equipped with nanoECR. All nanoindentation data that contains nanoECR information (constant applied voltage or current with increasing displacement) is analyzed from this sub tab. The Multi Channel sub tab will be discussed in the nanoECR user manual.

• Sweep AnalysisThe Sweep Analysis sub tab is optional and will be available only on instruments equipped with nanoECR. All nanoindentation data that contains nanoECR information (changing voltage or current; I-V curves) is analyzed from this sub tab. The Sweep Analysis sub tab will be discussed in the nanoECR user manual.

• XPMThe XPM sub tab is optional and will be available only on instruments equipped with a performech II and XPM (accelerated property mapping). XPM analysis is performed within the XPM sub tab. The XPM sub tab will be discussed in this section as most performech II equipped systems will have XPM testing installed. If your system does not have XPM testing contact your Hysitron sales engineer for more information.

Scratch The Scratch sub tab is composed of two additional sub tabs:• Scratch Data

The Scratch Data sub tab is standard on all instruments, however, lateral force (2D) transducer hardware is required for use. All nanoscratch analysis occurs from within the Scratch Data sub tab.

• TriboImageThe TriboImage sub tab is optional and will be available only on instruments equipped with TriboImage. The TriboImage sub tab contains all analysis routines for the TriboImage reciprocating scratch test upgrade.

nanoDMA The nanoDMA sub tab includes the analysis routines for nanoDMA data. This sub tab is optional and will be available only on instruments equipped with nanoDMA.

Image The Image sub tab opens TriboView, a stand alone image analysis software for the collected Hysitron in-situ images (*.hdf files).

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Figure 2.23 Quasi sub tab

2.4.1 QUASI SUB TABThe nanoindentation (sometimes referred to as quasi static nanoindentation) analysis is accessed from the Analysis

tab Quasi sub tab Quasi sub tab and is used for all open loop, load, and displacement controlled

nanoindentation analysis. Many of the shortcut icons on the menu bar at the top of the Quasi sub tab Quasi sub tab

are also located in the command bar and are defined below:

Open File (also available from File Open)

The Open File command allows the user to open any previously saved *.hysnanoindentation data file.

Edit File (also available from File Edit File)

The Edit File command opens the File Calibration Constants window (Figure 2.24) which allows the user to view and/or edit any previously saved *.hys nanoindentation file constants values.

The Edit Calibration Constants window is available for user information (to display the parameters used during the currently loaded test). Editing parameters within the File Calibration Constants is typically not recommended unless the user is familiar with more advanced operation of the Hysitron system. Editing values in the Edit Calibration Constants window are applied only to the currently open file and are not applied to the system transducer constants (values used for future tests).

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Figure 2.24 File Calibration Constants

window (accessed from the Editbutton)

Editable values include:• Spring force compensation• Drift rate• Load scale factor• Displacement scale factor• Electrostatic force constant• Machine compliance• Plate spacing• Number of data points to average• Probe area function

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Export Text File (also available from File Export Text File)

The Export Text File command creates a tab delimited text file of the currently open *.hys file so that the data can be viewed by third party programs. The text file includes the load and displacement information with respect to time.

Print Graph (also available from File Print Graph)

The Print Graph command prints the currently displayed plot as viewed on the monitor.

Print Window (also available from File Print Window)

The Print Window command prints the currently displayed window including any fitting information and calculated values.

Define Area Function (also available from Setup Tip Area Function)

The Define Area Function command opens the Calibration tab Tip Area Functionsub tab Open sub tab to allow the user to open a previously saved nanoindentation probe area function.

Plot vs. Time (also available from Analysis Plot vs. Time)

The Plot vs. Time command displays the currently open *.hys file as force and displacement versus time. This is a useful troubleshooting tool as well as useful for certain analysis routines.

Multiple Curve Analysis (also available from Analysis Multiple Curve Analysis)

The Multiple Curve Analysis command allows the user to load and fit several *.hysfiles to produce a hardness and reduced modulus plot vs. contact depth. The plot is saved as a tab delimited text file so that it may be accessed by third party programs as well.

Multiple Curve Analysis Partial Unload Fmt 1 (also available from Analysis Multiple Curve Analysis Partial Unload Fmt 1)

The Multiple Curve Analysis Partial Unload Fmt 1 command is used for performing analysis for partial unload load functions. After selecting this option, the user is prompted to select the files to analyze followed by a prompt to enter the segments for the analysis to be performed. This command produces the standard hardness and reduced modulus vs. contact depth plot for the selected data.

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Multiple Curve Analysis Partial Unload Fmt 2 (also available from Analysis Multiple Curve Analysis Partial Unload Fmt 2)

The Multiple Curve Analysis Partial Unload Fmt 2 command is used for performing analysis for partial unload load functions. After selecting this option, the user is prompted to select the type of modulus desired as well as the resulting text file delimiter and (if necessary) Young’s Modulus for the probe and Poisson’s Ratio for the probe and sample. This command produces individual text files, delimited as specified, that can be viewed by third party programs.

Plot Multiple Curves (also available from Analysis Plot Multiple Curves)

The Plot Multiple Curves command allows the user to plot several *.hys files on the same plot for visual comparison. From the Plot Multiple Curves window, the user can further analyze the plot by performing a Multiple Curve Analysis.

Hardness and Modulus Plot (also available from Analysis Hardness and Modulus Plot)

The Hardness and Modulus Plot command opens the standard hardness and reduced modulus versus contact depth plot used during the Multiple Curve Analysis routine. Any previously created hardness and reduced modulus versus contact depth text file can be opened by accessing this command.

The Quasi sub tab has additional options that do not have a corresponding icon:

File Export Multiple Text Files

The Export Multiple Text Files command allows the user to select several *.hys files to export as tab delimited text files to be used by third party programs.

File Update Multiple Files

The Update Multiple Files command works similar to the Edit icon but will update several files at the same time. To use the Update Multiple Files command:

1. Open one of the *.hys file to be updated.

2. Go to the Calibration tab System Calibration sub tab.

3. Enter ALL transducer constants as desired for the files to be updated.

4. Go to the Analysis tab Quasi sub tab Quasi sub tab File Update Multiple Files. When prompted select the files to be updated and click OK.

5. Open a *.hys file that was updated and click the Edit icon, the Current Parame-ter Values should read the desired updated values.

! Using the Update Multiple Files command will modify the *.hys file(s) with all parameters listed in the Calibration tab System Calibration sub tab. This includes ALL transducer constants, Plate Spacing, Electrostatic Force Constant and gain settings.

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File Combine Multiple Curve

Analysis Files

The Combine Multiple Curve Analysis Files command combines multiple hardness and modulus vs. contact depth plots into a single *.txt file.

File Multiple File Re-Zero Offsets

The Multiple File Re-Zero Offsets command allows the user to do the same offset commands (as described in the next section) to multiple files simultaneously.

The Analysis tab Quasi sub tab Quasi sub tab also several buttons, a check box, and a pull-down menu:

Force Offset The Force Offset button allows the user to select a new point to be the origin of the force axis. This option is primarily intended for use with feedback-controlled tests that have a pre-test lift height and may incorrectly register the point where the probe contacts the sample surface as the zero force value.

Auto The Auto button next to the Force Offset button is a shortcut button to quickly perform a force offset in the plot. The Auto feature will use the Displ. Cutoff for Force Offset parameter for the automatic calculation. The system will look at the approach data prior to the value defined in the Displ. Cutoff for Force Offset and average the force values in order to give a new zero force value. The Displ. Cutoff for Force Offset parameter should be chosen to be more negative than any adhesion effects while still allowing an adequate data sampling to obtain a reasonable zero force point.

Displ. Offset The Displ. Offset (Displacement Offset) button allows the user to select a new point to be the origin of the displacement axis. This option is primarily intended for use with feedback-controlled tests that have a pre-test lift height and may incorrectly register the point where the probe contacts the sample surface as the zero displacement value.

Auto The Auto button next to the Displ. Offset button is a shortcut button to quickly perform a displacement offset in the plot. The Auto feature will use the Force Endpoint for Displ. Fit parameter for the automatic calculation.

The system will look at the curve (at forces lower than the Force Endpoint for Displ. Fit) parameter and perform a complex, iterative, Hertzian fit on the curve to determine the zero displacement point. The optimal value will depend on the sample properties, shape of the curve, and data acquisition rate.

Include Load Offset in Displ. Fit (Adhesion)

The Include Load Offset in Displ. Fit (Adhesion) check box will take into account sample adhesion (if present) when performing the Hertzian fit with the Auto button next to the Displ. Offset button. This feature is enabled by default.

The Auto buttons perform the same process as what is performed when running the automatic calibration procedure (discussed in the Auto Calibration sub tab section).

Force and displacement offset commands permanently change the data files. The user may want to make a secondary copy of the data files before performing any offset commands.

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The Force Offset and Displ. Offset buttons allow the user to make any point on the plot the origin. This is helpful in

accounting for setpoint or lift height artifacts (Figure 2.25) that may be present with load or displacement controlled

testing. To use these options, select a new point (by left-clicking) on the plot to be the zero force or zero displacement

and click either Force Offset and/or Displ. Offset.

Figure 2.25 Displacement offset of load

control test

Only plots with a Lift Height should be used with the Force Offset or Displacement Offset. Without a proper lift height segment, such as Figure 2.25, where the test starts in the air above the sample the user will be unable to properly identify the zero loading point. These offsets should not be used with open loop testing as there is no Lift Height with open-loop testing.

TriboAnalysis offline analysis software available from Hysitron can perform multiple plot force or displacement offsets. Contact Hysitron for more information about TriboAnalysis.

Execute Fit The Execute Fit button uses the parameters listed above the buttons (as well as the defined probe area function) to fit the data in the displayed plot. Many of the fields given to the right of the plot are populated after the Execute Fit button has been clicked.

Go to The Go to button will move the X, Y and Z-axis to the optical camera location that the currently displayed test was performed.

Graph to Clipboard The Graph to Clipboard button copies the currently displayed plot onto the computer clipboard so that it may be copied into a third party program.

Toggle Grid The Toggle Grid button cycles through the available grid options for the displayed plot. Options include: no grid, vertical grid, horizontal grid and horizontal/vertical grid.

Area Function The Area Function pull-down menu determines which probe area function will be used to calculate the parameters listed to the right of the displayed plot when the Execute Fit button is clicked:

• Saved With Indent File uses whichever area function was saved on the system when the test was initially performed.

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• From Tip Area Tab uses the currently saved area function in the Calibration tab Tip Area Function sub tab Open sub tab.

The Analysis tab Quasi sub tab Quasi sub tab also has several fields listed to the right of the displayed plot.

Some fields are user definable while others are populated by clicking the Execute Fit button:

Be sure to analyze the UNLOADING segment or select the Auto check box next to the Unloading Segment parameter. The Auto check box will automatically execute a fit on the final segment (which is typically the unloading segment).

Figure 2.26 Graphical representation of

plotted values

Reduced Modulus The Reduced Modulus field is populated when the fit is executed and is calculated with the equation:

Where Er is Reduced Modulus, A(hc) is Contact Area, and S is Stiffness.

Hardness The Hardness field is populated when the fit is executed and is calculated with the equation:

Where H is Hardness, Pmax is Maximum Force, and A(hc) is Contact Area.

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Contact Depth The Contact Depth is populated when the fit is executed and is calculated with the equation:

Where hc is Contact Depth, hmax is Maximum Depth, Pmax is Maximum Force, and Sis Stiffness. The 0.75 value is often referred to as epsilon which is used to account for edge effects including the deflection of the surface at the contact perimeter. 0.75 is the historically used value and this value cannot be modified within TriboScan.

Contact Stiffness The Contact Stiffness field is populated after the fit has been executed and is defined as the stiffness of the material adjusted to remove any effects caused by spring stiffness of the transducer.

Max Force The Max Force parameter is the maximum recorded force of the test.

Max Depth The Max Depth parameter is the maximum recorded displacement of the test.

Contact Area The Contact Area is defined by the area function with respect to the contact displacement.

Drift Rate The Drift Rate parameter is automatically populated based on the displayed indentation drift rate calculation. The Drift Rate can be modified by selecting the Edit button on the menu bar.

Power Law Coefficients [A], [hf]

and [m]

The fit executed by TriboScan on standard nanoindentation tests follows the power law fit:

Upper Fit % The Upper Fit % parameter allows the user to determine how closely the fit should follow the data at the upper portion of the unloading segment. Increasing this value forces a closer fit at the initial unload portion while decreasing this value results in a closer fit further down on the unloading portion of the plot. The default Upper Fit %is 95.

Lower Fit % The Lower Fit % parameter allows the user to determine how closely the fit should follow the data at the lower portion of the unloading segment. The default Lower Fit % is 20.

Unload Point The Unload Point is defined as the index of the first point of the unloading segment of the displayed plot. This point is automatically selected by the software but can be modified by the user, if necessary.

Cursor Position The Cursor Position is given as the currently selected point on the plot as chosen by the user.

Unloading Segment The Unloading Segment field allows the user to select the unloading segment for the displayed plot. It is important that this field be properly set before clicking the Execute Fit button or the plot will not be properly fit. For a standard trapezoid load function with a load segment, hold segment and unload segment, the Unloading

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Segment should be set to 3 (or select the Auto check box to automatically fit to the final segment in a load function).

The value set in the Unloading Segment field is also used when performing the fit for the Multiple Curve Analysis.

Iterations This self-populated field displays the number of iterations performed by the computer before obtaining a reasonable fit for the plot.

Force The Force parameter displays the force for the currently selected point in the plot.

Displacement The Displacement parameter displays the displacement for the currently selected point in the plot.

PLOTTING MULTIPLE CURVESThe multiple curve plot is used to analyze multiple curves simultaneously. The multiple curve plot is useful in

showing the repeatability of a test on a sample as well as difference between two similar samples. The multiple curve

plot can be accessed by selecting the Plot Multiple Curves icon or from the Analysis menu Plot Multiple Curves

from the Analysis tab Quasi sub tab (Figure 2.27).

Figure 2.27 Multiple curve plot

To add curves to the plot click the Add Curves button. To remove individual curves, left-click the curve to remove and

then click the Remove Curve button. To fit the displayed curves (using the fitting parameters, including the Unloading

Segment, given on the Analysis tab Quasi sub tab) and receive a hardness and reduced modulus versus contact

depth plot click the Mult. Cur. Ana. button. To export each of the *.hys files as a text file, click the Mult. Cur. Expt.

button.

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The Remove TAF Outliers button is an automated routine that can autotically remove outlier curves from a set of load

vs. displacement curves. The routine is intneded to be used Berkovich probe tests on the fused quartz standard

performed in order from increasing load to decreasing load.

HARDNESS AND REDUCED MODULUS VS. CONTACT DEPTH PLOTThe hardness and reduced modulus versus contact depth plot (Figure 2.28) will be displayed each time a Multiple

Curve Analysis is performed or it can be accessed directly by selecting the Hardness and Reduced Modulus Plot icon

or the Analysis menu Hardness and Reduced Modulus Plot.

Figure 2.28 Hardness and Reduced Modulus

versus Contact Depth Plot

Average and standard deviation information for the selected data set is displayed at the top of the window. The

displayed values are given for the range of data for the currently selected data set (or all data sets if the Compute

Statistics Using All Data Sets check box is selected). The displayed values also only include data for the selected data

set between the two cursors (brown and blue cursor).

Add Data Set The Add Data Set button allows for more than one set of hardness and reduced modulus versus contact depth plot to be displayed simultaneously.

Remove Data Set The Remove Data Set button will remove the selected data set from the plot.

Toggle Path The Toggle Path button toggles between displayign the file name and the file path with file name.

Plot Data Sets The Plot Data Sets button will plot the statistical information for each of the currently viewed data sets. The Plot Data Sets plot uses the average value for the given data sets and standard deviation information to create error bars.

Export Summary Data

The Export Summary Data button creates a *.csv file containing the data file name, mean contact depth, standard deviation of contact depth, mean hardness, standard

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deviation of hardness, mean reduced modulus, and standard deviation of reduced modulus.

Print Graph The Print Graph button prints the current plot to an available system printer (Hysitron does not supply a printer with the standard system).

Close The Close button closes the Modulus and Hardness vs. Contact Depth plot. The plot must be closed before accessing any other tabs within TriboScan.

The data sets presented in the Hardness & Modulus vs. Contact Depth plots are saved as a *.txt file and can be opened as a tab delimited file in any third-party spreadsheet program.

2.4.2 XPM SUB TABThe XPM analysis is accessed from the Analysis tab Quasi sub tab XPM sub tab and is used for all XPM test

analysis. Menu items and buttons will be described below.

XPM data may also be displayed in the Quasi (standard indent analysis) sub tab. The Quasi sub tab does not properly account for zero point offset and should not be used for XPM analysis.

Figure 2.29 XPM sub tab

The following options appear under the File menu.

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Select File For Analysis

The Select File For Analysis menu item allows the user to select a single XPM test for analysis.

Analyze Current File The Analyze Current File menu item (also Analyze Current File button located at the bottom left of the XPM sub tab) will prompt the user to enter the load to use as the cut off for the zeroing (usually near set point force) and the data will be zeroed (in displacement) and fit using the fitting parameters on the Quasi sub tab. The Analyze Current File menu item will also populate the plots on the right side of the XPM sub tab.

Analyze Multiple Files

The Analyze Multiple Files menu item (also Analyze Multiple Files button located at the bottom left of the XPM sub tab) will open and analyze multiple XPM files. The plots on the right side of the XPM tab will be populated with multiple maps plotted on the same scale.

Export Curve to Text The Export Curve to Text menu item will export the current displayed curve to a single text file.

Export All Curves to Text

The Export All Curves to Text menu item will export all displayed curves to a single text file.

Export Plots to BCRF Images

The Export Plots to BCRF Images menu item will export the current plots on the right of the XPM sub tab to *.BCRF images that can be opened and analyzed further in TriboView.

The following options appear under the XPM Plot menu.

Smooth, Level, & Block

The Smooth, Level, and Block menu items allow the user to select different plotting structures for the hardness and modulus plots on the right side of the XPM sub tab.

Local Coordinates & Stage Coordinates

The Local Coordinates and Stage Coordinates menu items allow the user to toggle the plots on the right side of the XPM sub tab between piezo scanner range and X & Y stage axis range.

There are also parameters and buttons listed at the bottom of the XPM sub tab. The parameters and buttons

immediately under the curve plot relate to the currently selected curve. The user can select a different curve from the

plot by left clicking on the curve and the displayed values will update accordingly. There is also a Remove and Go To

button that will remove the curve from the plot and move the optical microscope to the selected location, respectively.

On the right side of the XPM sub tab there are two additional sub tabs. The data displayed on the

XPM Plot The XPM Plot sub tab displays a temperature plot for hardness and reduced modulus with respect to X and Y position. The hardness and reduced modulus plots are calculated (with the Analyze Current File button) by fitting the XPM test curves with the fitting parameters set in the Quasi sub tab and Calibration tab Tip Calibrationsub tab.

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Histogram The Histogram sub tab displays a histogram plot for hardness and modulus. The histogram plots are calculated (with the Analyze Current File button) by fitting the XPM test curves with the fitting parameters set in the Quasi sub tab and Calibration tab Tip Calibration sub tab.

2.4.3 SCRATCH SUB TABThe nanoscratch analysis (accessed from the Analysis tab Scratch sub tab Scratch Data sub tab) is used for all

open loop, load, and displacement controlled nanoscratch analysis. Many of the shortcut icons on the menu bar at the

top of the Scratch sub tab Scratch Data sub tab are also located in the command bar and are defined below:

Open File (also available from File Open)

The Open File command allows the user to open any previously saved *.hysnanoscratch data file.

Edit File (also available from File Edit File)

The Edit File command opens the File Constants window (Figure 2.30) which allows the user to view and/or edit any previously saved *.hys nanoscratch file constants values.

The File Constants window is available for user information (to display the parameters used during the currently loaded test). Editing parameters within the File Constants is typically not recommended unless the user is familiar with more advanced operation of the Hysitron system. Editing values in the File Constantswindow are applied only to the currently open file and are not applied to the system transducer constants (values used for future tests).

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Figure 2.30 Nanoscratch File Constants

window

Editable values include:• Spring force compensation• Drift rate• Indentation and scratch load scale factor• Indentation and scratch displacement scale factor• Indentation and scratch electrostatic force constant• Machine compliance• Scratch plate spacing• Scratch imaging position• Scratch displacement offset• Number of data points to average

Export Text File (also available from File Export Text File)

The Export Text File command creates a tab delimited text file of the currently open *.hys file so that the data can be viewed by third party programs. The text file includes the load and displacement information with respect to time.

The Scratch sub tab has additional options that do not have a corresponding icon:

File Resave The Resave command will save the current scratch data file with any corrections (such as tilt correction or edited transactor constants). The Resave command overwrites the original file.

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File Print The Print command allows the user to print a copy of the currently displayed nanoscratch file.

File Edit Constants File Area Function

The Area Function command allows the user to view the current area function and, if desired, apply a new area function to the data file. However, the nanoscratch analysis does not include a data fit and, because of that, is not area function dependent.

File Update Multiple Files

The Update Multiple Files command works similar to the Edit icon but will update several files at the same time. To use the Update Multiple Files command:

1. Open one of the *.hys file to be updated.2. Go to the Calibration tab System Calibration sub tab.

3. Enter ALL transducer constants as desired for the files to be updated.

4. Go to the Analysis tab Scratch sub tab Scratch Data sub tab File Update Multiple Files. When prompted select the files to be updated.

5. Open a *.hys file that was updated and click the Edit icon, the Current Parame-ter Values should read the desired updated values.

! Using the Update Multiple Files command will modify the *.hys file(s) with ALL parameters listed in the Calibration tab System Calibration sub tab. This includes all transducer constants, Plate Spacing, Electrostatic Force Constant and gain settings.

File Calibrate The Calibrate command is used to calibrate the lateral force transducer during the Lateral Force Calibration. The calibration is performed automatically by the software so the Calibrate button should be used only at the direction of a Hysitron service engineer.

The Analysis tab Scratch sub tab Scratch Data sub tab also contains five buttons and one pull-down menu:

Segment Plotted The Segment Plotted pull-down menu allows the user to select the segment of interest to view in the current plots or to view in the friction plot (by clicking the Friction button). All is selected by default, however, typically only the middle segment of a nanoscratch test (the actual scratching segment) is of interest.

Tilt Correction The Tilt Correction button is used to remove the effects of sample tilt on nanoscratch testing. It is very difficult, if not impossible, to mount a sample perfectly flat. Because of this, Hysitron has built a tilt correction procedure into the nanoscratch analysis window. The Tilt Correction procedure is given in the Analysis section of this user manual

Friction The Friction button (also available from Analysis Friction) opens a plot of Lateral Force divided by Normal Force [friction] versus Time.

Go to The Go to button will move the X, Y and Z-axis to the optical camera location that the currently displayed test was performed.

Graph to Clipboard The Graph to Clipboard button copies the currently displayed plot onto the computer clipboard so that it may be copied into a third party program.

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Toggle Grid The Toggle Grid button cycles through the available grid options for the displayed plot. Options include: no grid, vertical grid, horizontal grid and horizontal/vertical grid.

All of the parameters given in the upper right portion of the Analysis tab Scratch sub tab Scratch Data sub tab

are given from the relative and absolute positions of the two red indicator bars that can be adjusted by left-clicking on

any plot and dragging the bars to a new location.

2.4.4 IMAGE SUB TABThe in-situ SPM imaging analysis is accessed from the Analysis tab Image sub tab OR C: Program

Files Hysitron TriboView TriboView.exe. TriboView is used to analyze the in-situ SPM images captured

within TriboScan and is a standard stand-alone program included with all TI series systems. The functionality and

features available with TriboView will be discussed in the Analysis section of this user manual.

2.5 PLOT SCALINGThe plot scaling throughout TriboScan (and other Hysitron programs) is identical for all analysis and calibration

plots. To access the plot scaling options double left-click on any plot in TriboScan to open the Axis Settings window

(Figure 2.31). The settings in the Axis Settings window are standard plotting parameters. To adjust a parameter

uncheck the Auto Scale button or Auto Divisions check box and adjust the associated parameters.

Figure 2.31 Axis Settings window

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To reset a plot back to default scaling, open the Axis Settings window and toggle all Auto Scale and Auto Divisions check boxes to enabled.

In addition to the Axis Settings window the plots can be manually zoomed in or out by holding the CTRL key (on the

keyboard) and holding the left mouse button (to zoom in) and right mouse button (to zoom out).

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2.6 IMAGING TABThe TI series systems include in-situ SPM Imaging which is performed by using the feedback between the

TriboScanner piezo scanner and the indentation axis of the transducer to trace the sample surface with the

nanoindentation probe at a constant setpoint force. The TriboScanner piezo scanner is only used for imaging the

surface and positioning the probe. During a test, the TriboScanner piezo scanner is stationary and the indentation or

nanoscratch test is performed by the transducer.

The Imaging tab contains the parameters and tools for obtaining an in-situ SPM image and performing

nanomechanical testing from the current imaging location. Depending on the options and upgrades that the

instrument has been equipped, additional sub tabs may be available from the Imaging tab, each of which would be

discussed in the respective option or upgrade user manual.

Figure 2.32 in-situ sub tab

This user manual has been written with SPM+ which allows for higher resolution scanning and more customizable scanning options. If your system is not equipped with SPM+ contact your Hysitron saels engineer for upgrade options.

The Imaging tab in-situ sub tab contains five distinct areas:

• Imaging Button/Menu Bar• Image and Scan Settings• Positioning Controls• Scan Line/Histogram

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IMAGING BUTTON/MENU BAR

Figure 2.33 in-situ sub tab Button and Menu

Bar

The imaging button and menu bar have many of the important functions used to perform an in-situ image. Many of

the button bar functions at the top of the in-situ sub tab are also located in the menu bar and are defined below:

Approach (also available from Engage Approach)

The Approach command moves the X, Y, and Z axis stages from the current, defined, optical position and brings the nanoindentation probe into contact with the sample.

Withdraw (also available from Engage Withdraw)

The Withdraw command moves the X, Y, and Z axis stages to remove the probe from the sample surface and return the stages to the optically focused area of interest (where the probe was last located on the sample).

Start Scan (also available from Control Start Scan)

The Start Scan command, using the TriboScanner piezo scanner, begins scanning the sample surface using the parameters defined in the Imaging Controls area. The system will continue to scan the sample surface, reversing direction at the top and bottom of the image, until further action is taken.

Stop Scan (also available from Control Stop Scan)

The Stop Scan command stops scanning the sample surface and keeps the nanoindentation probe located on the sample surface in feedback. If the Stop button is used when the scanning is resumed the scan will restart at the edge of the scanning window.

Pause Scan (also available from Control Pause Scan)

The Pause Scan command stops scanning the sample surface and keeps the probe located on the sample surface in feedback at the location of the pause so the Go button can be used to resume scanning from the same location.

Capture (also available from Image Capture)

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The Capture command saves the next completed in-situ SPM image as an *.hdf file so that further analysis can be performed. Any changes within the Imaging Controls area will delay the Capture until the next completed in-situ image with no parameter changes.

When the Capture command is initiated, a camera icon will appear to the left of the upper left-most in-situ image. The camera icon will disappear when the image has successfully been captured. If the camera icon is right-clicked, the user may define how many consecutive images to capture (Figure 2.34).

Figure 2.34 Consecutive image capture

window

The first image that is captured for a new workspace will prompt the user to select a directory and filename (also accessed from Image Capture File Name...). The directory is selected by clicking the Browse Folders button. The base file name is entered into the Image File Base Name field, unless modified, any additional images will be saved in the same directory with the same filename with an underscore and number starting at 0000 (Figure 2.35).

Figure 2.35 in-situ image Capture Images

window

All of the images displayed on the Imaging tab in-situ sub tab will be saved when the Capture command is executed. Each of the image types is designated by a suffix code following the filename to distinguish the image type.

Not all channels are available on all systems. Some channels are available only for diagnostic or troubleshooting purposes.

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Figure 2.36 Captured *.hdf file suffixes

Capture Now (also available from Image Capture Now)

The Capture Now command captures the currently displayed in-situ images for further analysis with TriboView.

The Capture Now command will capture the currently displayed image despite differences in scan size, scan rate, setpoint, sample surface, etc… This command should be used carefully to ensure that the proper scanning parameters are being considered while analyzing the image.

Cancel Capture (also available from Image Cancel Capture)

The Cancel Capture command cancels any pending image capture command that has been executed.

Test (also available from Control Test)

The Test command forces the instrument to stop scanning the sample surface, move the probe to the center of the currently viewed in-situ image and perform a nanomechanical test.

The type of test performed when the Test command is executed is determined by the current Mode of the instrument (set on the Action Bar). The load function performed will be whichever load function is currently loaded on the Load Function tab for the given mode that the instrument is set.

Scanning Wear Test (also available from Control Wear)

The Scanning Wear Test command will perform the scanning wear load function as defined in the Load Function tab Scanning Wear sub tab.

_GGradient

_TTophography

_LFLateral Force

_LIA1Lock-In

Amplifier Channel 1

_LIA2Lock-In

Amplifier Channel 2

_ECRnanoECR

_ECRSnanoECR Sense

_ADC1-8Hysitron

Control Unit Backpanel ADC

1-8

_XPZTX Axis Piezo

Voltage

_YPZTY Axis Piezo

Voltage

_ZPZTZ Axis Piezo

Voltage

_DVTransducer

Displacement Voltage

_AMPAmplitude

_PHAPhase

_DAMPDamping

_LOSSLoss Stiffness

_STORStorage Stiffness

_TANDTan Delta

_LMODLoss Modulus

_SMODStorage

Modulus

_FRFriction

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Channel Selection (also available from Control Channel Selection)

The Channel Selection command will open the Channel Selection window (Figure 2.37) for the user to select the channels to view and/or save on the in-situ sub tab. The channels available on the Channel Selection window will vary depending on the options equipped on the system.

Figure 2.37 Channel Selection window

Users can select individual channels to display or use the Fast Selection section to quickly display images related to default (standard topography and gradient images), modulus mapping (if equipped), or nanoECR imaging (if equipped).

To select individual channels to display the User Mode menu will need to be in Advanced mode.

Background Subtraction (also available from Image Background Subtraction)

The Background Subtraction command will open the Background Subtraction window (Figure 2.38).

Figure 2.38 Background Subtraction window

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The default system background subtraction is None. Due to sample tilt and roughness users will typically need to use Linear Regression (line-by-line fit). Other background subtraction options (including offline options) will be discussed in the TriboView/in-situ imaging analysis section of this user manual.

No matter how the real-time background subtraction is set, all in-situ images captured from TriboScan will be saved with no background subtraction applied. Background subtraction can be re-applied to saved images using TriboView or any other third party *.hdf analysis program.

Color Table (also available from Image Color Table)

The Color Table command allows the user to adjust the image coloring for all visible images. The default color table setting is Brown.

Distance (also available from Pointer Distance)

The Distance command allows the user to measure a distance on any of the in-situSPM images by left-clicking the mouse and dragging the pointer. The distance value is given above the upper left-most in-situ image.

Offset (also available from Pointer Offset)

The Offset command allows the user to visually select the new center of the in-situSPM image. After selecting the Offset command, left-clicking on any of the in-situimages will perform a piezo offset to move the area of interest to the center of the viewed image.

Zoom (also available from Pointer Zoom)

The Zoom command allows the user to resize and re-center the in-situ SPM image. After the Zoom command is selected, left-clicking on any of the in-situ images and dragging the cursor will resize and re-center the image by performing a piezo offset and scan size adjustment.

Disengage Tip (also available from Engage Disengage Tip)

The Disengage Tip command pulls the probe away from the sample surface a small distance (defined in the Preferences sub tab) but does not return the stages to the current optical focus position.

The Disengage Tip command is primarily intended for short-term use when the user does not want to move the probe far from the sample surface but wants to be out of contact with the sample surface. By using the Disengage Tip command in place of a full withdraw, when possible, can reduce thermal drift and shorten test times by reducing stage motor moves.

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The Disengage Tip command is also useful when the Hysitron control unit requires re-zeroing while imaging a sample surface.

The software cannot be paused, perform tests or stage moves while the probe is disengaged and a full withdraw must be performed.

Engage Tip (also available from Engage Engage Tip)

The Engage Tip command brings the probe back into contact with the sample surface after a Disengage Tip command has been performed.

Modulus Mapping Setup (also available from Control Modulus Mapping Control)

(Modulus Mapping equipped TI series systems only) The Lock-In Control button opens the Lock-In Control window to allow users to set the lock-in amplifier parameters in order to perform a modulus mapping test.

nanoECR (also available from Control nanoECR Imaging Control)

(nanoECR equipped TI series systems only) The nanoECR Imaging Control button opens the nanoECR Imaging Setup window to allow the user to scan while applying a voltage or current.

! Due to small contact area between the probe and sample during in-situ imaging the current density from (even very small) applied voltages can cause probe damage. Care should be taken while performing nanoECR imaging.

The in-situ sub tab has additional options that do not have a corresponding icon:

File Save Imaging Parameters

The Save Imaging Parameters menu item allows the user to save all configured imaging settings to be easily accessed for future use. The file saved is a *.inpxextension is an XML format.

Saved imaging parameters work alongside the saved workspace. Whichever saved item is loaded last (workspace or *.inpx file) will take precedence.

File Open Imaging Parameters

The Open Imaging Parameters menu item allows users to open a pre-saved imaging parameter file (*.inpx).

Engage Re-Zero the Controller

The Re-Zero the Controller command is intended to be used if the zero reference of the Hysitron control unit has drifted over time due to either electronic drift, sample electrostatic attraction or thermal changes. The Re-Zero the Controller command

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will automatically perform a Disengage Tip command, measure a new zero reference point, perform an Engage Tip command and continue scanning the sample surface.

Control Scanner Head Selection

The Scanner Head Selection command allows the user to define the type of scanner being used with the system. Most systems are equipped with only an open loop scanner (for low load system operations). Other options that use the Scanner Head Selection field will be discussed in the respective user manual.

Control Load Calibration File

The Load Calibration File command allows the user to load any previously saved TriboScanner scanner calibration file (*.scl file). The Load Calibration Filecommand only allows scanner calibration files located in the C: Program Files Hysitron TriboScan Calibrations Scan directory to be loaded into the software.

Control Tip Radius Calibration

(Modulus Mapping equipped TI series systems only) The Tip Radius Calibrationcommand is used while performing a modulus mapping test to calculate the apparent probe radius at very small displacements (during an in-situ image). This command will be discussed in the nanoDMA/Modulus Mapping section of this user manual.

Image Capture File Name… ( )

The Capture File Name… ( ) command allows the user to define the directory and file name for any saved in-situ SPM images. This command is automatically executed if the Capture command is selected and a directory/filename has not previously been established for the current workspace. This command opens the window shown in Figure 2.35.

Image Copy To Clipboard

The Copy To Clipboard command copies the current in-situ SPM image to the computer clipboard to allow the user to quickly paste the image into a desired imaging program. Copied files cannot be used for further analysis in TriboScan or TriboView.

Image Save Bitmap

The Save Bitmap command saves the current in-situ SPM image as a bitmap file that can be used by third party programs for publishing in reports, presentations or other documentation. Because this is a picture, not a data file, there is no analysis available from Hysitron for this type of file captured from TriboScan.

Image Anti-Aliased Image Plot

The Anti-Aliased Image Plot command will smooth the viewed image and remove rough or abrupt edges. The default setting is on (checked) but the option may need to be disabled depending on the surface of the sample and observed imaging artifacts.

Pointer Color The Color command allows the user to select the color used for the in-situ imaging pointer (measured distances, selections, offsets, etc...). The default is Auto (which is blue).

Pointer Clear The Clear command removes any pointer indicators from the in-situ images (measured distances, selections, offsets, etc...).

User Mode The User Mode command allows the user to toggle between Standard and Advanced user modes. The Standard user mode will have the most commonly used

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imaging parameters and fields available for editing while the Advanced user mode has all imaging parameters available for viewing/editing.

This user manual is created with the user mode switched to Advanced. If a parameter discussed in this user manual is not visible in your software first try to toggle the user mode to Advanced and contact Hysitron for additional assistance.

IMAGE AND SCAN SETTINGSThe Image and Scan Settings area displays the current viewable in-situ images as well as the commands associated

with the image size, quality, probe location, and orientation. The parameters included in the Image and Scan Settings

area are identified in Figure 2.39.

Figure 2.39 Scan Settings area of the in-situ

sub tab

Probe Locators The Probe Locators determine where the nanoindentation probe is located and the direction of scanning while an in-situ image is being performed.

There are three side-arrow buttons [ ] in the Probe Locator area. Clicking the top arrow will move the probe to the top of the scanning area and restart the in-situ image from top to bottom. Clicking the middle arrow will move the probe to the middle of the image while retaining the same scanning direction and clicking the bottom arrow will move the probe to the bottom of the scanning image and restart the in-situ image from the bottom to top.

There is one up/down arrow button [ / ] in the Probe Locator area. Clicking the up/down arrow will reverse the current slow scan axis scanning direction.

There is a Passes field listed in the Probe Locator area. The Passes field counts the number of completed scans of the current in-situ image. The Passes field will

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continue to count the number of full scans that have been completed until the probe is disengaged or withdrawn from the sample surface (this resets the Passes field to zero). The Passes field information is primarily used for scanning wear tests.

Image Channel Selector

The Image Channel Selector area (the area below the primary image) contains the available channels to display in the primary image window. The channels available for display will depend what channels are selected on the Channel Selection window (on the button bar).

Scan Settings The Scan Settings area contains all physical properties of the in-situ SPM image. This includes:

• Scan Rate• (Fast/Slow) Scan Size• (Fast/Slow) Resolution• Scan Orientation• Setpoint• Integral Gain• Proportional Gain• Derivative Gain

The Scan Rate determines the speed of the scanned image and is changeable from 0.01 Hz up to 12 Hz. The default Scan Rate is 1.0 Hz; slower scan rates will offer less image distortion while higher scan rates may cause noise or artifacts depending on the sample.

The Scan Size will vary for each system and is based on the properties of the piezo ceramic material and the piezo scanner calibration. The maximum scan size for a new piezo scanner is typically greater than 60 μm. Typically the Scan Size is locked in a 1:1 ratio but in Advanced user mode the fast and slow scan sizes can be adjusted independently.

The Resolution determines the quality of the scanned images. The maximum resolution available will depend on the system configuration. Typically the resolutionis locked to be the same in the fast and slow scan axis, however, in Advanced user mode the resolution can be modified for each axis.

The Scan Orientation determines the fast and slow scan axis as well as the direction for the scan.

The Setpoint is the force that the nanoindentation probe applies to the sample surface while in contact and in feedback with the sample surface. The default value is 2.0 μN

The Integral Gain determines the feedback loop between the transducer and the piezo scanner. The default gain settings work well for most samples, however, this value can be increased to produce a sharper image but may cause ringing at larger values. The default Integral Gain is 240 for TI series systems.

If the system is being used with an xProbe MEMS-based transducer the usable integral gain range will be severely reduced (around 10x lower).

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The Proportional and Derivative Gains allow the users to adjust the gains with standard PID gain tuning. Typically, the Proportional and Derivative Gains are set to zero and can be adjusted by selecting the Modify P&D check box.

POSITION CONTROLSThe Position Controls area contains all of the commands associated with moving the X, Y, and/or Z axis stages as

well as the X and Y axis of the TriboScanner piezo scanner while performing the in-situ SPM images.

Figure 2.40 Position Controls area of the in-

situ sub tab

The blue bar on the left side of the Position Controls area shows the current Z axis position of the TriboScanner piezo

scanner. This blue bar should be near the center in order to allow the scanner to respond to most sample surface

changes by automatically retracting or extending to maintain contact. A fully extended or retracted blue bar

represents that the piezo scanner is out of range and the image quality will be very poor or no image will be present.

A fully extended or retracted piezo scanner is typically caused by: electronic drift in the setpoint, too low of a setpoint

and the probe has drifted off of the sample, static charge on the sample or probe, or the probe has sunken into a soft

sample. If the piezo scanner is out of range, the user should perform a Rezero the Controller (from the Engage menu).

The Piezo Offset values allow the user to adjust the X and Y axis center positioning by moving the piezo scanner. The

Piezo Offset is also used for the Offset and Zoom icons. Piezo Offset values are limited by the piezo scanner range.

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The Stage Navigation arrows allow the user to manually move the X, Y, and/or Z axis stages while performing an in-

situ SPM image. While imaging, the stage speeds are hard-coded to move at the defined Ultra Fine speed.

The Move (Relative) values allow the user to enter a value in micrometers and click the Move button to automatically

move the stages to a new location. Large stage moves (greater than approximately 100 μm) are not recommended

while the probe is in contact with the sample surface because of the time required and sample slope.

The Show Reticule check box places a cross hair on the primary in-situ SPM image to identify the center of the image

(Figure 2.41).

Figure 2.41 in-situ image with reticule

SCAN LINE/HISTOGRAMThe Scan Line/Histogram plots (Figure 2.42) display the histogram and scan line(s) for the currently selected in-situ

image.

Figure 2.42 Scan Line/Histogram are of the

in-situ sub tab

The Histogram plot has several functions that are given below with corresponding numbers in Figure 2.43:

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1. Expand and reduce the scale by left-clicking and dragging on the dark blue bar.

2. Expand and reduce the scale by left-clicking on the Minimum/Maximum up/down arrows.

3. Enter a new value for the Minimum/Maximum scale.

4. The double arrow is used to expand and reduce the scale; right-click to increase the Maximum scale and left-click to increase the Minimum scale.

5. The Auto button will automatically move the Minimum and Maximum scale values to cover all data points.

6. Move the Minimum/Maximum range by left-clicking and dragging on the light blue bar.

Figure 2.43 Location of histogram functions

The Scan Line plot shows the real-time scan line of the currently selected in-situ image. Using the pull-down menu,

the user can select which scan line(s) to view. The options include either the Forward, Reverse or Forward &

Reverse.

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2.7 AUTOMATION TABThe Automation tab contains the parameters and tools for performing automated testing routines. Depending on the

options and upgrades that the instrument has been equipped, additional sub tabs may be available from the

Automation tab. Additional options or upgrades will be covered in the respective user manuals.

The Automation tab contains the following sub tabs:

Methods The Methods sub tab contains the information and parameters used to setup and perform stage-driven automated testing routines. Methods utilize the automated X and Y axis staging system.

The Methods sub tab contains two side tabs:• Setup• Position

Piezo Automation The Piezo Automation sub tab contains the information and parameters used to setup and perform piezo-driven automated testing routines. Piezo automations utilize only the piezo scanner for positioning the probe during the automated routine.

Figure 2.44 Automation tab

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2.7.1 METHODS SUB TABThe Methods sub tab contains several items. This section will discuss the operation of each of the available options.

In addition to this section, in the Testing section of this user manual a procedure outlining how to set up and run a

basic automated method will be discussed.

Automated methods are configured and executed from the current optical position or a variety of previously defined

optical positions. Because of this, the left side of the Methods sub tab is nearly identical to the Sample Navigation tab

to allow the user to navigate the sample space, define samples and perform other functions without the need to toggle

between tabs. The operation of all function listed on the left side of the Methods sub tab is discussed in the Sample

Navigation tab section of this user manual.

The Methods sub tab consists of two side tabs:

• Setup• Positions

The functions available from each of the side tabs is discussed in the following sections.

Automated methods must be setup and performed from optical positions and cannot be executed while the nanoindentation probe is in contact with a sample surface.

SETUP SIDE TABThe Setup side tab is the primary tab used for configuring the properties of the automated methods. The Setup side tab

contains five distinct sub sections from top to bottom:

• Method Operation/Data Storage• Patterns Selection• Positions Selection• Load Function Configuration• in-situ Imaging/Method Chaining

Method Operation/Data Storage

The Method Operation/Data Storage area (Figure 2.45) is where the:• Method Name is defined• Method Type (Indent, Scratch, etc...) is selected• File Name and Directory for saving data is selected

To begin creating a new method, click the New Method button. To edit an existing method click the Edit Methods button. Automated methods are saved within the currently open workspace.

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Figure 2.45 Method Operation/Data

Storage area

Selecting the New Method or the Edit Properties button will open the New Method or the Edit Method window (Figure 2.46). The New Method or Edit Method window allows the user to select the name of the automated method, type of automated method (Indent, Scratch, ScanningWear), and the file name/directory. There is also a Position and Timestamp check box which would add the associated information to the file name of each test.

Figure 2.46 Edit Method window

Array Patterns The Array Patterns area (Figure 2.47) is where the user sets the pattern that will be performed at each defined area of an automated method. There are two options to create a pattern.

Figure 2.47 Pattern Selection area

The Simple Grid option allows the user to set a number of tests by rows and columns with spacing between tests. After changing the rows, columns, or spacing click the Update Grid button to update the display.

The Use Pattern option allows users to create a more complicated pattern for the automated method. Select the Use Pattern radio button then select a pre-made pattern from the pull-down menu or click the Edit Pattern button to open the Pattern Editorwindow (Figure 2.48) and create a new pattern.

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The system must be in Advanced user mode in order to have access to the Edit Pattern button.

Figure 2.48 Pattern Editor window

Use the New Grid or New Circle button to start a new pattern and use the remaining parameters on the window to adjust the grid or circle. When finished click the Closebutton to go back to the Setup tab.

Note the Scale Unit parameter setting. Default value in some versions of software are millimeter.

In the Array Patterns section the user can also select to adjust the pattern (either offset or rotate). The offset parameters are especially useful if the same automated method is being run multiple times and the user wishes to run the same patterns but offset to a slightly different location.

The Counter Clockwise parameter is useful when a grid pattern is needed but the entire grid needs to be rotated to match a sample orientation.

Target Positions Automated methods can be performed in three different ways:• From the current optical position• From optically defined Positions in a Group (defined on Position side tab)• From method specific positions (defined with Add Current Location button)

Figure 2.49 Target Positions area

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From the current optical position is a simple routine that will perform the defined load function over the defined pattern on whichever sample location the optical camera is currently located. The number of times the pattern is performed (and the offset between each successive pattern) can be adjusted with the relevant associated parameters.

From optically defined positions in a group is more complex but greatly increases the functionality of the automated testing method routine. Within the Position side tab Groups and Positions can be created. A Group can contain several Positions on the same sample or different defined samples, however, a Group can only perform one type of Pattern for all defined Positions. Each automated method can only perform tests within one Group. If more than one type of Pattern is required for the automated methods, several Groups must be created with varying Positions and individually selected Patterns. The relationship between Automated Testing Methods, Groups, Positions and Patterns is given in Figure 2.50.

Figure 2.50 Methods, Groups, Positions and

Patterns representation

When performing a method with defined Positions within a Group the user may choose to adjust the pattern in the X or Y direction for each Position within the Groupor rotate the Pattern. When performing a method from the current optical position, the Pattern can be adjusted, which modifies the X/Y placement all Patterns. The Offset command will offset each consecutive Pattern a defined amount.

The Method Specific Positions radio button was introduced as a simplified alternative to creating position groups and positions. To use the Method Specific Positions radio button focus on an area of a defined sample to perform the pattern and click the Add Current Location button (repeat as necessary to create as many positions as desired).

Load Function Configuration

The Load Function Configuration area (Figure 2.51) is where the user selects a pre-saved load function to be performed at the Positions defined within the method.

The load function is selected and configured by clicking the Load Function button. After the load function has been configured, a description of the load function will appear in the text box below the Load Function button.

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Figure 2.51 Load Function Configuration

area

The Load Function button will open the Load Function Setup window (Figure 2.52).

Figure 2.52 Load Function Setup window

Any pre-saved load function can be loaded by clicking the Select Load Functionbutton. The four radio buttons beneath the Select Load Function button define how the load function adjusts over the duration of the automated method.

Not all parameters are available for nanoscratch and ScanningWear testing.

Typically, the second option is selected for most automated method routine where users want the load to vary over the duration of the test while maintaining a reasonable testing time. The load parameters selected in the lower section of the window will vary based on the selection in the upper part of the window.

The load parameters are adjusted by selecting a radio button next to the parameter on the left that the user wants the instrument to automatically calculate. The user must then define a value for the two unchecked parameters and the checked parameter will automatically be calculated.

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Click OK on the Load Function Setup window when finished to return to the Automation tab Methods sub tab Setup side tab.

The Auto Cal at Start check box will initiate the Auto Calibration routine when starting the automation (from the Calibration tab Auto Calibration sub tab).

Delay Control/Imaging

The Delay Control button opens the Delay Control window (Figure 2.53). The Delay Control window allows the user to define scheduled time to start the automated method as well as additional delay times before the start of the automated method and between each event in the automated method.

Figure 2.53 Delay Control window

The Imaging button is used to set the imaging properties for pre and post imaging of the automated testing methods. Selecting the Imaging button opens the Imaging Setupwindow (Figure 2.54). Within the Imaging Setup window the user can choose to perform in-situ or optical image pre and/or post each event in the automated method. The in-situ imaging parameters must first be saved as an *.inpx file before using the Imaging Setup window.

Figure 2.54 Imaging Setup window

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Method Chaining Method Chaining is the process of combining multiple automations to be performed in sequential order. The Method Chain window (Figure 2.55) can be accessed by selecting the Method Chain button.

Figure 2.55 in-situ Imaging/Method

Chaining area

The list of automated methods that have been created is given on the right under the Avaialble Methods list with the Chain Content on the left showign the order and information regarding the automated method chain that will be performed.

The buttons in the center of the Method Chain window perform the following functions:

Move selected automated method order up in the defined method chain.

Move selected automated method order down the defined method chain.

Add selected automated method to method chain.

Remove selected automated method from the method chain.

To start the automated method (including any defined method chains) select the Start Method button from the

Automation tab Methods sub tab.

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POSITION SIDE TABThe Position side tab (Figure 2.56) is the tab used for creating and configuring groups that contain position locations

to perform the previously defined patterns. The Position side tab contains several buttons, all of which are described

in Figure 2.56.

The Position side tab only needs to be configured if the automated method is using the Indent Pattern Using Positions In radio button option.

Figure 2.56 Position side tab

New The New button is used to create a new group. Clicking the New button will open a window to assign a name to the new group, the user is then required to move the automated stages to desired location(s) within any available sample boundary and select various positions for a defined pattern to be performed.

Duplicate The Duplicate button creates a duplicate group for the currently selected group.

Rename The Rename button allows the user to rename the currently selected group.

Delete The Delete button allows the user to delete the currently viewed group.

Add Above The Add Above button uses the currently defined X, Y and Z-axis position and defines a new pattern location within the currently selected group above the currently displayed pattern location.

Add Below The Add Below button uses the currently defined X, Y and Z-axis position and defines a new pattern location within the currently selected group below the currently displayed pattern location.

Remove The Remove button removes the currently selected pattern location from the given group.

Combi Setup The Combi Setup button is used to setup position groups for testing combinatorial wafer sample sets. More information on the setup and running of combinatorial testing is provided in the Testing chapter of this user manual.

Go To The Go To button moves the X, Y and Z-axis so that the selected position location is in the current optical view.

Edit The Edit button opens the Edit Point window and allows the user to rename the currently selected pattern position as well as modify the defined X/Y-axis position of the point.

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2.7.2 PIEZO AUTOMATION SUB TABThe Piezo Automation sub tab (Figure 2.58) contains all of the required parameters to set up, configure and execute

automated tests using the piezo scanner for positioning (automated stages, if equipped, are not used during piezo

automation testing).

ScanningWear testing is not available while using the MultiRange NanoProbe (MRNP) or 3D OmniProbe transducers.

The Piezo Automation sub tab will always use the currently open load function (based on the Mode of the software)

when performing the automated testing. Because of this, the user will never be prompted to select a load function.

Piezo automations are configured and executed while the probe is in contact and scanning the sample that is to be

tested. The piezo automation will be limited to the current scan size (as set in the Imaging tab). There are two types of

piezo automations listed under the Script Mode pull-down menu (Figure 2.57): array script and click script.

Figure 2.57 Script Mode pull-down menu

ARRAY SCRIPT The Array Script (Figure 2.58) is used for performing a grid of indents over the available surface. When setting up an

Array Script the user will need to define the number of tests to perform in X as well as Y and the spacing between the

tests.

With an Array Script, the Piezo Translation Protocol must be selected as either Constant Direction (Always Left-to-

Right) or Serpentine (Start at Upper Left Corner). Constant Direction will perform the piezo automation from left-to-

right starting with the top row and moving downward. Serpentine will start at the upper left point, move across the

top row then move to the right-most point of the second row and move from right to left and so on (Figure 2.59).

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Figure 2.58 Array Script piezo automation

Figure 2.59 Constant direction and

serpentine translation protocols

CLICK SCRIPTThe Click Script (Figure 2.60) is used for performing precisely placed indents based on the currently viewed image in

the upper left quadrant of the Imaging tab. The user selects the testing locations by left-clicking the desired locations,

individual points can be removed by right-clicking the given points. Because piezo automations are set up while

scanning the sample surface, the image can be updated at any time by clicking the Update Image button.

Click Script piezo automation tests are always performed in the order that the locations were selected when clicking.

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Figure 2.60 Click Script piezo automation

Both Array Script and Click Script piezo automations have the following parameters:

Save Scan The Save Scan parameter will force the system to scan the surface following the piezo automation and save an image in the currently defined image directory from the Image tab. The scan settings (scan rate, size, setpoint, etc...) on the Image tab will be used for this image.

Stay in Contact The Stay in Contact parameter will keep the nanoindentation probe on the sample surface following the piezo automation. This option is not recommended if the user does not plan to be at the instrument when the test is finished (or soon thereafter). Selecting No will disengage the probe from the sample surface upon the completion of the automation.

Re-Zero Lift Height The Re-Zero Lift Height parameter allows the user to define how high the probe should be lifted from the sample surface between tests in order to zero the control unit. The default of 100 nm should work well for most samples and is typically increased for soft samples or samples with attractive properties.

Time Delays There are two time delay parameters: Before the 1st Test and Between Tests. The time delays define how much time to wait before the first test or between each test thereafter (this is in addition to the standard system feedback and drift measurement times). These values are typically increased in order to increase the accuracy of the piezo automation test placement by reducing the X/Y-axis piezo drift introduced by performing piezo offsets.

Scanning Wear To perform a scanning wear piezo automation, select the Scanning Wear Test box. The scanning wear load function defined in the Load Function tab will be performed at each testing location selected.

When the user is ready to start the piezo automation, click the Run Piezo Automation button. The user will be

prompted to select a folder to save the resulting files (Figure 2.61) followed by a prompt for the user to define a base

file name (Figure 2.62) and the Set Loads window (Figure 2.63).

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Figure 2.61 Select directory for piezo

automation data

Figure 2.62 Select base file name for piezo

automation data

Figure 2.63 Set beginning and ending forces

for piezo automation tests

On the Set Loads window, the user can choose the starting and ending loads for the array of tests. If all tests are to be

performed at the same load, the same value should be entered for the Start and End Load parameter.

The Adjust Load By parameter allows the user to select either Fixed Amount, Percent, or Custom.

Fixed Amount Fixed Amount is selected if the user wants the number of tests to be divided evenly over the given starting and ending load range.

Percent Percent is selected if the user wants the tests to be divided over the given starting and ending load range based on a percentage of the maximum defined force. The Percent option typically results in the indents being spaced further at higher loads and spaced more closely at lower loads.

Custom Custom is selected if the user wants to define a load for each test (or a range of tests) during an automation. When Custom is selected an Edit... button will appear next to

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the field, select the Edit... button will open the Piezo Automation Custom Parameterswindow where the user can define a peak load for each test as well as a post image (for an individual test).

The piezo automation will always perform the currently open load function (for the current system Mode) at each location of the automated test.

If the test being performed is an indentation test, the load function is used for the segment times only and after selecting a base file name, the user will be prompted to enter a beginning and ending force for the tests.

Nanoscratch tests can be performed with piezo automations. To run a piezo automation of nanoscratch tests, install a lateral force transducer, set the software to Scratch mode, image a sample surface, create a scratch load function and then execute a piezo automation. During a piezo automation the user can choose to run all scratches at the same normal force or adjust the normal force of the scratch over the array of nanoscratch tests.

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Calibration Tab

2.8 CALIBRATION TABThe Calibration tab contains the calibrations that are required for keeping Hysitron systems running properly.

Depending on the options and upgrades that the instrument has been equipped, additional sub tabs may be available

from the Calibration tab. Additional options and upgrades will be covered in the respective user manual.

The Calibration tab contains the following sub tabs:

System Calibrations The System Calibrations sub tab is available with all Hysitron instruments and is used to perform the calibrations necessary to verify the transducer is operating properly and account for small changes in transducer properties that may be caused by temperature, humidity or changing probe mass.

Stage Calibration The Stage Calibration sub tab is available with all TI series systems and is used to perform the calibrations associated with the stage and optical camera system alignment.

Tip Calibration The Tip Calibration sub tab is available with all Hysitron systems. The Tip Area Calibration sub tab contains the tools required for calculating, saving, and opening nanoindentation probe area function information.

Machine Compliance The Machine Compliance sub tab is available with all Hysitron systems. The Machine Compliance sub tab contains an automated method for calculating the instrument machine compliance.

in-situ The in-situ sub tab is available with the TI series systems. The in-situ sub tab contains the tools for calculating, saving, and opening calibration files for the TriboScanner piezo scanner.

Auto Calibration The Auto Calibration tab is available with all TI series systems. The Auto Calibrationtab allows the user to define the system automatic calibration routines timings and tolerances.

! It is important that the user is familiar with ALL calibrations associated with the options installed on the TI series system. The user must read and understand all sections of this user manual that are relevant to the installed options.

2.8.1 SYSTEM CALIBRATIONS SUB TABThe System Calibrations sub tab is used to perform the calibration necessary to verify the instrument is operating

properly and to account for small changes in transducer properties that may be caused by temperature, humidity or

changing probe mass. The System Calibrations sub tab is given in Figure 2.64.

There are three main areas of the System Calibration sub tab:

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Transducer Constants Constants in this area are copied directly from the transducer constants sheet or are properties of the transducer/instrument that WILL NOT be adjusted during the calibrations.

Transducer Calibrations

Constants in this area are copied directly from the transducer constants sheet or are properties of the transducer/instrument that WILL be adjusted during the calibrations.

System Parameters Variables in this area are intended to match corresponding hardware settings. This area contains gain and attenuations settings for the system.

A description of the parameters given in the System Calibrations sub tab is given below.

Figure 2.64 System Calibrations sub tab with

color-coded parameters

Indentation Axis Load Scale Factor

The Load Scale Factor for the transducer is measured at the Hysitron factory. The Load Scale Factor is measured by attaching various calibrated masses to the center plate of the transducer and recording the changing output voltage. The slope of the mass applied versus the measured output voltage is the Load Scale Factor in mV/mg.

Indentation Displacement Scale

Factor

The Displacement Scale Factor for the transducer is measured at the Hysitron factory. The Displacement Scale Factor is measured by installing a probe with a mirror and using an interferometer to measure the displacement of the probe (and thus center plate of the transducer). The slope of the displacement (as measured from the interferometer) versus the measured output voltage is the Displacement Scale Factorin mV/μm.

Sensor Bias The Sensor Bias is a property of the Hysitron control unit and should read On(-0.032)at all times unless otherwise advised by a Hysitron service engineer.

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Machine Compliance The Machine Compliance is a calculated value that represents the compliance of the entire system including the sample, probe, transducer, scanner, X/Y and Z-axis stage assemblies and any associated instrument base. The Machine Compliance calculation is discussed in the Indentation Analysis section of this user manual and will be approximately:

• 1.0 for a normal force transducer• 3.0 for a lateral force transducer• 0.5 for a nanoDMA II & III transducers

Bias Offset The Bias Offset is the amount of offset applied to the center plate of the transducer to allow for bi-directional movement of the nanoindentation probe.

The bi-directional movement is most important during the lift height before performing a feedback control nanoindentation test or measuring the drift rate before a test is begun. The default value is 180 nm, however, this value can be turned up to 2000 nm if larger bi-directional movement is required. Keep in mind, however, the transducer has a maximum range of 5 μm and any value entered into the Bias Offsetfield will be subtracted from the total available forward range of the Z-axis displacement.

Scratch Axis Load Scale Factor

The scratch axis Load Scale Factor is measured at the Hysitron factory by actuating the scratch axis of the transducer against a well-calibrated load cell and is given in mV/mg.

Scratch Axis Displacement Scale

Factor

The scratch axis Displacement Scale Factor is measured at the Hysitron factory by performing a light force scratch across a well-defined grid pattern and adjusting the Displacement Scale Factor to yield the expected result and is given in mV/μm.

Scratch Axis Imaging Positioning

The scratch axis Imaging Position is used to offset the nanoscratch test to be performed completely with only one of the two available drive plates on the lateral force transducer.

If the Imaging Position were set to zero, when a nanoscratch is performed, approximately half way through the scratch the transducer would switch from one drive plate to the other as the center plate passes through the neutral position. To prevent this, the Imaging Position is used to offset the probe when the transducer is toggled to Scratch mode and then the scratch is performed completely with one drive plate. This value is set at Hysitron, however, many times transducers may have a corresponding Imaging Position that works comparably as well located at approximately the opposite magnitude.

When the instrument is toggled between Indent, nanoDMA mode [or Modulus Mapping mode for nanoDMA III systems], and Scratch mode the probe will be offset by the Imaging Position value. This small amount (typically around 10 μm) is usually not an issue, but if the sample was imaged in Indentmode and switched to Scratch mode, the previous image would be offset by the Imaging Position value in the scratch axis direction.

E-Stop Delay Time The E-Stop Delay Time is used to reduce the frequency of a false emergency stop. With certain, high-sensitivity transducers it is possible to cause an emergency stop condition simply by moving the X, Y, or Z-axis stages even with the probe far from any sample surface. The E-Stop Delay Time allows the user to define a time for the system to sense an excessive force before producing an emergency stop condition.

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The default value is 3 ms and the maximum safe delay time allowed by the software is 100 ms.

Tare The Tare parameter displays the tare value of the transducer (indicator of the rest position of the center plate of the three-plate capacitive sensor). The Tare of the transducer, as measured at the Hysitron factory with no probe installed, is given on the supplied transducer constants sheet. The value given in the software will be slightly more negative due to the mass of the probe but should be similar to the value given on the supplied sheet. The Tare value can be updated whenever the system is not performing a test or in contact with a sample surface by clicking the Updatebutton.

Lateral Tare The Lateral Tare parameter is similar to the Tare parameter given above but this is a measure of the rest position of the transducer scratch axis (if equipped). Because the lateral rest position can vary greatly based on transducer leveling (and other factors which do not affect system performance) there is no suggested value for the Lateral Tare and this parameter is primarily used for troubleshooting, if necessary.

ADC Calibration The ADC Calibration is used to calibrate the data acquisition boards and the associated gains within the Hysitron control unit. The ADC Calibration is only required to be performed once for each system (typically during the initial installation) but can be performed as frequent as desired to confirm that the gain settings are accurate.

Lock-in Input Gain The Lock-in Input Gain is available for instruments equipped with nanoDMA and/or Modulus Mapping. The Lock-in Input Gain parameter determines the gain on the AC signal being input into the lock-in amplifier. The default setting is 100, if the AC signal displacement amplitude is greater than about 300 nm, this gain should be set to 10. If the first point in the nanoDMA test is greater than about 300 nm, the gain will automatically adjust to 10 for the duration of the test.

Modulus Mapping Low Pass Filter

The Modulus Mapping Low Pass Filter is available for instruments equipped with Modulus Mapping and is used to reduce the speed of the feedback loop between the transducer and TriboScanner piezo scanner to prevent the scanner from attempting to correct for oscillations being performed by the nanoindentation probe. This option should be enabled for Modulus Mapping and disabled for all other testing routines.

Indentation Axis Electrostatic Force

The Electrostatic Force (F) is a property of the transducer that is calibrated during the Indentation Axis Calibration. The Electrostatic Force (F) is calculated with the voltage applied (V), distance between the center plate and lower plate (d), permittivity of free space (ε), and area of the plates. The Electrostatic Force parameter will be approximately 0.03 μN/V2 but varies by transducer model.

Indentation Axis Plate Spacing

The Plate Spacing is the distance between the center plate of the transducer and the lower drive plate. The default setting is 80 μm but will be calibrated during the Indentation Axis Calibration and will vary slightly with ambient temperature/humidity as well as probe mass.

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Calibration Tab

Scratch Axis transducer constants are given for all transducers but are only required to be entered or calibrated for lateral force transducers. If the transducer being used is a normal force only or nanoDMA transducer any transducer constants associated with the scratch axis can be disregarded.

Scratch Axis Electrostatic Force

The Electrostatic Force is a property of the transducer that is calibrated during the Scratch Axis Calibration. The Electrostatic Force will be similar to the value given on the transducer constants sheet but will vary with temperature/humidity and probe mass.

Scratch Axis Plate Spacing

The Plate Spacing is the distance between the center plate of the transducer and the drive plate nearest to the transducer probe. The default will vary based on transducer but should be entered from the transducer constants sheet, will be calibrated during the Scratch Axis Calibration and will vary slightly with ambient temperature/humidity as well as probe mass.

Displacement Offset The Displacement Offset indicates the amount that the probe is offset from the center position of the transducer when the system is in Indent mode. This value is given following the Lateral Axis Calibration but is not used for any data analysis or collection purposes and is used primarily as a troubleshooting value. This value should typically be near zero (any value less than about +/-10 μm should be reasonable).

If the instrument is equipped with nanoDMA testing, nanoDMA transducer constants will be given for all transducers but are only required to be entered or calibrated for nanoDMA transducers. If the transducer being used is a normal force only or lateral force transducer, any transducer constants associated with nanoDMA can be disregarded.

nanoDMA Spring Constant

The Spring Constant parameter is for nanoDMA transducers only and is given in N/m. The Spring Constant is calibrated with the nanoDMA Calibration and is calculated based on the properties of the spring assemblies within the transducer. The default Spring Constant is around 150 N/m for nanoDMA I transducers and around 300 N/m for nanoDMA II & III transducers (most common).

nanoDMA Mass The Mass parameter is for nanoDMA transducers only and is given in milligrams. The Mass is calibrated with the nanoDMA Calibration and is calculated based on the properties of the mass of the center plate of the transducer with the probe installed. The default Mass is around 220 mg for nanoDMA I transducers and around 440 mg for nanoDMA II & III transducers (most common).

nanoDMA Damping The Damping parameter is for nanoDMA transducers only and is given in kg/s. TheDamping is calibrated with the nanoDMA calibration and is a calculated property of the springs within the transducers. The default Damping for nanoDMA I, II & III transducers is approximately 0.004 kg/s.

Calibrations for the individual components of the transducer are performed by selecting the corresponding Calibrate

button under the Transducer Calibrations heading.

The calibration process will be discussed in the System Calibrations section of this user manual.

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Stage Calibration Sub Tab

2.8.2 STAGE CALIBRATION SUB TABThe Stage Calibration sub tab contains the calibrations necessary for the motorized X, Y, and Z-axis stage

components. The Stage Calibration sub tab contains calibrations for the top-down optical camera systems (Optic-

Probe Tip Offset Calibration and Optical Zoom calibration). The Stage Calibration sub tab is given in Figure 2.65. A

description of the functions within the Stage Calibration sub tab is given below.

Figure 2.65 Stage Calibration sub tab

The Stage Calibration sub tab, in addition to the necessary stage and optical camera functions, also contains a copy of the video window, stage navigation pad, and current sample boundaries from the Sample Navigation tab.

OPTICAL ZOOM CALIBRATIONThe Optical Zoom calibration is available from the Setup Calibrate Optics Zoom menu. The Optical Zoom

calibration accounts for any shift that may occur when the optical column is adjusted between zoom factors and also

calibrates the distances measured from the optical image. The Optical Zoom calibration process will be discussed in

the System Calibrations section of this user manual.

It is important to note that the Optic Zoom calibration is not required for precise positioning of the probe (this is accomplished through the Optic-Probe Tip Offset calibration).

XY STAGE MOVE LIMITS CALIBRATION

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The XY Stage Move Limits command (Setup Calibrate Stage XY Move Limits) will move the X/Y axis to the

end of the available travel in all directions and properly update the stage boundaries as needed. This command is

typically only required upon a new software installation or other advanced hardware changes.

HOME X, Y, & Z AXISThe Home X & Y Axis or Z Axis command (Setup Home X & Y Axis or Home Z Axis) moves the X, Y, and

Z axis back to the home position (0.0, 0.0) or just the Z axis as defined by the hardware flags within the stage

electronics. To prevent the Z-axis from hitting any sample, the Z-axis is homed first, followed by the X and Y axis

(when selecting the Home X & Y Axis command). The Home Z Axis command is typically used following an

emergency stop.

NAVIGATION SPEEDSThe Navigation Speeds command (Setup Navigation Speeds) opens the Set Speeds window (Figure 2.66).

To change the speed of the four TriboScan preset speed identifiers (coarse, medium, fine and ultra fine) move the

slider bar on the left to the desired speed and then either type in a new value for the speeds or use the slider bars on

the right to select the new speed setting.

The four preset speed identifiers correspond to the four levels of stage speeds around the X/Y axis stage move pad

and the Z axis move bar. The speeds can be reset to the default settings by selecting the Set Default button. The

default stage speeds typically work well for most users and testing applications. Modifying the stage speeds is

primarily a personal preference and will have little affect on the collected data.

TI 980/950 TriboIndenter systems X/Y axis stage speeds may not exceed 10 mm/sec and TI Premier systems X/Y-

axis stage speeds may not exceed 0.4 mm/sec. The maximum Z axis stage speed for TI 980/950 TriboIndenter and

TI Premier systems is 2 mm/sec

Figure 2.66 Set Speeds window

In order to maintain the accuracy of the X/Y and Z-axis stages, the coarse speed cannot be increased passed the 100% setting from the Set Speeds window.

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MOTORSThe Motors command (Setup Motors) is used to force the stage motors to stay on or power off following stage

moves. It is recommended to leave the default as Motor Off After Moves in order to minimize system drift due to

thermal variance.

RESPONSE CHECKThe Response Check command (Setup Response Check Allow Continue) allows the user to determine if the

system can continue to operate even after receiving a Transducer Response Check error from the software. This error

would normally indicate there is a problem with a cable connection, transducer constant parameter, or other

hardware/software setting that can easily cause damage to the system if ignored so it is strongly suggested to leave

this option deselected unless instructed by a Hysitron service engineer.

! To avoid system damage it is strongly suggested to leave the Response Check enabled (deselected) for normal system operation.

ADJUST OPTIC-PROBE TIP OFFSET CALIBRATIONThe Adjust Optic-Probe Tip Offset Calibration command (Setup Adjust Optic-Probe Tip Offset) can be used to

modify the Optic-Probe Tip Offset calibration (discussed in the System Calibrations section of this user manual).

Typically it is only required to modify this calibration if the system is using a non-standard probe or very low force

transducer. If the system is unable to complete the Optic-Probe Tip Offset calibration successfully contact a Hysitron

service engineer for suggestions to manually adjust the calibration with this command

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Tip Calibration Sub Tab

2.8.3 TIP CALIBRATION SUB TABThe Calibration tab Tip Calibration sub tab contains the tools required for calculating, saving and opening

nanoindentation probe area function information.

The process for calibrating a more is more involved and requires knowledge of how to perform a test on a sample and analyze data. Because of this the process for performing a probe calibration is covered in the Analysis section of this user manual.

Figure 2.67 Define sub tab

There are two sub tabs within the Tip Calibration sub tab. The Define sub tab (Figure 2.67) is intended to be used to

view the currently defined probe area function or for opening a previously saved probe area function. The Calculate

sub tab is used for calculating a new probe area function (discussed in the System Calibration section of this user

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manual). By default, the probe currently loaded in the Define sub tab any system test is performed will be used for

fitting routine for that data (unless otherwise specified).

Most parameters on the Define sub tab are populated when calculating the probe area function and will be discussed

in the System Calibration section of this user manual.

2.8.4 MACHINE COMPLIANCE SUB TABThe measured displacement of depth sensing indentation instrument is the sum of the indentation depth into the

specimen and the displacement associated with the measuring instrument, otherwise known as machine compliance.

It is important that machine compliance be properly measured for the instrument because, especially at high forces,

the machine compliance of the system can be a significant amount of the total displacement.

There are many factors which can affect the machine compliance of a system. The most common factors include:

Transducer Different transducers have varying amount of compliance. The bridge on lateral axis transducers makes them more compliant than 1D transducers. In general, stiffness of the center plate, or thickness of epoxy holding parts together can cause different amounts of compliance.

Probe Nanoindentation probes are handmade, so depending on the amounts of epoxy, or lengths of the shank on the probe, the compliance induced by the probe may vary.

Sample Mounting Depending upon the sample mounting method, additional compliance may be introduced into the system. Never use a soft material, such as putty or double-sided tape to mount a sample. If a thin layer of stiff glue or epoxy is used, the added compliance is typically negligible.

Transducer Mounting The transducer must be mounted to the TriboScanner in the same way each time. The transducer should also be level, and seated as well as possible.

Using the above guidelines, the machine compliance can be checked for each transducer and type of probe/sample

stage configuration. The machine compliance calibration can be performed in conjunction with calculating the probe

area function and is discussed further in the System Calibrations section of this user manual.

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Figure 2.68 Machine Compliance sub tab

2.8.5 IN-SITU SUB TABThe in-situ sub tab (Figure 2.69) displays the current TriboScanner piezo scanner calibration file as well as the X, Y,

and Z Piezo Gain values and Max Scan Size (all calculated during the scanner calibration and initially supplied with

any system equipped with a TriboScanner piezo scanner). Figure 2.69

in-situ sub tab

The Do Scanner Calibration button will initiate the scanner calibration process and will be discussed in the System

Calibrations section of this user manual.

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2.8.6 AUTO CALIBRATION SUB TABThe Auto Cal sub tab (Figure 2.70) is available with all TI series systems. The Auto Cal sub tab contains information

and parameters that define how the automatic calibration procedures will be performed.

More detail, including a definition of the parameters, regarding the Auto Cal sub tab can be found in the Calibration

section of this user manual.

Figure 2.70 Auto Cal sub tab

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Preferences Tab

2.9 PREFERENCES TABThe Preferences tab contains parameters regarding the movement of the X, Y, and Z axis stages, sample tilt and

approach parameters, piezo scanner attenuation, settle time, approach gains and any applicable optical camera

settings.

! It is recommended that only users familiar with the advanced operation of the Hysitron system modify parameters within the Preferences tab.

The Preferences tab contains two sub tabs: Table and Piezo. The two sub tabs are discussed in the following pages.

2.9.1 TABLE SUB TABThe Table sub tab contains parameters regarding the movement of the X, Y, and Z axis stages as well as sample tilt

and approach parameters. A description of the parameters given in the Preferences sub tab are given below:

XY Speed Between Optic and Tip

The XY Speed Between Optic and Tip parameter is defined as the speed of the X and Y stages while moving from the optical focus to the probe in-contact position. This parameter also defines the speed of the current optical position to a new optical position when moving between sample boundaries (by right-clicking between sample boundaries).

Z Speed Between Optic and Tip

The Z Speed Between Optic and Tip parameter is defined as the speed of the Z stage while moving from the optical focus to the location when the probe is over the sample area of interest. This parameter also defines the speed of the current optical position to a new optical position when moving between sample boundaries (by right-clicking between sample boundaries).

Z Withdraw Speed From Sample

The Z Withdraw Speed from Sample parameter is defined as the speed of the Z stage while the probe is moving from the in-contact position back to the Z safety height.

Z Approach Speed to Sample

The Z Approach Speed to Sample parameter is defined as the approach speed of the Z stage from the sample safety height to the probe in-contact position.

Z to Safety Speed The Z to Safety Speed parameter is defined as the approach speed of the Z stage from the starting position (focus height) downward to the Z safety height. When the system reaches the Z safety height, the Z Approach Speed to Sample parameter is used for the final approach.

Maximum X Speed The Maximum X Speed defines the maximum allowable speed for the X stage.

Maximum Y Speed The Maximum Y Speed defines the maximum allowable speed for the Y stage.

Maximum Z Speed The Maximum Z Speed defines the maximum allowable speed for the Z stage.

X Motor Acceleration The X Motor Acceleration defines the acceleration rate for the X stage.

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Preferences Tab

Y Motor Acceleration The Y Motor Acceleration defines the acceleration rate for the Y stage.

Z Motor Acceleration The Z Motor Acceleration defines the acceleration rate for the Z stage.

Sample Surface Tilt The Sample Surface Tilt is a sample property that is used to help reduce the likelihood of a probe crash when engaging the probe in different areas of the sample. The Sample Surface Tilt functions by assuming a certain amount of tilt (1 degree is the default) upward in every direction from the last contact position of a sample boundary. The Sample Surface Tilt value is calculated and added to the Z Refined Back Off Distance to yield the new Z safety height of the sample for the next approach.

Z Disengage Distance From Sample

The Z Disengage Distance From Sample defines the height of the probe disengage while using the Disengage command from the Imaging tab. The Z Disengage Distance From Sample is also defined as the disengage height used within the patterns of an automated method.

Z Refined Back Off Distance

When defining a new sample boundary, the Z Refined Back Off Distance parameter is added to the Z sample height (as determined from the optical focus). This component in addition to the Sample Surface Tilt parameter defines the approach height when the first sample approach is performed.

Z Back Off for Coarse Z Safety

The Z Back Off for Coarse Z Safety parameter is used whenever a previously saved workspace is opened (including when the software is restarted). The Z Back Off for Coarse Z Safety value is added to the last known contact height to yield the new Z safety height (height at which the Z Approach Speed to Sample is started) for the sample. This is to help prevent sample crashes following reloading a workspace when sample heights may have changed slightly with respect to time, temperature, or humidity.

Z Calibration Contact The Z Calibration Contact is a non-editable parameter (displayed for the users information) that is defined as the Z stage height of the probe during the Optics-Probe Tip Offset (H-Pattern) calibration.

Z Calibration Focus The Z Calibration Focus is a non-editable parameter (displayed for the users information) that is defined as the Z stage height of the optics during the Optics-Probe Tip Offset (H-Pattern) calibration.

Z Approach Offset The Z Approach Offset is a non-editable parameter (displayed for the users information) that is defined as the difference between the Z Calibration Contact and the Z Calibration Focus plus the Z Back Off For Coarse Z Safety.

Approach Auto E-Stop Recover

The Approach Auto E-STop Recover option (when enabled) allows the system to recover from an emergency stop if it occurs during the sample approach. If the system detects an emergency top while moving to the Z axis safety height the system will retract the Z axis stage until the emergency stop clears and then begin the sample approach process until sample contact has been achieved. The default setting is off (which requires manual emergency stop clearing).

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Preferences Tab

The default settings of the Table sub tab work very well for most samples and testing routines, however, it may be

necessary to modify values slightly for very specific testing situations. The default settings for the Table sub tab are

given in Table 2.A:

Table 2.A Table sub tab default

parameters

2.9.2 PIEZO SUB TABThe Piezo sub tab contains parameters regarding the feedback settle times and approach gains of the piezo scanner.

Only experienced users that are very familiar with Hysitron system operation should adjust parameters within the

Piezo sub tab. A description of the parameters given in the Piezo sub tab are given below:

Motor Settle Time The Motor Settle Time defines the time for the instrument to settle before performing a test from the optical focus position. Tests performed from the in-situ SPM imaging position will not perform this settle time. The settle time values are very important to instrument stability and data reproducibility. Because of this, it is recommended to leave this value somewhere near the default unless the users is experienced and has very specific testing needs (such as very soft samples, for which the settle times would be much reduced).

TI 980/950 TriboIndenter TI Premier

XY Speed Between Optic and Tip (mm/sec) 10.000 4.500

Z Speed Between Optic and Tip (mm/sec) 1.000

Z Withdraw Speed From Sample (mm/sec) 0.050

Z Approach Speed to Sample (mm/sec) 0.001000

Z to Safety Speed (mm/sec) 0.500

Maximum X Speed (mm/sec) 10.000 4.500

Maximum Y Speed (mm/sec) 10.000 4.500

Maximum Z Speed (mm/sec) 1.000

X Motor Acceleration (mm/sec2) 10.0 5.0

Y Motor Acceleration (mm/sec2) 10.0 5.0

Z Motor Acceleration (mm/sec2) 1.000

Sample Surface Tilt (deg) 1.00

Z Disengage Distance From Sample (mm) -0.10000

Z Refined Back Off Distance (mm) 0.01000

Z Back Off for Coarse Z Safety (mm) 0.20000

Z Calibration Contact (mm)* transducer/probe dependent (not editable)

Z Calibration Focus (mm)* transducer/probe dependent (not editable)

Z Approach Offset (mm)* transducer/probe dependent (not editable)

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Piezo Settle Time The Piezo Settle Time defines additional time for the instrument to settle (especially to help reduce piezo wander and hysteresis). All tests performed from the optical focus position and the in-situ SPM Imaging tab performs this settle time. The settle time values are very important to instrument stability and data reproducibility. Because of this, it is recommended to leave this value somewhere near the default unless the users is experienced and has very specific testing needs (such as very soft samples, for which the settle times would be much reduced).

Approach Z Piezo Attenuation

The Approach Z Piezo Attenuation defines the amount of extension for the Z piezo tube during the initial sample approach or any sample Quick Approach. Increasing the Approach Z Piezo Attenuation will have little effect, decreasing the Approach Z Piezo Attenuation will reduce the Z piezo ability to stop in a timely manner after contacting the sample surface.

Approach Integral Gain Standard/Rapid

Probe

The Approach Integral Gain Standard/Rapid Probe defines the integral gain (how well the probe maintains contact with the sample surface) during the initial approach for the three-plate capacitive transducer and RapidProbe transducer. Tuning this gain too high will result in ringing and possible emergency stop issues. Tuning this gain too low will reduce the ability of the piezo scanner to respond in a timely manner.

The default settings of the Piezo sub tab work very well for most samples and testing routines, however, it may be

necessary to modify values slightly for very specific testing situations. The default settings for the Piezo sub tab are

given in Table 2.B:

Table 2.B Piezo sub tab default

parameters

PHASE APPROACHThe phase approach options allow the user to set the system to use a measured phase change (as opposed to measured

setpoint force) to perform the probe to sample approach. A phase approach can be significantly more sensitive to

finding the sample surface with very soft samples. To use the phase approach, place a check in the Phase Approach

check box and enter the Phase Approach Threshold for the approach to identify the sample surface.

The Phase Approach Setup button opens the lock-in amplifier settings to allow the user to define the probe amplitude

and frequency during the phase approach.

TI Series Systems

Z Motor Settle Time (sec) 60.0

Z Piezo Settle Time (sec) 45.0

Approach Z Piezo Attenuation (%) 90

Approach Integral Gain Standard/Rapid Probe 90.0000

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Preferences Tab

2.10 HYSITRON CUSTOMER SUPPORT SITE & THE ABOUT TABThe About tab contains information about the TriboScan software version number, any associated National

Instruments data acquisition version numbers, stage control unit, and software engine revision numbers. The

information provided in the About tab (especially the TriboScan version number) is often very useful to provide to the

customer service engineer when calling for assistance.

Hysitron customer support email: [email protected]

Hysitron customer support phone: +1-952-835-6366

Hysitron now offers an extensive online customer support site. Go to:

https://support.hysitron.com

to request a login username and password to access the Hysitron customer support site (you can also email

[email protected] to request a login username and password). The Hysitron customer support site offers live

online chat with support representatives, downloadable documentation, and hundreds of knowledgebase articles to

assist with common issues and testing routines.

Figure 2.71 Hysitron customer support

center website

Double left-clicking on the TriboScan in the first line of the information in the About tab will display the current features installed and licensed on the system.

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TI Series System Calibrations

SECTION | TI SERIES SYSTEM CALIBRATIONS

• System calibrations and procedures for maintaining a properly operating system

• Frequency of system calibrations and other maintenance items

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CHAPTER 3 CALIBRATIONS

System calibrations are important to maintain a properly operating Hysitron system. This section will discuss the

system calibrations and other regular maintenance items. The user should be familiar with the TriboScan software

operation presented in the previous section before proceeding.

The System Calibrations section requires the user be familiar with the TriboScan software as presented in the previous Software section of this user manual.

3.1 LOADING A TRANSDUCER CONSTANTS FILEWhen a new transducer is first used, a transducer constants file should be created. A new transducer constants file can

be created from the Calibration tab System Calibration sub tab. To create a new file, select File Save as and

create a new file name. Each transducer constants file will display the indentation and lateral axis calibration data. If

the transducer being used is a 1D (indentation axis only or nanoDMA) the X axis (lateral axis) constants are unused

and may be ignored.

If a transducer constants file has already been created for the transducer, it can simply be loaded from the Calibration

tab System Calibration sub tab, select File Open.

After a transducer constants file has been loaded or created, the proper constants can be copied from the transducer

constants sheet provided with the transducer and then fine-tuned with the respective calibration(s).

TRANSDUCER CONSTANTS SHEETA unique transducer constants sheet is produced each time a transducer is calibrated at the Hysitron factory. An

example transducer constants sheet for a lateral axis transducer is given in Figure 3.1.

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Figure 3.1 Example transducer constants

sheet

There are two common parameters that appear on the transducer constants sheet that are not discussed in the System

Calibration sub tab section of this user manual:

Self Calibration Check The Self Calibration Check is a troubleshooting tool to verify that the springs that suspend the center plate of the transducer have not been damaged since the transducer has been calibrated. The Self Calibration Check is performed by viewing the tare value of the transducer then pausing TriboScan, turning the transducer upside-down, un-pausing TriboScan and viewing the tare value. The Self Calibration Check value should be the difference between these two measured tare values. It is unnecessary to perform the Self Calibration Check unless instructed by a Hysitron service engineer.

Displacement Range The Displacement Range is the maximum scratch length that was measured at Hysitron with the given transducer. The Displacement Range may change over time or may vary with different probes installed.

Upon entering or changing any values in the System Calibration sub tab, the file will be saved to the currently open

transducer constants file (the file path is given at the top of the System Calibration sub tab). Different calibration files

can be accessed by clicking the Open icon and a new file can be created by clicking the Save As icon.

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3.2 TARE VALUE VERIFICATIONThe tare value of the system can be read at any time the nanoindentation probe is not in contact with a sample surface.

Verifying the tare value is approximately the value given on the supplied transducer constants sheet (typically located

within the black transducer case) after the components are installed and TriboScan has been started indicates that the

transducer and probe are installed correctly and the connections are secure.

To read the tare value of the system, click the Calibration tab System Calibration sub tab and click the Update

button under the System Parameters heading (Figure 3.2). The tare value will be displayed in the parameter box to the

right of the Update button.

Figure 3.2 Location of Update button and

verification of tare value

The observed tare value is typically higher (more negative) than the value on the transducer constants as the recorded

value was taken with no probe installed. If different probes are used with the system it can be expected that the tare

value will vary.

The tare value of the system should be verified each time the Hysitron control unit is powered on or any hardware components have been removed, replaced or modified.

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A tare value reading that is positive, zero or greater than approximately ± 50 mg from the recorded value indicates that there may be a problem with the transducer or probe installation. If the tare value reading is not in agreement with the transducer constants sheet, reinstall the nanoindentation probe. Many times an incorrect tare value reading is caused by a poorly mounted probe.

3.3 ADC CALIBRATIONThe Hysitron DSP-based controller requires an ADC calibration in order to calibrate the data acquisition boards and

the associated gains within the Hysitron control unit. The ADC calibration is only required to be performed once for

each system configuration (typically performed during the initial installation) but can be performed as frequent as

desired to confirm that the gain settings are accurate.

The ADC calibration is accessed from the Calibration tab System Calibration sub tab ADC Cal button. After

selecting the ADC Cal button the system will automatically perform the ADC calibration and generate the DSP

Calibration Results window (Figure 3.3).

Figure 3.3 DSP Calibration Result window

Within the DSP Calibration Results window there will be one tab for each of the installed data acquisition cards

within the Hysitron control unit (the number of data acquisition cards depends on the instrument options and

upgrades). The Measured Gain values on all tabs should be -1 ± 0.004. The Measured Offset values should be near

zero (less than 10-3). The Gain Value and Offset Value are not used for the ADC calibration and the listed values are

unimportant. If any of the values within the DSP Calibration Result are not within the given range (values out-of-

range will be RED) contact Hysitron for further instruction.

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! Do not perform the ADC calibration while the probe is on the sample surface.

Table 3.A Installed data acquisition cards

by instrument configuration

If the system has nanoDMA and is using an external SR 830 lock-in amplifier an Auxiliary I/O Board 3 will be required. Other options may require additional boards or wire harnesses.

3.4 INDENTATION AXIS CALIBRATIONThe Electrostatic Force Constant for the Hysitron three-plate capacitive transducer is determined by the area of the

drive plate, the area of the center electrode and the distance between the two squared. Because the center plate of the

transducer is floating on springs, the spacing between the plates can change and thus change the Electrostatic Force

Constant.

During an indentation test, the center plate (to which the probe is attached) of the transducer is driven into the sample

surface. This movement of the center plate will cause a fluctuation in the Electrostatic Force Constant and if the

transducer has not been properly calibrated a significant amount of error may be present in the results.

TriboScan automatically accounts for changes in the Electrostatic Force Constant at large displacements. However,

in order to make this correction, TriboScan must know the Plate Spacing of the transducer. The Plate Spacing and

Electrostatic Force Constant are given by performing the Indentation Axis calibration (a contact-free actuation of the

transducer).

It is important that the Indentation Axis calibration be performed every day or each time the instrument is used,

whichever comes first. The Electrostatic Force Constant is likely to vary slightly from day to day based on factors

such as a change in temperature or humidity. Additionally, the Indentation Axis calibration is a good indication that

the system is working properly and the components are connected securely.

TI Series Base System 3D OmniProbe/MRNP Transducer Option

nanoECR Option

Transducer I/O Board 1 X X X

Transducer I/O Board 2 X

Auxiliary I/O Board 3 X

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3.4.1 PERFORMING THE INDENTATION AXIS CALIBRATIONThe Indentation Axis calibration is performed with the nanoindentation probe installed in the transducer and the

transducer installed in the instrument. The Indentation Axis calibration will be performed in the air, far from any

sample so it is important that there is adequate space between the nanoindentation probe and any samples or the

sample stage.

The transducer is carefully calibrated at Hysitron prior to shipment and will be supplied with a constants sheet. The

constants given on the supplied transducer constants sheet must be entered into the System Calibration tab. A brief

definition of the parameters given on the Calibration tab System Calibration sub tab is discussed in the previous

section.

Figure 3.4 Verification of indentation axis

transducer constants

With the transducer constants correctly entered, click the Calibrate button located under the Indentation Axis heading

given in Figure 3.4 to begin the Indentation Axis calibration process.

Upon selecting the Calibrate button, the system will automatically open the Load Function tab Indentation sub tab

(Figure 3.5).

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Figure 3.5 Indentation Axis calibration load

function

When the system is in the Indentation Axis calibration mode, the user can double right-click on the Cal Air Indent button to return to normal system operation.

Verify that the current load function is the Indentation Axis Calibration.ldf. The Peak Force will vary with the

transducer calibration values but it is typically around 600-800 μN for a three-plate capacitive transducer and 1000-

1400 μN for a nanoDMA transducer (a lower Load Scale Factor typically requires a higher force to achieve the same

actuation displacement). The force defined for the Indentation Axis calibration should achieve a displacement of

approximately 3-4 μm. Click the Cal Air Indent button and the Indentation Axis calibration reminder window

(Figure 3.6) will open. Click Start to continue with the calibration.

Figure 3.6 Indentation Axis calibration

reminder window

Upon clicking Start in Figure 3.6, a contact-free indentation test will be performed and the real-time plot will be

displayed similar to Figure 3.7

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Figure 3.7 Real-time indentation plot for

the Indentation Axis calibration

When the real-time plot has finished, Figure 3.8 will open prompting the user to keep or discard the calibration

information. If the calibration has been performed successfully, click YES. If a setting was overlooked and the

calibration was unsuccessful, click NO, locate the source of the unsuccessful calibration and re-perform the

Indentation Axis calibration starting from the beginning of this procedure.


confirmation window

After clicking YES in Figure 3.8 the ESF versus displacement plot (Figure 3.9) will open to show the actual data

collected during the Indentation Axis calibration (shown in red) with respect to the fitted linear plot (shown in blue).

The red plot should be very close to the blue plot and the total displacement should be approximately 3 - 4.5 μm. Any

significant deviation between the two plots will result in a poor calibration and may indicate further problems within

the transducer or other system components.

Displacements greater than about 4.5 μm may be exceeding the transducer displacement limit and the calibration

should be performed at a lower force. Displacements less than about 3 μm typically have not exercised the sensor

enough to collect a reasonable amount of displacement data for the calibration. Typically, very low displacement

calibrations will appear much noisier due to the reduced calibratable range.

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Figure 3.9 Indentation Axis calibration ESF

vs. displacement plot

Depending on the version of software an RMSE plot (to quantify the quality of the fit) may be given below the ESF

versus displacement plot. The RMSE should be less than 5 10-5.

! Do not attempt to approach a sample for testing without first obtaining a satisfactory Indentation Axis calibration and ESF versus displacement plot.

The Indentation Axis calibration will finish with the result being displayed in the Analysis tab Quasi sub tab. The

result should be a scatter of data points around 0 μN and a displacement of between 3 - 4.5 μm (Figure 3.10).

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result

The Indentation Axis calibration is now complete and the user can proceed with additional calibrations (if necessary,

depending on the instrument features) or continue with sample testing.

3.5 LATERAL AXIS CALIBRATIONNanoscratch testing is an upgrade option available for the TI series systems. The nanoscratch option requires a

transducer upgrade to include lateral axis sensors. Contact Hysitron if you are unsure if your transducer has this

capability or for upgrade information.

Just as the Indentation Axis calibration was required to calibrate the indentation axis of the transducer there is an

analogous calibration required for the lateral axis. The Lateral Axis calibration is only required if nanoscratch testing

will be performed and is not required for standard indentation testing with a lateral axis transducer. This calibration

should be performed daily before any scratch testing is begun or any time the transducer is removed, replaced and

scratch testing will be performed.

The Lateral Axis calibration is only intended for transducers equipped with a lateral axis.

PERFORMING THE CALIBRATIONTo perform the Lateral Axis calibration follow the procedure below:

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1. Click the Mode pull-down menu at the top of the TriboScan software to select Scratch.

2. Go to the Calibration tab System Calibration sub tab and verify that the lateral (X) axis transducer constants match the values on the transducer constants sheet (do not change any indentation (Z) axis constants as they have already been calibrated with the Indentation Axis calibration).

3. Click the Calibrate button under the Scratch Axis heading.

4. When the scratch load function editor window opens, ensure that the currently open load function is the scratch axis calibration.scf

5. In the lower right corner click the Cal Air Scratch button and follow the on-screen prompts to perform the Lateral Axis calibration.

6. Following the Lateral Axis calibration (after the user accepts the calibration results), the software will automatically calculate the lateral axis transducer constants and fill in the new values on the Calibration tab System Calibration sub tab Transducer Calibrations heading Scratch Axis sub heading. The lateral axis calibration is now complete.

With the completion of the Lateral Axis calibration, the data that is of interest is the lateral force versus time data. To

verify a satisfactory Lateral Axis calibration, the bulk of the data should fall within a range of about 10 μN on the

lateral force versus time plot. In the example shown in Figure 3.11 the calibrated data falls within a range of about

5 μN.

If the user is attempting to set up a standard nanoscratch test and the system is currently in the Lateral Axis calibration mode, double right-click on the Cal Air Scratch button to exit the Lateral Axis calibration mode and return to the standard nanoscratch load function mode.

Figure 3.11 Lateral Axis calibration result

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3.5.1 NOTES ON LATERAL AXIS RANGEThe lateral axis transducer consists of an indentation sensor suspended by two, identical, lateral sensors. The center

plate is electrostatically attracted towards the drive plate so when the center plate moves, the distance between the

drive plate and center plate is reduced, causing an increase in the electrostatic force. In order for the software to

compensate this change, the exact plate spacing must be found for the transducer by performing the Lateral Axis

calibration with no resistance (in the air). Knowing the plate spacing, the software can make the required corrections

to compensate for the changing force constant.

When the plates reach a critical distance, the force constant becomes too high, causing the plates to snap together. The

control loop will attempt to compensate for this by reducing the force to zero and the system may then become

unstable or oscillate. This typically happens well before the maximum physical displacement of the transducer has

been reached. Inside the sensors, used to create the lateral axis transducers, there are plate spacings of approximately

70-100 µm. This means that the total physical travel that can be allowed in the scratch axis will be physically limited

to this amount. The typical range for a transducer is ±25 µm when operated in air. The usable range that is linear and

can be calibrated is typically much shorter than this (around 10-15 µm).

The range of operation of the transducer can be found by making a long scratch in the air. At the point where the

plates snap together, the lateral axis signal will change dramatically and either begin to oscillate or become a large

magnitude number.

3.5.2 TRANSDUCER BREAKPOINTThe other critical point in the lateral axis transducer occurs when a scratch switches from one drive plate to another.

When the center plate moves through its natural rest position, the voltage on the drive plate moving the center plate

goes to zero, and the other drive plate begins to control the center plate. Because the voltage on both plates goes to

zero for an instant, the control loop loses operation of the force and a breakpoint appears on the lateral displacement

signal of the scratch. Usually this is within several microns of the zero point of the transducer, where the measured

capacitance is zero.

The breakpoint appears as a flattened region on the result curve and can be seen on the lateral displacement plot in the

Analysis tab Scratch sub tab. The position of the breakpoint may be slightly affected by the tilt of the transducer so

it is not uncommon to notice slight changes in the transducer breakpoint over the life of the system.

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At the transducer breakpoint, the actuation changes from one drive plate to the other. This means that the electrostatic

force constant, plate spacing, and displacement offset will change. These values will affect only the lateral axis signal

and friction measurements. If the lateral axis signal is required for analysis all scratch testing should be performed

completely on one side of the transducer breakpoint.

3.5.3 IMAGING POSITIONBecause of the transducer breakpoint discussed above, scratching through the center of the transducer will not yield

quantitative results for friction or lateral axis measurements. For this reason (and also to keep the tested location at

the center of the current in-situ image) the Imaging Position was introduced as a lateral axis transducer constant. The

Imaging Position is the position that the probe will be held at when the transducer is not performing a nanoscratch

test and the Mode pull-down menu (located at the top of the TriboScan window) is switched to Scratch. The Mode

pull-down menu controls the rest position of the probe (at the imaging position if set on Scratch and at the natural

zero position if set to Indentation).

3.5.4 OPTIMIZING THE IMAGING POSITION PARAMETERThe Imaging Position has been optimized at Hysitron during calibration. However, over time the Imaging Position

may change if the transducer is tilted when mounted or if the springs become slightly bent. The Imaging Position

typically will only vary by a few microns. If short scratches are being made (less than 6 µm) the value on the

transducer constants sheet should be sufficient. If longer scratches are being made or if the Lateral Axis calibration

will not calibrate linearly then the user may have to optimize this the Imaging Position parameter.

The Imaging Position is set to the center of the longest linear range of the transducer. By finding the critical

parameters discussed above (the maximum and minimum displacement ranges, and the breakpoint), the user can

determine the best location for the Imaging Position. The three linear ranges that are seen with the lateral axis

transducer:

• Negative range to zero position OR negative range to breakpoint• Zero position to breakpoint OR breakpoint to zero position• Positive range to zero position OR positive range to breakpoint

With the Imaging Position on the System Calibration sub tab set to ‘0’, perform an air scratch using the

scratch axis calibration.scf scratch load function file adjusted for a minimum and maximum scratch lateral scratch

distance of -25 µm and +25 µm, respectively. By examining the resulting data file, the largest linear segment can be

located. To allow for the greatest lateral movement, the lateral displacement value at the center of this segment should

be the new Imaging Position value. Enter this value in the System Calibration sub tab.

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The Mode pull-down menu cannot be changed while the system is performing an in-situ image (the probe must be disengaged and re-engaged). To save time, the user should decide which mode will be used prior to engaging a surface for imaging.

When the Mode pull-down menu is toggled between indentation and scratch, the probe will be shifted by the value listed in the Imaging Position field. This corresponds to an apparent optical shift in the Y-axis.

3.6 OPTICAL ZOOM CALIBRATIONThe Optical Zoom calibration is available from the Calibration tab Stage Calibration sub

tab Setup Calibrate Optics Zoom menu. The Optical Zoom calibration accounts for any shift that may

occur when the optical zoom is adjusted and also calibrates the distances measured from the optical image.

It is important to note that the Optic Zoom calibration is not required for precise positioning of the probe (this is accomplished through the Optic-Probe Tip Offset calibration).

The Optical Zoom calibration is only required if the physical positioning of the optical camera column has changed or

the objective lens is change (which is infrequent) so this calibration is not performed regularly.

If the user changes the objective lens to a different objective zoom factor this calibration must be performed.

The Optical Zoom calibration is performed by locating an area of interest in two different sets of reticules. The

Optical Zoom calibration is performed at 3x maginification and other zoom factor measurements extrapolated

automatically. Figure 3.12 illustrates the start of a Optical Zoom calibration with the blue reticule centered over a

large feature.

An on-screen window will prompt the user to first locate an area of interest in the blue reticule then click OK. The

user will then need to use the X, Y and Z-axis software controls to move the stages so that the same area of interest is

located in the red reticule and click OK.

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Figure 3.12 Performing an Optical Zoom

calibration

During the Optical Zoom calibration only the X and Y axis stage coordinates are saved. The Z axis coordinates are not saved as part of the Optical Zoom calibration.

If the calibration varies by more than a defined percentage of the previous calibration a warning message will appear. If the user is changing between two different objective lenses it is normal for the calibration to vary by enough to generate a warning.

3.7 XY STAGE MOVE LIMITS CALIBRATIONThe XY Stage Move Limits command (Calibration tab Stage Calibration sub tab Setup Calibrate

Stage XY Move Limits) will move the X/Y axis to the end of the available travel in all directions and properly

update the stage boundaries as needed. This command is typically only required upon a new software installation or

other advanced hardware changes.

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3.8 OPTIC-PROBE TIP OFFSET CALIBRATIONHysitron TI series instruments are optically driven instruments. With a properly calibrated instrument the user will be

able to optically focus the camera on an area of interest, define a sample boundary and perform a test. In order to

accomplish this task, TriboScan needs to record the distances in the X, Y, and Z axis between the center of the optical

focal plane and the probe. This calibration is required if any of the system hardware components related to the

distance of the probe or optics has changed. These parameters include:

• The TriboScanner is removed or changed• The transducer is removed or changed• The nanoindentation probe is removed or changed• Any of the optical camera system hardware is adjusted or changed

If any of the items in the list above occur, the Optic-Probe Tip Offset must be calibrated. Because the Optic-Probe Tip

Offset calibration is required only following certain events, the frequency of the calibration depends on how the

instrument is operated and how often the hardware components are modified.

The Optic-Probe Tip Offset calibration should only be performed after a satisfactory Indentation Axis calibration has

been performed.

! The Optic-Probe Tip Offset calibration should only be performed after a satisfactory Indentation Axis calibration has been performed. The Indentation Axis calibration is discussed earlier in this user manual.

3.8.1 AUTOMATIC OPTIC-PROBE TIP OFFSET CALIBRATIONThe Automatic Optic-Probe Tip Offset calibration is available with TriboScan 10 and later. A special ATOCW

patterned wafer sample (supplied with TI 980 TriboIndenter systems and available for purchase for other systems) is

required to complete this calibration. For most systems the Traditional Optic-Probe Tip Offset calibration (in the

following section) should be used or contact Hysitron for instrument upgrade information.

The ATOCW procedure can be used for all standard transducers and 3D OmniProbe/MRNP transducers. Transducers

with sensitivity to magnetic attraction or probes with large radius tips may need to proceed with the Traditional

Optic-Probe Tip Offset calibration.

The Automatic Optic-Probe Tip Offset calibration is available on IEEE 1394 or USB 3.0 optical camera systems running TriboScan 10 and higher. Contact Hysitron for additional information regarding this feature.

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The ATOCW is intended for probe geometries that are sharp enough to accurately measure the channels of the ATOCW patterned wafer sample (Berkovich, cube corner, and conical probes with radius less than about 10 µm).

The ATOCW can only account for small offsets in the X and Y axis calibration. If the calibration is very far from default a Traditional Optic-Probe Tip Offset calibrating will likely be required before performing the ATOCW.

The Automatic Optic-Probe Tip Offset calibration (referred to as the ATOCW [Automatic Tip Optic Calibration

Wafer] in this procedure) requires a special ATOCW patterned wafer. The patterned wafer will be about 1 mm thick

and 10 mm square with a few different patterns (identified with diagram in Figure 3.13). The ATOCW patterned

wafer has 6 spot indicators (two for each style of objective lens offered) and an X and Y range calibration region. The

X and Y range has one long channel in the center followed by short channels which increase in length when moving

toward the edges. During the calibration procedure the system is looking for the long channel (and adjacent short

channels) to identify the location on the wafer.

Figure 3.13 ATOCW patterned wafer sample

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Figure 3.14 Optical images of ATOCW

patterned wafer

The procedure for performing the ATOCW follows:

1. Install the ATOCW sample and define the entire sample boundary (including all patterns on the silicon wafer). The sample must be installed square with the optical camera image (within approximately 1° of axis).

2. Name the sample ATOCW.

3. Go to the Automation tab Methods sub tab Position side tab.

4. Under the Position Groups heading select the New button.

5. Name the position group ATOCW.

6. Move the stages to focus at the center one of the 10x, 20x, or 50x indicators depending on which objective lens is currently installed on the system (identified in Figure 3.13). The default objective lens on the TI 980/950 TriboIndenter is 20x; the default objective lens on the TI Premier is 10x.

7. Under the Positions heading select the Add Above button.

8. Under the Positions heading select the Edit button and rename the position to be one of the following (depending if you focused on the left or right indicator): ATOCW Left 20x ATOCW Right 20x

9. Repeat step 8 for the opposite indicator.

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If the system is using the 10x or 50x objective replace the 20x with 10x or 50x.

10. Go to the Preferences tab Table sub tab Approach Auto E-Stop Recovercheck box and enable the feature. This allows the system to automatically recover if the probe touches the sample during the rough positioning portion of the ATOCW.

Figure 3.15 Enable the Approach Auto E-

Stop Recover feature

11. Go to the Stage Calibration tab Tip to Optic Calibration button ATOCWbutton (Figure 3.16) to initiate the ATOCW calibration.

Figure 3.16 Initiating the ATOCW

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12. The user will be prompted to center the reticle on the image 1 pattern indicator (Figure 3.17) and click Continue then the same for image 2 pattern indicator (Figure 3.18).

Figure 3.17 ATOCW center on image 1

Figure 3.18 ATOCW center on image 2

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The system will move the probe to the X axis calibration region and perform a light force scratch across the sample

surface (using the translational stages) until the location is known from the width and location of the channels

(typically about 5 transitions in length). A real-time image will be displayed of the progress (Figure 3.19) and after

the system has identified the location the system will automatically move to the Y axis calibration region and perform

the same test in the Y axis.Figure 3.19

ATOCW real-time plot

The ATOCW real-time plot is only informational and there is no user input or adjustments available (with the

exception of a Cancel button that can be used to end the process). After the X and Y calibration is complete the Optic

Probe-Tip Offset Calibration will be complete.

If the user would like to review past ATOCW calibration results the ATOCW real-time plot saves an image of the

final result following the calibration in the C: Hysitron Data ATOCW folder.

3.8.2 TRADITIONAL OPTIC-PROBE TIP OFFSET CALIBRATIONThe Optic-Probe Tip Offset calibration is located on the Calibration tab Stage Calibration sub tab Tip to Optic

Calibration button (near the bottom left). There are two different types of Optic-Probe Tip Offset calibrations that

may be performed:

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Figure 3.20 Optic-Probe Tip Offset

calibration options

“H” Pattern Selecting the “H” Pattern option will automatically make seven indents in the shape of an H (three on each side for the legs and one in the middle). This is the simplest pattern to find and it is recommended to use this during most Optic-Probe Tip Offset calibrations. During the H pattern, the indents are spaced 15 μm apart (30 μm apart with 3D OmniProbe/MRNP transducers). In order to keep the calibration time as short as possible, no piezo settle time or drift correction is used for these tests so the collected load vs. displacement plot will likely not produce accurate hardness or modulus values.

Single Indent Selecting the Single Indent option is best if the Optic-Probe Tip Offset has only changed slightly as this will be the fastest way to update the offset. The system will perform only one indent, which may be difficult to distinguish optically from other surface imperfections. This option is also used for very large radius probes that will not be capable of creating a distinguishable H pattern.

In addition to the two types of Optic-Probe Tip Offset calibrations, there are two additional options available:

Set X & Y Offsets to Default Values

Selecting the Set X & Y Offsets to Default Values button will set the Optic-Probe Tip Offset calibration to the factory default settings. Before making the change, a window will display the default values and the software will prompt for a confirmation from the user.

Move to Previous Indent

The Move to Previous Indent button will allow the user to update the Optic-Probe Tip Offset calibration for a new zoom factor or to verify the calibration is valid. Selecting this button will move the X, Y, and Z axis stages to optically focus on the last Optic-Probe Tip Offset calibration indent pattern. This option is only valid if the sample the to the Previous Optic-Probe Tip Offset calibration was performed on is still installed in the system.

The Optic-Probe Tip Offset calibration requires that a transducer with a nanoindentation probe be installed on the system and the aluminum (001), polycarbonate, or similar smooth, soft sample be mounted on the sample stage and sample boundary defined.

1. Place the supplied (001) aluminum, polycarbonate sample, or any other smooth sample that can produce indents large enough to see optically on the sample stage and define the sample boundary as discussed in the Sample Navigation tab section of this user manual.

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2. Optically focus near the center of the sample defined in step 1.

3. Ensure that the same load function created for the Indentation Axis calibration is the current load function in the Load Function tab and the Mode pull-down at the top of the TriboScan software is set to Indentation.

4. Click Calibration tab Stage Calibration sub tab Tip to Optic Calibrationbutton (near the bottom left) “H” Pattern button (Figure 3.20).

5. The software will prompt the user that the Z Safety is disabled (Figure 3.21). This will allow the software to move in the X, Y, and Z-axis over a defined but non-approached sample space. This is okay, click OK.

Figure 3.21 Z Safety Disabled prompt

6. The software will prompt the user to enter a peak force (Figure 3.22). For the Optic-Probe Tip Offset, a displacement of around 1 μm is typically required to see the H optically. For a Berkovich probe this corresponds to 8,000-10,000 μN and for a cube corner probe this corresponds to 2,000-4,000 μN on the aluminum or polycarbonate standard sample. The 3D OmniProbe/MRNP transducer requires the user to define a maximum displacement instead of a force; the maximum displacement should be between 1500-3000 nm.

Figure 3.22 Enter force for calibration

indents prompt

Using a force that is too high may push the probe so deep into the sample surface that an excessive force is sensed while withdrawing and an emergency stop error is generated. If this occurs, manually withdraw the probe from the sample surface (yellow knob on top of the Z axis), home the Z axis and restart the Optic-Probe Tip Offset calibration using a lower peak force.

7. After a peak force has been selected click OK, the system will move the sample under the nanoindentation probe.

8. A window will prompt the user to manually (with the software Z axis motor control) lower the Z axis until the probe is approximately 1 mm above the sample (Figure 3.23).

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9. When the user has gotten sufficiently close to the sample (any height will work, the further away, the longer it will take for the calibration), click OK (Figure 3.23). The system will automatically approach the surface and make seven indents in the shape of an H.

Figure 3.23 Lower the Z-axis prompt

10. After the seven indents are complete, the system will move the area of the sample with the newly created H under the optics.

11. It is the user’s responsibility to find the H using the X, and Y axis stage controls and focus the center indent of the H in the center of the field of view as shown in Figure 3.24. The first time this procedure is run, the H pattern may not be in the current optics view and it may take some time to locate the area of interest.

12. Click OK on Figure 3.25 when the H has been found and centered in the current optics view.

Figure 3.24 H pattern on aluminum standard

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Figure 3.25 Locate the H pattern prompt

It is recommended that the user make a note of the approximate location on the sample where the probe is located when the calibration is being performed (by looking in the enclosure windows) so that the general area of the sample for the optical search is known.

When OK is clicked on the last step, the software will use the stage coordinates to calculate the offsets between the

probe and the center of the optical field of view so that future samples can be accurately approached from an optical

focus position.

If the H pattern is not visible in the current optics view, it may be helpful to use the Auto Search button (Figure 3.26).

Selecting the Auto Search button will open the Auto Search prompt (Figure 3.27). Clicking the Go button from the

Auto Search prompt will slowly move the stages in concentric squares originating from the last known Optic-Probe

Tip Offset calibration. While performing an Auto Search, it is still the users responsibility to locate the H pattern and

stop the auto search by clicking the Stop button (Figure 3.27), then center the stages over the H pattern and click OK

on Figure 3.25.

Figure 3.26 Auto Search button

Figure 3.27 Auto Search prompt

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It is recommended to perform an additional indent to mark the H pattern as being used (Figure 3.28). Performing a single indent between the legs of the H will prevent the pattern from being confused with further calibrations and verifies that the proper pattern was selected

Figure 3.28 H pattern with eight indent to

identify pattern as used

3.9 TRIBOSCANNER PIEZO SCANNER CALIBRATIONThe TriboScanner piezo scanner that is standard on all Hysitron TI series systems may require an occasional

recalibration. Piezo ceramic material inherently changes properties over time and the rate of which the changes occur

can be increased by long periods of inactivity or performing high-demand/large surface scans. Under normal

operating conditions, Hysitron recommends performing the scanner calibration annually.

Typically, the piezo scanner is recalibrated on an as-needed basis and will vary by use and desired scanning accuracy.

If the images appear to be distorted or measured dimensions seem to be incorrect the TriboScanner piezo scanner may

need to be recalibrated.

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Figure 3.29 Calibration grating scanned with

an uncalibrated (left) and calibrated scanner (right)

The recalibration of the TriboScanner piezo scanner is an involved process that, if performed incorrectly, may severely reduce the functionality of the system. It is recommended that this calibration be performed only by experienced users or under the guidance of a Hysitron service engineer.

In order to perform a TriboScanner piezo scanner calibration the user will need to acquire (not included with the

system) an X/Y axis grating with a period of around 3 μm (such as the TGX01 grating available from MikroMasch™)

and a Z axis grating with a step size of around 100 nm (such as the TGZ02 grating available from MikroMasch™).

The TriboScanner piezo scanner calibration procedure assumes that the instrument has been set up properly and all standard calibrations have been satisfactorily performed.

The following procedure should be used for calibrating the piezo scanner:

1. Place the X/Y-axis and Z-axis gratings on the sample stage and define the gratings as sample boundaries. The gratings should be aligned so that the patterns, when scanned, appear to be as perpendicular as possible.

2. Approach the X/Y-axis grating from the in-situ SPM Imaging tab and begin scanning the sample surface at a setpoint of around 2 μN, scan size of around 10 μm at a 1 Hz scan rate.

3. From the Calibration tab in-situ sub tab click the Do Scanner Calibrationbutton. The software will automatically open the modified Imaging tab in-situ sub tab (Figure 3.30).

The system will force the in-situ imaging parameters to 1 Hz scan rate and 256x256 resolution. Scan size and orientation will automatically change during calibration process.

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Figure 3.30 Modified Imaging tab with

Scanner Calibration area

4. Two different scan sizes are used during the scanner calibration. The default values are 6 μm and 20 μm. However, these scan sizes can be modified for the specific use of the piezo scanner to achieve the most accurate calibration. The default settings work very well and the user may want to contact a service engineer for advice before modifying the default scanning sizes.

5. Click the Scan at size 6.0 (or the smaller of the two user defined sizes) button. The button will turn green indicating that the scanner calibration has begun.

6. When the grating image begins to appear, using the Measure tool, the user will need to left-click at the edge of one of the gratings and drag the mouse pointer to the edge of the next grating. The measured distance will be given above the image (Figure 3.31).

Figure 3.31 Measuring the X/Y axis grating

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7. Use the Measure tool to measure the grating in both the X and Y-axis direction. If the measured distances do not correspond to the distances as given by the grating manufacturer the Adjust X and Adjust Y values must be modified.

The Adjust X and Adjust Y parameters should be modified in real-time while the system continues to scan the sample surface. Withdrawing the probe from the sample surface will terminate the scanner calibration procedure.

8. If the measured distance is too large, the adjustment value should be increased. If the measured distance is too small, the adjustment value should be decreased. An approximation of the new adjustment values can be found by using the following relationship:

9. When an appropriate measurement can be obtained in both the X and Y axis for the small scan size, click the Scan at size 20.0 (or other user defined large value) button. The system will adjust to scan at the larger scan size and steps 6 through 8 must be performed again at the larger scan size.

10. Hysitron systems are also capable of performing a vertical scan (swapped fast and slow scanning direction). Because of this the vertical scanning direction should also be calibrated. Select the Vertical Scanning check box and perform steps 6 through 9 (measuring and adjusting values for both the small and large scan size for the new scanning direction).

During the vertical scanning mode, the X axis (and thus X axis adjustment value) corresponds to the vertical direction and the Y-axis corresponds to the horizontal direction.

11. When the calibration has finished, click the OK button at the bottom of the Scan Calibration area and the user will be prompted to select a file name and save the calibration file. The new calibration file can be loaded by selecting the Calibration tab in-situ sub tab Load Scanner Calibration Filebutton OR from the Imaging tab in-situ sub tab Control Load Calibration File and select the newly created calibration file from the list.

Only scanner calibration files saved in the directory C: Program Files Hysitron TriboScan Calibrations Scan directory can be loaded from the Load Scanner Calibration File menu item.

12. The Z Piezo Gain parameter located on the Calibration tab in-situ sub tab is the Z-axis calibration value. This value will be adjusted to yield the correct step size for the sample grating.

13. Approach the Z-axis step grating sample and begin scanning the sample surface.

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14. While scanning the sample surface, on the Imaging tab in-situ sub tab set the scan line plot to show the topography image and set the background subtraction to Zone. The height should read the value given by the grating sample manufacturer.

15. If the measured step height is too small, the Z Piezo Gain must be increased. If the measured step height is too large, the Z Piezo Gain must be decreased.

The Z Piezo Gain parameter cannot be adjusted while the probe is in contact. The probe will need to be disengaged before adjusting the Z Piezo Gain value then re-engaged to image the surface to see if the new value produces reasonable results.

16. When the correct Z Piezo Gain value has been found, click the Save Z Gain To the Current Scanner Calibration File button.

The scanner calibration is now complete. If the new scanner calibration either yields a skewed image, short scan

range or other anomalies it is recommend to re-load the original scanner calibration file and re-attempt the scanner

calibration procedure.

TriboScan 9 is not compatible with previous TriboScan scanner calibration files. The X and Y axis adjustment values should be about 16x greater. The Z Piezo Gain should be about the same.

3.10 PROBE CALIBRATIONThe probe calibration procedure requires the user is familiar with the following software operations (discussed in the

Sample Navigation, Indentation Testing, and Automated Testing Methods sections of this user manual):

• Creating sample boundaries• Set up, execution, and analysis of an indentation tests• Set up and execution of an automated method of tests• Multiple curve analysis

Furthermore, the probe calibration procedure assumes the Indentation Axis calibration and the Optic-Probe Tip Offset

calibration have been performed satisfactorily.

! No in-contact testing should be performed without first obtaining a satisfactory Indentation Axis calibration and a current (valid for the hardware configuration) Optic-Probe Tip Offset calibration.

Performing a probe calibration for each probe will compensate for non-perfect probe shape. The probe radius of

curvature and normal dulling of the probe can both be corrected by recalibrating the probe.

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During an indentation test, the probe is driven into a sample and then withdrawn by decreasing the applied force. The

applied load P and depth of penetration h into the sample are continuously monitored and a load versus displacement

plot is produced.

The contact area is determined from the probe area function A(hc) where hc, the contact depth, is found with:

To account for edge effects, the deflection of the surface at the contact perimeter is estimated by taking the geometric

constant as 0.75.

The cross-sectional area of an indentation shown in Figure 3.32 illustrates the relationship of P, A, hc, and h.

Figure 3.32 Schematic of nanoindentation

The reduced modulus is related to the modulus of elasticity E with:

For a standard diamond indenter probe, Eindenter is 1140 GPa and νindenter is 0.07. Poisson’s ratio varies between 0

and 0.5 for most materials.

The hardness has the normal definition given by:

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where Pmax is the maximum indentation force and A is the resultant projected contact area at that load.

The reduced modulus is defined as:

Where S is the stiffness of the unloading curve and A is the projected contact area. The initial unloading contact

stiffness (the slope of the initial portion of the unloading curve) is defined by:

Rearranging and substituting the above equations yields:.

To determine the area function, a series of indents at various contact depths (varying normal loads) are performed in a

sample of known elastic modulus (typically fused quartz) and the contact area A is calculated. A plot of the calculated

area as a function of contact depth is created and the TriboScan software fits the A versus hc curve to the sixth order

sixth order polynomial:

C0 for an ideal Berkovich probe is 24.5 while for a cube corner (90o) probe is 2.598 with C1 through C5 set equal to

zero. In order to fit the shape of the actual probe geometry, C1 through C5 will be allowed to vary.

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3.10.1 PROCEDURE FOR PROBE CALIBRATIONTo begin the calibration of the probe, install the probe and fused quartz sample provided with the instrument. Several

indents (a minimum of 25 recommended) will be performed on the standard sample.

CREATE THE LOAD FUNCTIONThe load function used for the probe calibration should be a load control load function with a 5 second load time, 2

second hold time and a 5 second unload time. For a generic probe area calibration the maximum load should be close

to the maximum allowable of the transducer (around 10,000 μN for a three-plate capacitive transducer; around

100 mN for a MRNP transducer). The minimum load should be small enough so that the contact depth will be lower

than the lowest contact depth desired on other samples. Save this load function so that it can be opened from the

automated methods window.

The Basic QS Trapizoid from th Standard Load Function menu on the Load Function tab Indentation sub tab

woks well for the probe calibration ons fused quartz.

! The maximum recommended load for a MRNP transducer is about 100 mN (with a Berkovich probe). Larger forces will cause sample cracking and offer an incorrectly measured displacement.

RUN AN AUTOMATED TESTING METHOD ON THE FUSED QUARTZ SAMPLEA 10 by 10 array is recommended to increase the accuracy and reliability of the calibration. The method should cover

the entire range of loads that the transducer is capable of, typically from about 10,000 μN down to around 100 μN

(100 mN down to 1 mN with a MRNP transducer). The exact loads used will depend on which type of probe is being

used and where the user desires the calibration to be valid.

A piezo automation with about 100 tests spaced a minimum of 5 μm apart with a similar load range as discussed in the above paragraph could also be used.

The probe calibration procedure is intended to be performed on the standard fused quartz sample supplied with the system.

The load function for the automated method should be configured as given in Figure 3.33 from the Load Function

Setup window within the Automation tab Methods sub tab Load Function button.

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Figure 3.33 Load Function Setup window for

probe area function procedure

ANALYZE THE INDENTATION TESTS

After the indents have been completed click the Analysis tab Quasi sub tab in the TriboScan software. Ensure the

Unloading Segment parameter is set to 5 (or 3 if no Lift Segments are used); checking the Auto box next to the

Unloading Segment will automatically select the last segment as the unloading segment. Select the Plot Multiple

Curves icon or click the Analysis menu Plot Multiple Curves. From the Plot Multiple Curves window, click the

Add Curves button on the right side of the screen and select the curves that were performed in the previous step. The

resulting screen should look similar to Figure 3.34.

Figure 3.34 Multiple curve plot of

calibration indents

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Notice that in Figure 3.34 there are outlier curves that need to be removed before proceeding. A number of things

including a dirty sample, or a pre-existing scratch or indent on the sample could cause these outliers. If there are more

than a few outlier curves from the method, check that the sample is clean and that the sample is the fused quartz

sample provided with the instrument and then re-perform the indents. Remove unwanted curves by selecting the

curve on the plot or on the list of file names and click the Remove Curve button.

After the outlier(s) have been removed from the data set click the Mult. Cur. Ana. button on the right hand side of the

screen and save the text file. A screen showing hardness and reduced modulus will open; close and disregard this

screen. These values for hardness and modulus were calculated with a default probe area function, not the function

specific to the probe and are likely to be incorrect.

CALCULATE THE NEW PROBE AREA FUNCTIONCalculating the new probe area function is started by accessing the area function calculation window by clicking the

Calibrate tab Tip Calibration sub tab Calculate sub tab. Select the File menu Open command (or Open

Multiple if fitting multiple fitting files) near the top left of the window.

It is recommended to perform the area function in Indentation mode.

When prompted, select the text file saved from the Plot Multiple Curve window (in the previous section) and click

Load to populate the curve with the Contact Depth vs. Contact Area information (Figure 3.35).

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Figure 3.35 Calculate sub tab

The parameters on the Calculate sub tab will automatically populate for a diamond probe and fused quartz standard.

If an alternate sample or probe material is used the values in the following tables should be referenced.

Figure 3.36 Standard samples reference

table

Figure 3.37 Standard probes reference table

Young’s Modulus Poisson’s Ratio

Fused Quartz (recommended for most probe calibrations) 72,000 N/mm2 0.17

Polymethyl Methacrylate (PMMA) 4,400 N/mm2 0.38

Polycarbonate (PC) 2,700 N/mm2 0.37

Aluminum (001) 71,000 N/mm2 0.31

Vitreous Carbon (glassy carbon) 120,000 N/mm2 0.28

Silicon (primarily used with PI series) 150,000 N/mm2 0.17

Young’s Modulus Poisson’s Ratio

Diamond (recommended for most applications) 1,140,000 N/mm2 0.07

Sapphire 345,000 N/mm2 0.29

Stainless Steel 193,000 N/mm2 0.30

Pulsar-D (boron doped diamond) 1,140,000 N/mm2 0.07

Pulsar-C (conductive ceramic) 380,000 N/mm2 0.22

Pulsar-M (conductive metallic) - -

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Choose the Tip Geometry or enter the C0 value in the Fix C0 Value at: field (24.5 for a Berkovich probe; 2.598 for a

cube corner probe; [-π] for conical probes) and click the Execute Area Fit button and the software will fit a

polynomial to the data. The fit should be a smooth parabolic shape with no inflections.

The user may choose to click on the plot and drag the red and blue lines (or use the Min (nm) and Max (nm)

parameters) to define a tighter area to calibrate if indentations will only be occurring at a very specific depth. The user

can also choose to Split Data Into Two Zones for Differential Weighting if it is preferred that the area function fit

favors the lower or higher displacements.

SHALLOW VS. DEEP INDENTATION TESTSIt is important to know when computing the area function whether the probe will be used primarily for deep

indentations or shallow indentations.

When planning to perform deep indents, it is desirable to keep C0 at the ideal coefficient (24.5 for a Berkovich

probe), which the probe will approach as it goes deeper into the sample. As hC increases C1 through C5 of the area

function polynomial fit become negligible and the first term of the polynomial becomes the most important term:

Figure 3.38 Probe radius effects with

shallow indentation

If planning to perform shallower indentations, consider allowing C0 to vary because at shallower depths the radius of

curvature becomes the dominating effect in the area function. The probe will not go deep enough to approach the

ideal Berkovich shape and the values in the area function polynomial cannot be neglected. Allowing C0 to vary will

help take the non-perfect probe shape into account at shallower depths. The value for C0 should still be near 24.5 (or

2.598 for a cube corner probe) when C0 is allowed to vary. If the value for C0 is far (±~5) from the standard value

(24.5 for a Berkovich, 2.598 for a cube corner probe) the probe may be damaged or the machine compliance value

may be incorrectly set.

When finding the coefficients for the area function, it is also best to use as few coefficients as possible. When too

many coefficients are used, the function will begin to fit to the noise in the data, and inflection points will develop. If

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the curve can fit well with only two coefficients, this is the best. However, if many data points are used, sometimes all

6 coefficients will need to be used to get a good area function; typically, 3 or 4 coefficients works well.

VERIFY THE PROBE AREA FUNCTIONWhen the fit of the curve is satisfactory, click Save Area Function on the right hand side of the screen in Figure 3.35

and the area function will automatically be applied to the system. To check that the area function was saved correctly

(or load a previously defined area function), either select the Calibration tab Tip Area Function sub tab Open

sub tab. The displayed area function is the current area function applied to the system. Previous probe area functions

can be loaded by clicking File Open.

The probe is now calibrated and saved to the system. All of the indents can be analyzed again using the new probe

area function (the Area Function toggle button on the Analysis tab Quasi sub tab must be set to From Tip Area Tab

to use the newly created area function on previous *.hys files). The resulting values for hardness and reduced

modulus should be correct for fused quartz (hardness ~9.25 GPa, reduced modulus ~69.6 GPa). The hardness and

reduced modulus versus contact depth plot should now look similar to Figure 3.39. Notice that below around 40 nm

the values for hardness become unreliable; this is a normal effect related to the radius of curvature of the probe.

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Figure 3.39 Hardness and reduced modulus

plot for a probe with radius of around 120 nm

When the contact depth approaches approximately one-third the radius of the probe the hardness values become

sporadic. The values for reduced modulus will stay relatively constant because that value was defined as 69.6 GPa

when the area function was fit. However, hardness is a computed value that is dependent on the contact area of the

probe and is thusly related to the radius of curvature of the probe. Testing below approximately one-third the radius of

the probe is typically not valid (illustrated with Figure 3.39 with a probe of radius of curvature of approximately 120

nm). To test in the displacement range less than this cutoff it is recommended to use a sharper probe with a smaller

radius of curvature such as a cube corner.

In fact, it is recommended that testing be performed only in the displacement range that the probe is calibrated for

(from 40 nm up to 166 nm in this example). However, it can be assumed (given the probe has not been damaged) that

the shape will continue as a Berkovich, cube corner or other geometry beyond the calibrated depth. With that said,

given that the correct value for C0 has been entered when the area function was performed, testing may be executed

deeper than the calibrated depths assuming the probe will imitate its ideal shape at higher displacements.

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3.11 MACHINE COMPLIANCE CALIBRATIONThe measured displacement of depth sensing indentation instrument is the sum of the indentation depth into the

specimen and the displacement associated with the measuring instrument, otherwise known as machine compliance.

It is important that machine compliance be properly measured for the instrument because, especially at high forces,

the machine compliance of the system can be a significant amount of the total displacement.

There are many factors which can affect the machine compliance of a system. The most common factors include:

Transducer Different transducers have varying amount of compliance. The bridge on lateral axis transducers makes them more compliant than 1D transducers. In general, stiffness of the center plate, or thickness of epoxy holding parts together can cause different amounts of compliance.

Probe Nanoindentation probes are handmade, so depending on the amounts of epoxy, or lengths of the shank on the probe, the compliance induced by the probe may vary.

Sample Mounting Depending upon the sample mounting method, additional compliance may be introduced into the system. Never use a soft material, such as putty or double-sided tape to mount a sample. If a thin layer of stiff glue or epoxy is used, the added compliance is typically negligible.

Transducer Mounting The transducer must be mounted to the TriboScanner in the same way each time. The transducer should also be level, and seated as well as possible.

Using the above guidelines, the machine compliance can be checked for each transducer and type of probe/sample

stage configuration. The machine compliance calibration can be performed in conjunction with calculating the probe

area function.

Although the machine compliance is unique for each transducer/probe/sample mounting method it can often be assumed that the machine compliance will remain constant for most probes and sample mounting methods used with each type of transducer. Because of this, the frequency of verifying the machine compliance is left to the user for verification.

The relationship for machine compliance (inverse of stiffness) of the contact between any axis-symmetric indenter

and an elastically isotropic half-space is:

Where Er is the reduced modulus given by:

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And E and ν are Young’s modulus and Poisson’s ratio, respectively.

Here h is the displacement of the probe relative to the specimen, P is the load and A is the projected contact area. To

account for elastic displacements of the machine compliance, Cm must be added to the contact compliance Cc

yielding the total compliance of the system:

The hardness of a sample is given by the relationship:

Where H is the hardness, Pmax is the maximum applied force and A is the projected contact area. Substituting the

above equations yields:

For fused quartz, it is a reasonable assumption that hardness and reduced modulus are constant at large displacements

(hc > 1/3 probe radius) with a Berkovich probe with no sample cracking. Given this assumption, a graph of the

inverse measured stiffness versus the inverse of the square root of the maximum force for a series of high-force

indentations on fused quartz will produce a linear line with a Y-axis intercept of the machine compliance value.

The Machine Compliance sub tab (Figure 3.40) is available with all Hysitron systems. The Machine Compliance sub

tab is an automated plotting routine for calculating the system machine compliance and can be accessed from the

Calibration tab Machine Compliance sub tab.

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Figure 3.40 Machine Compliance sub tab

The Machine Compliance sub tab is a fitted plot of [1/sqrt(maximum force)] versus [1/(stiffness)]. A machine

compliance calculated in this way is valid for the following probe geometries:

• Berkovich• Cube Corner• Vickers

The Machine Compliance sub tab should NOT be used to calculate the machine compliance for the following probe

geometries:

• Conical• Cono-spherical• Flat-ended• Wedge• Specialty probes

To use the Machine Compliance sub tab, use the following procedure:

1. An array of several indents (typically more than 100) should be performed on the fused quartz standard at loads higher than 5000 μN (for MRNP/3D OmniProbe transducers the load should not exceed 100 mN).

2. Fit the data and generate a text file using the Multiple Curve Analysis routine found on the Analysis tab.

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3. Go to the Machine Compliance tab and select the File Open to select the data file generated in step 2.

4. A window similar to Figure 3.41 will open; enter the desired load range for the machine compliance calculation. Typically, the machine compliance calculation is only performed at loads greater than 5000 μN.

Figure 3.41 Machine compliance load range

selection

5. With the data displayed in the Machine Compliance sub tab, choose the range to fit by clicking and dragging the blue and red indicator bars.

6. Click the Calculate button to fit the machine compliance data.

7. The Change in Compliance is given in the lower right portion of the software, this value should be added to the Machine Compliance value given in the Calibration tab System Calibration sub tab.

Approximate Machine Compliance values are given as:

• Indentation axis transducer= 1.0• Lateral axis transducer = 3.0• nanoDMA transducer = 0.5• nanoECR transducer = 1.0• TriboAE transducer = 1.0• MRNP transducer = 0.35

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Auto Calibration Sub Tab

CHAPTER 4 AUTO CALIBRATION SUB TAB

The Auto Calibration sub tab (Figure 4.1) is available with all TI series systems. The Auto Calibration sub tab

contains information and parameters that determine the frequency, flow, and details of the various automatic

calibration procedures.

Figure 4.1 Auto Calibration sub tab

The automatic calibrations presented in this section are primarily intended to be performed as part of an automated testing method.

The automated calibrations provided as part of the TriboScan package are accessed from the Calibration tab Auto

Calibration sub tab. The calibrations are intended to be performed in the order given in the flow chart show in

Figure 4.2.

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Figure 4.2 Automated calibrations flow

chart

The calibration flow chart indicated in Figure 4.2 is initiated by selecting the Initiate Auto Calibration button OR the

Auto Cal at Start check box from the Automation tab Methods sub tab shown in Figure 4.3. Using the check box

would perform the flow chart prior to starting the automated method and using the button would initiate the flow cart

immediately.

Figure 4.3 Auto calibration initiation

options

The Determine by Event # option is discussed in the Tip Calibration (Analysis) section of this user manual.

Even with the automated calibration procedures the position/group for the standard fused quartz sample must be defined by the user (from the Automation tab Methods sub tab) prior to initiating any automated calibration procedure that will be performed on the standard quartz sample.

In addition to initiating the flow chart shown in Figure 4.2 the user can also select to perform each of the three

automated calibrations individually.

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AUTO CALIBRATION HEADINGThe parameters listed under the Auto Calibration heading (Figure 4.4) are used to determine the frequency and

number of attempts of each calibration. A description of the parameters is listed below.Figure 4.4

Auto Calibration sub section

Events Between Auto Cal

The Events Between Auto Cal parameter allows the user to determine the number of tests that can be performed before the automated calibration is initiated. The automated calibration steps that would be preformed are defined by the check boxes (also within the Auto Calibration heading). This parameter is linked to the parameter in the Calibration tab Tip Calibration sub tab Define sub tab.

This option is intended to be used while chaining multiple automated testing methods of tests, however, the Tip Check procedure will only activate following the completion of an automated testing method. For example, if the Events Between Tip Checks is set to 50 and two automated testing methods of 100 indents each are chained together, the Tip Check procedure will only initiate following the first automated testing method (following the 100 indents). The Tip Check procedure will only initiate between automated testing methods and will not initiate during an automated testing method or between positions (for the same automated testing method) on the same sample or different samples.

Using the Events Between Auto Cal option will initiate the flow chart in Figure 4.2starting with the Indentation Axis calibration and (if selected) proceeding to the Tip Check (and, if necessary, Tip Calibration) procedures.

Activate the Events Between Auto Cal option by selecting the Determine by Event #check box from the Automation tab Methods sub tab Setup side tab.

Events Since Last Tip Calibration

The Events Since Last Tip Calibration parameter will count the number of tests that have been performed since the last Tip Check procedure or Tip Area Function procedure. This parameter is linked to the parameter in the Calibration tab Tip Calibration sub tab Define sub tab. The Events Since Last Tip Calibration will be reset to zero following a new Tip Calibration process.

Transducer Calibration

The Transducer Calibration pull-down menu allows the user to determine the frequency to initiate the automatic calibration process (always starting with the Transducer Calibration). The options include:

• Disabled - No Transducer Calibration or automatic calibration process will be performed.

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• With Auto Cal - The Transducer Calibration (beginning of the automatic calibration process) will be performed based on the Events Between Auto Cal setting.

• Every Method - The Transducer Calibration (beginning of the automatic calibration process) will be performed at the beginning of each automated testing method.

• Elapsed Time - The Transducer Calibration (beginning of the automatic calibration process) will be at the time interval set in the Every [blank] Hours parameter.

Every [blank] Hours The Every [blank] Hours parameter defines the interval for the automatic calibration process to be performed if the Elapsed Time option is selected from the Transducer Calibration pull-down menu.

Tip Check Enable Selecting the Tip Check Enable check box will include the Tip Check as part of the automatic calibration process (starting with the Transducer Calibration). A Position Group and Load Function must be defined within the Tip Check heading.

Tip Calibration Enable Selecting the Tip Calibration Enable check box will include the Tip Calibration as part of the automatic calibration process (starting with the Transducer Calibration). If both the Tip Check Enable and the Tip Calibration Enable are selected the system will only perform a Tip Calibration if the Tip Check fails. If only the Tip CalibrationEnable is selected a tip calibration will be performed following the successful Transducer Calibration. A Position Group and Load Function must be defined within the Tip Calibration heading.

Retries The Retries parameters for the different Transducer Calibration parameters (indentation, scratch, nanoDMA) as well as the Tip Check and Tip Calibration parameters allows the user to define the number of times the automatic calibration should be attempted for each step (if failed the first time).

Initiate Auto Calibration button

The Initiate Auto Calibration button will manually start the automatic calibration process with the options (Tip Check, Tip Calibration, and number of Retries) defined under the Auto Calibration heading. The automatic calibration process will automatically be initiated if the feature is selected from the Automation tab Methods sub tab Auto Cal at Start OR Determined by Event # check box.

TRANSDUCER CALIBRATION HEADINGThe parameters listed under the Transducer Calibration heading (Figure 4.4) are used to determine which portion(s)

of the transducer to calibrate and the tolerance ranges to determine if the calibration is satisfactory. The Transducer

Calibration is the first step in the automated calibration flow chart (Figure 4.2). A description of the parameters is

listed below.

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Figure 4.5 Transducer Calibration sub

section

Calibration check boxes

The Transducer Calibration always includes the Indentation Axis calibration and the user can select to include the Lateral Axis calibration and/or nanoDMA calibration by selecting the check box next to the corresponding calibration.

Copy [---] Values buttons

There are three Copy [---] Values buttons (one for each of the three possible calibration processes). Clicking the Copy [---] Values button will copy the associated transducer calibration values from the Calibration tab System Calibration sub tab. Tolerance values can be set for each calibration value. The tolerance values will determine if the Transducer Calibration is within specification for the automatic calibration process. If any Transducer Calibration result is outside of the listed tolerance the calibration will be retried (as defined in the Retries parameters from the Auto Calibration heading). If the Transducer Calibration continues to fail the automatic calibration process will end and an error will be generated stating the Automatic Calibration has failed!.

Initiate Transducer Calibration button

The Initiate Transducer Calibration button will perform the Indentation Axis calibration followed by any additional calibrations (Lateral Axis or nanoDMAcalibration) that are selected with the check box and then stop. The Initiate Transducer Calibration will not perform any additional steps in the automatic calibration process.

To avoid a failed automatic calibration process, the Copy [---] Values buttons should be used after having successfully completed a normal calibration (from the Calibration tab System Calibrationsub tab) and before attempting any automatic calibration procedures.

TIP CHECK HEADINGThe parameters listed under the Tip Check heading (Figure 4.4) are used to define the number, spacing, and tolerance

for the indentation tests during an automated Tip Check process. The Tip Check is the second step in the automated

calibration flow chart (Figure 4.2). The Tip Check procedure will perform a defined number of tests on the standard

sample (typically fused quartz) and compare the results to the Modulus and Hardness values defined by the user

(located near the middle of Figure 4.6). A description of the parameters is listed below.

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Figure 4.6 Tip Check section

Number of Indents The Number of Indents parameter allows the user to define the number of indents to be used for the Tip Check process.

Spacing The Spacing parameter allows the user to define the spacing between each indent that is performed for the Tip Check. The Tip Check indents will be performed in a line from left to right (-X to +X) across the sample starting at the current Position Group. Each consecutive Tip Check will start at the end of the last Tip Check position (plus the Spacing amount). When the Tip Check indents reach the edge of the defined sample space the next indent (and following Tip Check indents) will be placed one Spacing in the -Y axis direction and the system will continue across the sample from left to right.

Modulus The Modulus parameter allows the user to define the reduced modulus and tolerance of the standard sample used for the Tip Check process. A Tip Check process that measures outside of these values will end with a message stating the automatic calibration process has failed.

Hardness The Hardness parameter allows the user to define the hardness and tolerance of the standard sample used for the Tip Check process. A Tip Check process that measures outside of these values will end with a message stating the automatic calibration process has failed.

Force & Displacement Offset

The Force & Displacement Offset (Same Values as Tip Calibration) check box will use the same automatic offset parameters for locating the origin of the load vs. displacement curve as defined in the Tip Calibration section. Typically, the user will want to allow the automatic offset (parameter checked) and the default parameters will normally be sufficient for testing standard samples such as fused quartz. The automatic offset parameters are the same as the Force Offset Auto button and Displacement Offset Auto button on the Analysis tab Quasi sub tab Quasi sub tab and more information can be found in the Analysis tab section of this user manual.

Position Group & Position Editor

The Position Group pull-down menu and associated Position Editor button allows the user to select the sample/location that the Tip Check process will be performed. The Position Editor button is a shortcut to the Automation tab Methods sub tab Position side tab where the user can create the position group and positions on their choice of standard sample (typically fused quartz). After the Position Group has been created it can be selected from the Position Group pull down menu.

Load Function The Load Function button allows the user to associate a previously saved load function with the Tip Check process.

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TIP CALIBRATION HEADINGThe parameters listed under the Tip Calibration heading (Figure 4.7) are used to define the number, spacing,

tolerance, and fitting parameters for the indentation tests during an automated Tip Calibration process. The Tip

Calibration is the third step in the automated calibration flow chart (Figure 4.2). The Tip Calibration procedure will

perform a defined number of tests on the standard sample (typically fused quartz) and calculate a new tip area

function. A description of the parameters is listed below.

Figure 4.7 Tip Calibration section

Number of Indents The Number of Indents parameter allows the user to define the number of indents to be used for the Tip Calibration process.

Spacing The Spacing parameter allows the user to define the spacing between each indent that is performed for the Tip Calibration. The Tip Calibration indents will be performed in a line from left to right (-X to +X) across the sample starting at the current Position Group. Each consecutive Tip Calibration will start at the end of the last Tip Calibration position (plus the Spacing amount). When the Tip Calibration indents reach the edge of the defined sample space the next indent (and following Tip Calibration indents) will be placed one Spacing in the -Y axis direction and the system will continue across the sample from left to right.

Modulus The Modulus parameter allows the user to define the reduced modulus and tolerance of the standard sample used for the Tip Calibration process. A Tip Calibrationprocess that measures outside of these values will end with a message stating the automatic calibration process has failed.

Hardness The Hardness parameter allows the user to define the hardness and tolerance of the standard sample used for the Tip Calibration process. A Tip Calibration process that measures outside of these values will end with a message stating the automatic calibration process has failed.

Cutoff The Cutoff is defined as the calculated displacement where the tip area function is no longer valid to produce reasonable fit results. To obtain reliable results, all testing should be performed at contact depths larger than the Cutoff. The Cutoff parameter and check box, when activated, will fail the Tip Calibration process if the automatically measured Cutoff (discussed in the Analysis section of this user manual) is below the value entered.

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Position Group & Position Editor

The Position Group pull-down menu and associated Position Editor button allows the user to select the sample/location that the Tip Check process will be performed. The Position Editor button is a shortcut to the Automation tab Methods sub tab Position side tab where the user can create the position group and positions on their choice of standard sample (typically fused quartz). After the Position Group has been created it can be selected from the Position Group pull down menu.

Load Function The Load Function button allows the user to associate a previously saved load function with the Tip Check process.

Minimum Number of Files

The Minimum Number of Files parameter allows the user to define the minimum number of data files to use for the Tip Calibration process. If the Minimum Number of Files is not adequate (after removal of any data files that fall below the defined Cutoff) the Tip Calibration process will fail.

Number of Coefficients

The Number of Coefficients parameter allows the user to define the number of coefficients to use for the Tip Calibration fitting routine. The Number of Coefficientsis the same coefficients mentioned in the Analysis Tip Calibration section of this user manual.

Initial C0 The Initial C0 pull-down menu and associated parameter allows the user to define the C0 coefficient for the Tip Calibration. Ideal C0 values are given in the appendix of this user manual otherwise the user can set the Initial C0 pull-down menu to Vary C0which would allow C0 to float and fit instead of being user defined.

All Coefficients Positive

The All Coefficients Positive check box allows the user to force the Tip Calibration to use only positive coefficients. The same parameter is discussed in the Analysis Tip Calibration section of this user manual.

Force & Displacement Offset

The Force & Displacement Offset check box will enable the same automatic offset parameters for locating the origin of the load vs. displacement curve. Typically, the user will want to allow the automatic offset (parameter checked) and the default parameters will normally be sufficient for testing standard samples such as fused quartz. The automatic offset parameters are the same as the Force Offset Auto button and Displacement Offset Auto button on the Analysis tab Quasi sub tab Quasisub tab and more information can be found in the Analysis tab section of this user manual.

The following parameters are all enabled with the Force & Displacement Offset check box. More information regarding each parameter can be found in the Analysis tab section of this user manual.

• Displ. Cutoff for Force Offset• Force Endpoint for Displ. Fit• Include Load Offset in Displ. Fit (Adhesion)

When comparing the measured hardness and reduced modulus values to the values defined by the user the system will automatically calculate a cutoff for tip radius effect. At low displacements, due to variance in the tip geometry the hardness and reduced modulus values will vary and this automated tip check and tip area function procedure will measure identify and avoid data that is collected below the cutoff threshold.

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AUTOMATIC OUTLIER REMOVALTriboScan has the option to automatically remove outlier curves from the Plot Multiple Curves window (Figure 4.8).

Figure 4.8 Plot Multiple Curves window

The Remove TAF Outlier button will evaluate the average of the loading curves and remove any curves that deviate

from the average loading curve by more than about 5% or any curves that fall out order (for example, the load and

displacement of each progressive curve should decrease from the previous plot).

If the user initiates the automated Tip Calibration procedure from the Auto Calibration sub tab the data used for the

calibration will automatically have the outliers removed or the user can choose to use the Remove Outlier button on

the Plot Multiple Curve Analysis window to evaluate data that was not collected during the automated Tip Area

Function procedure.

The Automatic Outlier Removal procedure requires that the data be collected in order of decreasing load.

The Automatic Outlier Removal procedure will automatically initiate with both the Tip Check and Tip Calibration procedure.

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SECTION | TI SERIES TESTING• Sample mounting and software set up• in-situ SPM imaging• Testing from the optical focus and in-situ SPM imaging position• Automated testing routines

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CHAPTER 5 TESTING

TriboScan is a full-featured software package that combines both testing and analysis into one easy-to-use software

suite. The Testing section will cover common testing routines equipped on most systems as well as basic testing

routines that beginning users can refer to for a simple step-by-step method of performing a specific test.

The Testing section assumes that all calibrations listed in the System Calibrations section have been satisfactorily

completed and the user is familiar with the TriboScan software package and TI series system hardware.

! It is dangerous to perform procedures within the Testing section without first completing or verifying the hardware is correctly setup and calibrated as given in the System Calibrations section. Failure to follow the preceding procedures, as given in the System Calibrations section can result in damaged hardware, probes or samples.

Detailed descriptions of the various TriboScan software tabs is given in the Software section and will not be covered

in the Testing section. For information on the particular function, button or parameter that is mentioned but not

discussed within the Testing section, refer to the appropriate tab within the Software section for a more thorough

description.

5.1 TESTING OVERVIEWBecause of the differing abilities of the various Hysitron system platforms, this Testing chapter may include topics

that are not available on every system. Table 5.A illustrates the different testing abilities* of the Hysitron system

platforms.

Table 5.A Hysitron standard system testing

modes

*Standard system testing abilities subject to changes without notice.

Base TI SeriesnanoDMA/nanoECR

Option

MRNP/3D OmniProbe

Option

Requires Optically Defined Sample Boundaries YES

Testing from Optics Position YES

Testing from in-situ Imaging Position YES NO

Nanoindentation Testing YES

Nanoscratch TestingYES (with applicable transducer)

NOYES

(3D OmniProbe only)

Scanning Wear Testing YES NO

Feedback Control Testing YES

Automated Methods YES

Piezo Automation YES NO

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5.2 SAMPLE MOUNTINGSamples used with Hysitron systems must be mounted rigidly to reduce system compliance. The most

straightforward technique for mounting samples is to adhere the sample to a steel SPM puck with a cyanoacrylate-

based adhesive (super glue). Soft adhesives such as double-sided tape or putty should never be used to mount samples

due to the increased machine compliance. The basic sample mounting procedure is given below:

1. Acquire some steel SPM sample pucks (available from Hysitron and many other AFM supply companies).

2. Clean the steel SPM sample puck with some alcohol or acetone to remove any oily residue.

3. Put a small amount of cyanoacrylate-based adhesive on the sample puck.

4. Place the sample on the adhesive and press firmly for 20 seconds. It may take longer than this for the adhesive to fully cure, however, the sample should be usable within a few minutes.

5. Place the sample on the sample stage and allow the magnetic attraction to firmly hold the steel SPM puck (firmly adhered to the sample) to the stage.

Vacuum or clips may also be used for the samples (if equipped), however, flatness and rigidity to stage should be

considered when determining if mounting is sufficient.

One of the advantages of Hysitron instruments over some competitors instruments is the Z axis stage, which allows

samples of differing heights to be placed on the stage at the same time. To prevent the transducer, piezo scanner or

optical camera system from crashing into objects, samples should be spaced a minimum of 3 cm from other samples.

Samples with a height variation of more than 1 cm between each other should be tested individually with no other

samples on the stage.

! Hysitron nanoindentation systems are designed for samples with similar heights. Samples of similar height (less than 1 cm difference) should be placed a minimum of 3 cm from each other. Samples with more variation than this should be tested individually with no other samples on the stage.

It is important that TI series systems always have taller sample located on the side of the stage closest to the optical

camera column. Placing taller samples on the side away from the optical camera column may allow the transducer,

scanner or probe to crash into an undefined, taller sample while optically focusing on a shorter sample (Figure 5.1).

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Figure 5.1 Placement of samples with

height differences

Hysitron offers an array of sample mounting options that include a vacuum sample stage and non-magnetic sample

clips. For more information on additional sample mounting options contact a Hysitron service engineer.

All user samples are different so the mounting procedure will differ for each sample, however, the user should take

care to mount the samples as rigid as possible to avoid increased or non-linear machine compliance measurements.

Further suggestions for different sample mounting options will be discussed in the Testing section of this user manual.

5.2.1 DUAL HEAD MODEHysitron TI series systems may be equipped with a dual head mode which allows the operation of a standard

transducer (indentation, nanoscratch, nanoDMA, nanoECR) and 3D OmniProbe/MRNP (high load) transducer. If

operating in this mode it is important to use the supplied dual head sample stage which allows for only a single row of

samples (to help avoid damage to the transducers, tips, and other hardware).

All TI 980 TriboIndenter systems are equipped with dual low load mode (and 3D OmniProbe/MRNP may be added).

TI 950 TriboIndenter systems using the performech II control unit may be upgraded to include dual standard

transducer (dual low load) and the same requirement for using the dual head sample stage applies to the dual standard

transducer mode.

! If operating the system in dual head mode the dual head sample stage (single row of samples) is required for safe operation.

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5.2.2 CREATING SAMPLE BOUNDARIESThe top-down optical camera system is used to visibly focus on the sample surface, create a boundary that defines the

edges of the sample and then, given that the Optic-Probe Tip Offset calibration has been performed correctly,

approach the surface.

It is important that the upper surface of the sample be in focus when the boundary is created. This is especially

important when the sample being tested is translucent as the bottom surface can many times be mistaken for the upper

surface resulting in a probe crash and system emergency stop.

Procedure for creating a sample boundary is given below. The numbers in Figure 5.2 correspond to the numbered

listed in the procedure below.

Figure 5.2 Sample boundary creation

procedure

1. Place the desired sample(s) on the sample stage.

2. To get close enough to the sample and still be able to move in the X/Y-axis direction the Z Safety Disabled and X-Y Safety Disabled must be selected (Figure 5.3). Select this option by clicking the grey circle near each option in the Stage Controls area.

Figure 5.3 Disable X, Y and Z Safety

Disabled radio buttons

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3. Click the New Sample button to add a sample (Figure 5.4). Specify a sample name for the sample when prompted (Figure 5.5). The new sample can be renamed at any time by selecting the sample from the pull down menu and clicking Rename.

Figure 5.4 New Sample button location

Figure 5.5 Rename Sample prompt

4. Select the sample that safety limits are to be set for from the pull-down menu in the Sample Boundaries area (Figure 5.6).

Figure 5.6 Sample Boundaries pull-down

menu

5. Bring the sample into focus by using the stage controls. It is typically easier to first locate an edge of the sample as opposed to the bulk material.

All sample boundaries must be created while optically focused on the sample surface. Creating a sample boundary out of focus is dangerous and can cause serious hardware damage.

6. With the sample in focus and the desired X and Y axis position in the center of the video window, click the Pos. Add button (Figure 5.7). This will be the first point defining the sample boundary. A small blue point will appear on the map of the stage (left side of the Sample Boundaries area) representing the first point of the sample.

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Figure 5.7 Pos. Add button to add first

point

7. Using the stage controls, trace around the sample and locate additional points on the edge of the sample.

8. Again, click the Pos. Add button. An additional blue point will be displayed in the window, with the points connected by a line (Figure 5.8).

Figure 5.8 Pos. Add button to add

additional sample points

9. Repeat steps 7 and 8 above until the sample has been completely traced in the Sample Boundaries area (Figure 5.9).

Figure 5.9 Completed sample boundary

10. The Z Safety Disabled and X-Y Safety Disabled should be enabled (grey circle) after the sample boundaries have been created to help protect the system (Figure 5.10). Continue to the Quick Approach sub-section located within this section.

Figure 5.10 Enable X, Y and Z Safety

Disabled radio buttons

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If testing will be performed from the optical position, the actual height of each sample to be tested must first be

measured using the quick approach feature by left-clicking the Quick Approach button with the optics focused within

the sample boundary. A quick approach is not necessary if the user will be performing an in-situ image before testing

the sample.

The optic position is indicated by a hollow pink circle. A hollow green diamond indicates the probe position. It is

possible to move to specific locations on the sample by right-clicking on a desired position within the stage map in

the Sample Boundaries area. Sample boundary points can be removed by selecting the point to remove and clicking

the Pos. Remove button.

If the user would like to test only on the image shown in the video window, the Create Boundary button can be used

instead of tracing the sample. The Create Boundary button will create a boundary of the current optic position and

record the current in-focus height.

The Create Boundary option should be used only on very flat samples or only the highest portion of an uneven sample to prevent the probe from crashing into undefined sample features.

The sample boundary should be in focus at all defined points. The Z-axis stage control may be adjusted throughout the sample boundary defining process and the software will automatically calculate a plane fit through the defined points to assume the height of the sample. If the sample boundary differs greatly in height from the center of the sample (such as a curved surface) several smaller sample boundaries may need to be created within the sample to accommodate the differing Z-axis heights.

A single right-click within a defined sample boundary will move the X, Y, and Z-axis stages to the optical focus of the selected location.

! The tallest portion of any sample MUST always be defined. By not defining the tallest portion of any installed sample the user risks the possibility of crashing the probe, transducer or scanner on an undefined sample area which will likely result in damage to the system or sample.

5.2.3 QUICK APPROACHThe Quick Approach button (Figure 5.11) will move the probe towards the sample in order to find the exact Z-height

of the sample. A Quick Approach is performed by optically focusing on the sample of interest and clicking the Quick

Approach button from the Sample Boundaries area of the Sample Navigation tab. This will quickly bring the probe

into contact at the current optics position on the sample and update the sample height (given as the Last Contact

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Height parameter) with an exact value. Each sample must have a Quick Approach performed before performing tests

on that sample.

Figure 5.11 Location of Quick Approach

button

A Quick Approach of the sample can only be successfully completed following an Optic-Probe Tip Offset calibration.

Without the aforesaid calibration being completed, the probe will likely either crash into the sample or begin the

approach so far from the sample that it will take several hours to contact the surface.

If the first approach to a sample is for in-situ imaging, the Quick Approach may be bypassed. During the first

approach for in-situ imaging, if a Quick Approach has not been completed for the sample, the system will use quick

approach parameters to bring the probe into contact with the sample.

Performing a Quick Approach may leave a small indent on the sample. It is best to perform the Quick Approach on a portion of the sample that will not be tested but is near the desired testing location.

The sample Last Contact Heights are cleared whenever the workspace is re-opened or the software is restarted. Before testing can continue, a Quick Approach must be re-performed on all samples that will be tested.

! Do not perform a quick approach procedure before a Optic-Probe Tip Offset calibration has been performed. The Optic-Probe Tip Offset calibration procedure must be performed before a quick approach or any testing is performed.

! Do not attempt normal operation of the instrument with the X/Y or Z Safety Disabled. This could cause the probe to crash into a sample, and extreme damage may occur to the transducer, piezo scanner and/or probe.

! Samples placed on the sample stage should be spaced greater than 3 cm apart from each other. If samples are spaced closer than this distance, extreme damage may occur to the transducer, piezo scanner and/or probe.

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5.3 CHOOSING A TEST TYPEAll standard TI series systems are limited to maximum displacement of approximately 5 µm and a maximum force of

approximately 10 mN. For softer materials (exhibiting viscoelastic behavior) nanoDMA testing is typically

recommended. For materials requiring higher forces (up to 10 N) or displacements (up to 80 µm) MRNP transducer

testing is typically recommended.

Open Loop Open Loop testing has no feedback and is typically not used as frequently as other test types. There may be certain situations where the user wants to perform a test without feedback (for example, if the test is in air or the user does not want to adjust gain values) but typically a feedback control option will be selected. It is important to note that Open Loop also does not include any Lift Height (pre test sample lift) which may cause error in the measured displacement.

Load Control Load Control testing is the most commonly used with the Hysitron system. Load Control testing is ideal for standard indentation on hard materials (such as metals, porcelains, ceramics, and glasses) as well as indentation on hard polymer samples. Load Control tests can also be used for measuring creep of a sample by applying and holding a constant force to measure how the displacement changes with respect to time.

Displacement Control Displacement Control testing is typically used for softer materials or biological samples. A relaxation test can be performed by applying a constant displacement into a sample and measuring the changing force. Displacement Control testing is also typically used for adhesion testing by performing a test and measuring the amount of negative force in the load vs. displacement plot.

Partial Unload Partial Unload tests are a good way to get a fast representation of a sample that has different properties with respect to displacement (films, layers, surface effects, etc...). A Partial Unload test (due to the longer time required) is more susceptible to drift so the user should use caution when using results from a Partial Unload test.

XPM (Requires performech II) XPM testing can quickly map a large (up to maximum piezo scanner range) sample area and produce hardness and modulus with respect to area. XPM testing requires that a satisfactory in-situ image can be obtained of the sample surface and correct hardware is installed for the testing parameters.

5.4 PERFORM A TEST FROM THE OPTICAL FOCUSThe basic procedure for performing a test from the optical focus position is given below. This procedure assumes the

required calibrations have been satisfactorily completed.

Most TI series systems (MRNP and 3D OmniProbe transducers are not capable of in-situ imaging) can also perform

tests from the in-situ image position (discussed in the next section) which offers more precise placement and lower

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drift. Because of this, when possible, testing from the in-situ image position is the desired testing method. When

possible, testing within an automated method (discussed later in this user manual) can offer lower drift due to the

reduced X, Y, and Z-axis stage movements.

! All calibrations presented in the System Calibrations section must be satisfactorily completed prior to attempting to test a sample.

1. Move the optical focus over a defined sample space (Figure 5.12). This can be done by moving the X and Y-axis stage controls or right-clicking within a defined sample space on the stage map.

Figure 5.12 Move optics over a defined

sample space

2. On the Action bar, set the Mode of the system to the desired testing mode.

Figure 5.13 Select test Mode

3. Open or create the load function from the Load Function tab Indent or Scratch sub tab.

4. Modify the load function as desired by left-clicking the segment to adjust and modifying the parameters in the lower portion of the window.

5. Click the Perform Indent button (Figure 5.14) at the bottom of the respective load function tab to start the test.

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Figure 5.14 Click the Perform Indent button

to start an indentation test from the optical focus position

6. Click OK on the software prompt to continue with the test from the optical position (Figure 5.15).

Figure 5.15 Single Indent window

The system will move the stages to bring the probe into contact at the current optical focus position, perform the

necessary stage/piezo settle times (Figure 5.16) and drift monitor/correction (Figure 5.17), which takes

approximately 2 minutes, and then perform the user defined test.

Figure 5.16 Progress window

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Figure 5.17 Drift Monitor window

The Real Time Plot window (Figure 5.18) will display the load vs. displacement, displacement vs. time and load vs.

time plot as the test is performed. When the test has finished, the user will be prompted to select a directory and

filename (Figure 5.19) for the test and the system will move the stages back to the original optical position. The result

of the test will be displayed in the Analysis tab. Test analysis will be discussed in the Analysis section of this user

manual.

Figure 5.18 Real Time Plot window

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Figure 5.19 Save As window

! To prevent a system crash, it is important that the necessary system calibrations be completed prior to attempting to perform any test.

Testing can only be performed on defined sample boundaries.

Turn on the Automatic Save feature on the Load Function tab to save time while performing tests from the optical focus position.

5.5 TUNING FEEDBACK GAINSIt is important, when testing with load or displacement controlled testing, to ensure good feedback control during the

indentation. There are several gains (located within the Load Function tab) to control the probe during the test but for

most testing needs only a few of the gains are used.

Table 5.B Default gain settings Default Gain Settings

Three-Plate Capacitive Indentation MultiRange NanoProbe

Integral 1.0 1.0

Proportional 0.0 1.0 (displacement control)0.0 (load control)

Derivative 0.0 0.5

Adaptive 0.0 0.0

Preload Integral 0.2 0.1

Lift Integral 1.0 1.0

Lateral Proportional (if applicable) 0.5 0.5

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The Integral Gain has the biggest effect on the feedback controlled testing and will determine how strongly the force

or displacement signal will react to varying sample properties. If the Integral Gain is too low, the force or

displacement may not change quickly enough when there is an error from the requested load. If the Integral Gain is

too high, the force may react too quickly to small changes caused by noise, and oscillations will begin to appear on

the plot.

The Pre-Load Integral Gain setting is the integral gain setting during the drift monitor time. The force is not changing

during this hold, so the gain setting should be lower to avoid oscillations.

The Lift Integral Gain is the gain setting when the probe is in the air during the pre-indent lift height movement or

after the probe has come out of contact with the sample at the end of the indentation. During these times, the stiffness

of the contact is much less, and there is no damping from the sample.

In order to tune the gains for any particular sample, a few practice indentations at similar loads and loading rates

should be run. The Integral Gain can then be increased until oscillations occur. The Integral Gain should then be

reduced by about 30% for the best results. When the gains are tuned properly, the acquired data will plot directly over

the requested ramp on the real-time data plot. Examples of feedback control real-time plots are given in Figure 5.20.

If large oscillations occur due to improperly tuned gains, the displacement may exceed 5 μm (80 μm for MultiRange NanoProbe systems) and the user may receive a Displacement Limit Exceeded error.

Suggestions for tuning the gains are given below.

• Adjust the gains in small increments (by 0.1 up or down). A small adjustment in the gains will often result in dramatic effects.

• Try testing with the default gain settings first. The default gain settings work well for most samples and typically require very little adjusting.

• In general, higher gains will increase potential for noise-induced oscillations, and lower gains will cause the displacement to deviate from the requested ramp.

Lateral Integral (if applicable) 0.5 0.5

Lateral Derivative (if applicable) 0.0 0.0

Lateral Adaptive (if applicable) 0.0 0.0

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• Keep the adaptive gain near zero. Larger values will cause oscillations in most materials.

• Turn the proportional and derivative gains to zero to start. Use only the adaptive gain and integral gain to force the displacement to follow the load function then use the other gains to track small changes.

• Keep the derivative and proportional gains at a similar ratio when changing them. The derivative gain will act as a stabilizing factor to damp oscillations, but can also increase the effect of noise.

• If oscillations are observed at the point where the tip leaves the surface, lower the Lift Integral Gain, as this causes the oscillations in the air.

• Reduce the rate of the nanoindentation test. In some very stiff metal samples, the load has to change very quickly for a very small change in displacement. The feedback loop may have a difficult time in ramping the force this quickly to maintain the proper displacement rate so increasing the time will help.

Examples of incorrect gain settings for indentations on single crystal aluminum are given in Figure 5.20.

Figure 5.20 Feedback control gain

suggestions

DISPLACEMENT CONTROLLED TESTINGFor displacement controlled nanoindentation tests, it is best to start tuning the gains by running practice tests in the

air. If the gains are tuned properly in the air, they will be close to the correct settings on a sample. After setting the

gains from the air tests practice several nanoindentation tests on the sample in order to fine tune the feedback gains.

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Displacement controlled testing has a program to assist the user in tuning the PID gain settings. When a displacement

controlled nanoindentation or nanoscratch has been selected from the Load Function tab, an additional Tune PID

Gains button will appear. Selecting the Tune PID Gains button will open the PID Tuning window (Figure 5.21).

The PID Tuning window allows the user to modify and toggle the step response on and off as well as select which

axis (Z-axis [indentation] or X-axis [lateral axis]) gains to modify. When the step response is enabled a desired blue

step response will appear in the Step Response plot and a red (measured data) plot will appear over the plot. It is

desirable for the red and blue plots to follow closely (as shown in Figure 5.21). The PID gains can be modified in

real-time while the result continues to update on the Step Response plot. When satisfied with the gain settings, click

the Close button and the software will prompt the user to save the current gain settings. The gain setting will

automatically be populated in the Load Function tab.

Figure 5.21 PID Tuning window

! The desired gain settings are typically very near the default settings. Over-tuning the gains will cause severe oscillations within the transducer and cause an emergency stop loop that requires a software restart. Although the PID gains have slider bars that go from 0.0 up to 1000, the gains should be adjusted slowly and monitored to prevent any severe oscillation.

! DO NOT attempt to use the PID Tuning window when the system is performing a test or in contact with a sample.

The default step response in the PID Tuning window is 100 nm. If displacement controlled testing is being performed at much higher displacements the step response may not accurately represent the response of the system while the actual test is performed.

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5.6 TESTING TROUBLESHOOTINGHysitron systems are designed to be easy-to-operate and produce exceptional results under an array of conditions,

however, due to software settings or an incorrect order of operations the system may appear to be operating

incorrectly. This section is intended to diagnose and correct some of the most common testing issues encountered.

Cannot Approach Undefined Sample

Space

This error will be generated anytime the user attempts to approach a sample for imaging or testing and has not first defined the sample boundary. First define the sample boundary, perform a quick approach (if necessary) and then attempt to approach the surface for imaging or for testing.

System Timeout While Stepping Away

From the Surface

This error occurs when the system cannot successfully break contact with the sample surface. Likely causes for this are:

• Dirty probe• Dirty sample• Static charge on the sample • Very low setpoint value

If the user receives this error, the sample and probe should be cleaned (a probe cleaning procedure is given at the end of this user manual). The setpoint, as defined on the Imaging tab, should be verified and should be around 2 μN for successfully approaching most samples. If the problem persists, attempt to increase the setpoint to a higher value (10-20 μN) in an attempt to push through any debris or static charge that may be present on the sample surface.

Poor in-situ Image Quality

If the in-situ image quality is streaky or blurred the issue is likely one or more of the following:

• Dirty probe• Dirty sample• Very low setpoint value• Incorrectly set integral gain value

If the image quality is very poor, the sample and probe should be cleaned. The setpoint value should be adjusted to a reasonable value (1-2 μN) and the imaging integral gain value should be set to 90 for TI series systems (small adjustments can be made after obtaining a reasonable image).

Hardness and/or Modulus Results Vary

with Indentation Load

Most samples will show varying hardness or modulus as the load is changed and the probe is driven further into the sample. However, if the results are suspect, it is best to verify the system operation by performing similar force indents on the standard fused quartz sample to check for system consistency. If the values are not consistent on fused quartz, then there may be an issue with the system that can be the result of a number of issues including:

The Probe Shape has Changed

When the modulus of fused quartz is not showing approximately 69.6 GPa the probe calibration may be incorrect. This is the most common issue when inconsistent hardness and modulus values are under question. It is a good idea to check the calibration of the probe as often as possible. The calibration can be easily checked by making a few indents at various loads on the fused quartz sample and verify that the hardness and modulus values are close to the expected values.

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The Machine Compliance Value is

Incorrect

If, after performing a probe calibration, the modulus is showing 69.6 GPa, but the hardness is showing a linearly increasing or decreasing trend, the problem may be an incorrect machine compliance value. When the machine compliance parameter is set too low, the hardness will increase with depth. If the machine compliance needs to be increased a considerable amount to correct the problem, it is a sign that the probe or transducer is poorly mounted or loose; consider remounting the probe and transducer.

The Probe is Dull With dull probes, the hardness value may show higher or lower values as the force is decreased. This effect is usually most visible when the contact depth approaches about 20% of the radius of curvature of the indenter probe. The reason for this is that the indents at these loads are mostly elastic and the hardness value will have a large elastic component. This causes the hardness values to deviate from the mostly plastic values seen at higher forces.

XPM Testing The most common issue with XPM testing is the testing is performed too quickly for the hardware. If the time between tests is performed too quickly there will be obvious waviness in the individual XPM files due to piezo overshoot/ringing and insufficient settle time for the piezo between tests. Increase the time between tests and run the XPM test again.

Figure 5.22 XPM test performed too fast

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in-situ SPM Imaging Procedure

CHAPTER 6 IN-SITU SPM IMAGING PROCEDURE

in-situ SPM imaging is not available with MultiRange NanoProbe (MRNP) or 3D OmniProbe transducers. To use the

in-situ imaging capabilities the three-plate capacitive (or nanoDMA/nanoECR) transducer and piezo scanner must be

installed.

! This procedure assumes the calibrations required for the instrument have been satisfactorily completed.

The basic procedure for performing an in-situ image of a defined sample space is:

1. Optically locate the area of interest within a defined sample boundary.

2. On the Imaging tab click the Approach button (Figure 6.1) or from the menu bar click Engage Approach.

Figure 6.1 Approach button

3. The system will move the stages to bring the probe into contact with the sample surface at the currently defined sample setpoint value (default value is 2 μN).

4. The Progress window will close when the probe has reached the defined setpoint value.

5. Click the Go button (Figure 6.2) or from the menu bar click Control Start Scan to start scanning the sample surface.

Figure 6.2 Go button

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Image parameters (scan size, setpoint, integral gain, etc…) can be changed while the system is scanning. Images can

be saved by clicking the Camera icon or Image Capture from the menu bar. When imaging is complete, click the

Withdraw button (Figure 6.3) or from the menu bar Engage Withdraw.

If the TriboScan background flashes red when a parameter or button is selected, this indicates the software is currently busy performing a stage move, piezo move, test, or other function. Wait for the current function to complete and then attempt to access the parameter or button.

Figure 6.3 Withdraw button

When capturing an image of the sample surface, the system will capture the next full scan (top to bottom or bottom to top) that has been completed without modifying any of the Imaging Controlsparameters.

! To prevent a system crash or hardware damage, it is important that the necessary system calibrations be completed prior to attempting to perform any test.

Testing can only be performed within a defined sample boundary.

6.1 SCANNING WEAR TESTINGA scanning wear test is performed by scanning an area a prescribed number of passes at an elevated setpoint and then

measuring the height difference from the surrounding area to calculate the amount of material worn away.

The procedure given below is for a manual scanning wear test. TriboScan is equipped with a Scanning Wear load function tab that allows the user to define more complex scanning wear tests (with varying loads or scan passes). For more information, refer to the section after the manual scanning wear test. The analysis given at the end of this section is valid for both the manual scanning wear tests and the tests created with the Scanning Wear load function tab.

The procedure for a basic scanning wear test is:

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1. Approach the sample surface from the Imaging tab.

2. Set the scan size and wearing setpoint force (typically much higher than a standard scanning setpoint... 10 μN, 20 μN, etc...).

3. Scan the sample surface. The number of passes is shown at the left side of the upper left in-situ image.

4. When the desired number of passes have been completed, change the setpoint to a reasonable, standard imaging setpoint (typically 1-2 μN).

5. Increase the scan size to a size larger than the scanning wear test (typically, twice the scanning wear region works well).

6. Scan the sample surface and capture the resulting image.

The wear volume can be computed by analyzing the saved image in TriboView. Open the image in TriboView and

select Tools Roughness Sub Image (Figure 6.4) and draw a rectangle over the worn area as well as the area

either above or below the worn area to measure the average heights (Figure 6.5).

Figure 6.4 Measuring roughness within

TriboView

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Figure 6.5 Calculating wear volume with

TriboView

The wear volume is given as the square of the scan size multiplied by the measured wear depth. In the example given

in Figure 6.5, the average height of the 5 μm square worn area is -0.289 nm and the average height of the non-worn

area is -0.108 nm:

|Height outside wear region [nm]| - |Height inside wear region [nm]| = Wear height [nm]

| -0.108| - |-0.289| = 0.181

(Square of wear scan size [μm]) (wear height [μm]) = Wear volume [μm3]

(52) (0.181 10-3) = 4.53 10-3 μm3

Scanning wear testing will dull nanoindentation probes much more quickly than nanoindentation or nanoscratch testing.

6.2 TESTING FROM THE IN-SITU IMAGING POSITIONSince the probe is already in contact with the sample surface while performing an in-situ image, testing from the in-

situ imaging position typically results in lower drift rates and can usually be performed much more quickly than

testing from the optical position. Because of this, Hysitron recommends, when possible, to perform tests from the in-

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situ imaging position. The basic procedure for executing a nanoindentation or nanoscratch test while performing an

in-situ SPM image is:

1. Approach the surface and image the sample as described in earlier in this section.

2. While imaging the sample surface, go to the Load Function tab Indentation, Scratch, Scanning Wear, or nanoDMA sub tab and either open or create a load function. Leave the desired load function open on the Load Functiontab.

3. On the Imaging tab, locate and center the area of interest using the stage and/or piezo offsets. The test is always performed in the center of the in-situ image.

4. Click the Test button (Figure 6.6) or from the menu bar click Control Test.

Figure 6.6 Test button

To perform a scanning wear test, select the button next to the Test button:

The system will automatically stop scanning and move the probe to the center of the in-situ image, perform the

necessary stage/piezo settle times and drift correction (approximately 1.5 minutes) and then perform the user defined

test.

Similar to performing a test from the optical position, the real-time plot of the load vs. displacement, displacement vs.

time and load vs. time plot as the test is performed (prior to drift correction) will be displayed. When the test has

finished, the user will be prompted to select a directory and filename for the test and the system will resume scanning

the tested region.

Performing a test from the in-situ imaging position will perform the currently defined load function for the currently selected Mode (nanoindentation, nanoscratch, etc…) of the system.

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The nanoindentation probe cannot be in contact with a sample surface when changing the Mode of the system. If the Mode is changed while in-contact with a sample surface, TriboScan will force the probe to be disengaged and then automatically re-engage the sample surface.

6.2.1 PIEZO AUTOMATION PROCEDUREPiezo Automations are always set up from the in-situ imaging position and can only be executed if the

nanoindentation probe is in contact with a sample surface.

Although there are additional options available within the Piezo Automation sub tab, this procedure is a basic

overview to perform a standard piezo automation. As the user becomes more familiar with the system, additional

options can be explored (a full description of all available options is given in the Software chapter of this user

manual).

1. Set the system Mode pull-down menu (Figure 6.7) to the desired testing mode (nanoindentation, nanoscratch, etc…)

Scanning wear test automations are performed with the system in Indentation mode and the Scanning Wear Test check box selected (Figure 6.10).

Figure 6.7 Mode pull-down menu

2. Approach the sample surface from the Imaging tab and begin scanning the sample surface as outlined in the in-situ SPM Imaging section of this user manual.

3. With the system performing an in-situ image of a sample surface, go to the Load Function tab and set up the load function to be performed (must be the same type of load function as defined by the Mode pull-down menu). Leave the desired load function open.

4. Go to the Automation tab Piezo Automation sub tab (Figure 6.8).

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Figure 6.8 Piezo Automation sub tab

5. Select the type of Script Mode to perform (Figure 6.9):•Array Script will perform a rectangular array of tests over the sample

surface.•Click Script will display the current in-situ image and allow the user to

left-click to select testing locations.

Figure 6.9 Script Mode pull-down menu

6. Either choose Array Script and define the number of tests to perform in X and Y with a spacing between each test (Figure 6.10) or choose Click Script and left click the desired locations on the displayed image to define the test locations (Figure 6.11).

Figure 6.10 Array Script options

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Figure 6.11 Click Script options

The Total Distance parameter given while creating an Array Script piezo automation cannot exceed the current in-situ SPM image scan size.

7. In the lower, center area, the user can insert a time delay before the first test and between each of the following test (Figure 6.12). Depending upon the desired test placement accuracy, these times will likely need to be increased (perhaps 240 sec and 120 sec, respectively). Additional options include, Save Scan (saves post-test image in the currently defined directory from Imaging tab; user preference), Stay In Contact (keeps the probe in contact following the tests; typically not recommended) and Re-Zero Lift Height (height the probe will lift off of sample surface to re-zero controller between tests; 100 nm default works well for most samples).

Figure 6.12 Piezo automation testing

options

8. Click the Run Piezo Automation button, the system will automatically stop scanning the sample surface and move the probe to the center of the image.

9. When prompted, select a directory and click OK (Figure 6.13).

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Figure 6.13 Selecting directory for saving

piezo automation data

10. When prompted, select a base file name and click OK (Figure 6.14).

Figure 6.14 Selecting base file name for

piezo automation data

11. When prompted, enter the beginning force and ending force for the array of tests (fewer options are available with nanoscratch and nanoDMA piezo automations) and click OK (Figure 6.15).

Figure 6.15 Piezo automation load

adjustment parameters

When the piezo automation has completed the software will return to the Imaging tab and the data files will be saved

to the desired directory.

Unless the user has selected the Stay In Contact option, the probe will Disengage from the sample surface and will

either require an Engage command to continue scanning the sample surface or a Withdraw command to go back to the

optical focus position.

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If a test during an automated method exceeds either the force or displacement limit of the system, the test will end and the method will attempt to perform the next test in the sequence without saving any data for the prematurely ended test. If an automated method completes with fewer then the prescribed number of tests, this is a likely cause for the discrepancy.

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Automated Method Testing

CHAPTER 7 AUTOMATED METHOD TESTING

Automated testing methods are always set up from the optical position and cannot be accessed, modified or executed

if the nanoindentation probe is in contact with a sample surface.

There are many options available within the automated testing methods side tabs (discussed in the previous sections).

This procedure is an overview to perform a basic grid array automated testing method. As the user becomes more

familiar with the system, additional options can be explored.

1. Go to the Automation tab Methods sub tab.

2. Select the New Method button to enter the method name, type, file name, and directory.

3. Set a simple grid Pattern to be performed at the sample location(s) by clicking on the Simple Grid radio button (Figure 7.1).

Figure 7.1 Pattern Selection area

4. Set a value for the Rows, Columns, and Spacing between tests.

5. If the pattern will be performed at more than one location, select the Positionside tab, create a new Position Group, move the X and Y-axis stages to define Positions for the pattern to be performed (not required if performing the pattern at one location).

6. If a Position Group was created, select the group from the Indent pattern using positions in option (Figure 7.2). If the Pattern will be performed at only one location, select the Pattern, Starting at the Current Optic option (Figure 7.2) and make sure the optics are located over the area of interest.

Figure 7.2 Target Positions area

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7. Click the Load Function button (Figure 7.3).

Figure 7.3 Load Function button

8. Load the desired load function by selecting the Select load function button. Choose how to modify the load or displacement over the range of tests being performed with the radio buttons and start/end load values. Click OK when finished.

Figure 7.4 Load Function Setup window

9. Save the Workspace by clicking the small down arrow [ ] in the upper left of the Action Bar, which saves all automated methods, positions, and patterns.

10. Click the Start Method button and follow any additional on-screen direction.

When the automated testing method has finished a status window will appear showing the number of tests completed.

The automated testing method, pattern, groups, and pattern positions will be saved with the workspace and can be

reused for future automated methods.

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If a test during an automated testing method exceeds either the force or displacement limit of the system, the test will end and the method will attempt to perform the next test in the sequence without saving any data for the prematurely ended test. If an automated testing method completes with fewer then the prescribed number of tests, this is a likely cause for the discrepancy.

The user cannot save over the existing system Default workspace, the user must choose the Save As... option the first time to choose a name for the workspace.

To chain multiple automated methods (differen load functions, different test types, etc...) the user should create each

method individually then use the Method Chain button to link the methods together.

7.1 COMBI UTILITYThe Combi® software utility is used to set up position groups for testing of a circular or rectangular combinatorial

wafer. The high-throughput wafer testing is made easy by obtaining the list of positions, locations on various samples

on the wafer, which could be used in a method type testing. This procedure helps in automating the testing process for

as many as 1000 samples on a single wafer. The nomenclature of the data files obtained from indentation tests is

made very logical by implementing the row and column convention for naming the samples. The following procedure

needs to be performed, based on the shape of the wafer, to setup the wafer positions. Typically the wafer is mounted it

on a vacuum chuck. It is advised to put the wafer in the exact alignment that was used to generate the text file.

COMBI POSITIONS SETUP PROCEDURETypically, wafer manufacturers provide the X/Y-axis spacing for the samples on the wafer. Make a note of the X and

Y-axis spacing for future use. If the X and Y-axis spacing is not provided, it can be calculated using the system optics.

Calculations can be performed by optically choosing the corners of the samples and calculating the distance between

the points using the X and Y-axis coordinate values as measured with TriboScan.

CIRCULAR WAFER (WITH CIRCULAR OR RECTANGULAR SAMPLES)1. Place the circular wafer on a clean surface in such a way that the only straight

edge of the wafer, provided for alignment, is positioned at the front of the instrument.

2. Open the a blank Notepad document (Start Program Files Accessories Notepad). Create a new, blank text file and save it with an appropriate name.

3. Create three columns with names: Row, Samples and Shift in the text file, as tab delimited (Figure 7.5).

4. On the wafer, locate the longest row with the most number of samples on the wafer. An example is row 2, 3 or 4 in Figure 7.6. The Shift for this row is 0.

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5. Locate the bottom most row. This row is termed as Row 0.

6. Count the number of samples in this row.

7. Count the number of sample offsets on this row with respect to the longest row, from the left.

8. Input the data in the text file below the text of the column names, created above in step 3, as 0, 3, 2 as tab delimited.

9. Perform steps 6 through 8 for consecutive rows, going upwards (Figure 7.5 is a text file that corresponds to Figure 7.6).

10. Save the completed text file.

Figure 7.5 Combi utility text file

Figure 7.6 Combi circular wafer setup

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The Combi positions setup procedure can be initiated from the Automation tab Position side tab. The Combi utility

requires an empty group for building the position locations so first click New under the Position Groups heading and

create an empty group then click the Combi setup button located on the right side of the window.

The Combi Setup button initiates the COMBI Panel. The type of wafer being used for the test, either Circular or

Rectangular is selected from this window.

Figure 7.7 Combi Panel

When the Sample type is selected, a window will prompt the user to load the text file that was created earlier with the

row, sample and shift information. For circular wafer samples, the measured X and Y-axis spacing are input in the

respective fields.

The Sample type must be selected even if the desired sample type is already displayed, to initiate the Load Text File window, the Sample type must be re-selected.

RECTANGULAR WAFER (WITH CIRCULAR OR RECTANGULAR SAMPLES)Rectangular wafer setup assumes that the number of samples on each row is the same, there is no offset between the

sample columns and the X/Y-axis spacing is consistent over the surface of the sample.

Unlike a circular wafer, a rectangular wafer does not require the creation of a text file to setup the test, however, X/Y-

axis spacing values are needed to setup the test. For a rectangular wafer the window in Figure 7.8 will open up after

selecting the sample type.

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Figure 7.8 Wafer Details Panel

Input the X/Y-axis spacings along with the number of rows and number of columns of samples on the wafer. The

Total # Samples parameter will display the total number of samples available on the wafer. When finished, click OK.

WAFER ANGLE/SAMPLE SHAPEWith the sample type/spacing entered for the wafer type, the angle of orientation of the samples on the wafer must be

calculated. In the COMBI Panel, click the Calculate Angle button.

To calculate the wafer angle of a rectangular sample, optically locate a position on the wafer sample, the top-left

corner of a sample in a row, and click the Top-Left button in the COMBI Panel (Figure 7.9). This function selects the

specified location. Click the Confirm Point button, which in turn reads the co-ordinates of the specified position.

Then, move horizontally to the farthest sample in that row, linearly, and locate another position, the top-left corner of

the last sample in that row, and click the Top-Right button followed by the Confirm Point button. This will read the

coordinates of the right position and accordingly calculate the wafer angle and display it on the Wafer Angle text field

on the COMBI Panel.

With the calculated angle displayed on the panel, the general outline of a sample must be identified. Optically go to

the left most, first sample on the first row from bottom, and perform the following procedure with respect to the

sample shape on the wafer.

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Figure 7.9 Calculate wafer angle & sample

shape

The procedure for defining the sample shape for a circular or rectangular sample is given as:

1. Locate the top or top-left corner of the sample, click the Top or Top-Left button and click the Confirm Point button.

2. Move to the right or top-right corner of the sample, click the Right or Top-Rightbutton and click the Confirm Point button.

3. Move to the bottom or bottom-right corner of the sample, click the Bottom or Bottom-Right button and click the Confirm Point button.

4. Move to the left or bottom-left corner of the sample, click the Left or Bottom-Left button and click the Confirm Point button.

When the sample shape has been defined, click the Done button. This will generate a list of positions in a serpentine

manner. The position names are based on the row and column numbers from the wafer. The group is now filled with

the new positions in the Positions Group panel. This group can be used to describe a method positions to run a

method type of indentation test on the wafer samples.

Clicking the Preview button on the Positions area will start the preview process to view the locations of each of the

test points. The preview process can be time controlled and if the user feels a need to change the position coordinates,

as in a case where the test surface is flawed or dirty, the user can move around optically and locate a better location

and save the new position coordinates with the old position name.

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SECTION | TI SERIES ANALYSIS• Indentation, nanoscratch, XPM, and in-situ SPM imaging analysis

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CHAPTER 8 ANALYSIS

Detailed descriptions of the various TriboScan software tabs is given in the Software section and will not be covered

in the Analysis section. For information on the particular function, button or parameter that is mentioned but not

discussed within the Analysis section, refer to the appropriate tab within the Software section for a more thorough

description.

The analysis procedures presented below are for standard test types performed on standard samples. Analysis routines will vary for samples, testing conditions, and the information the user is attempting to obtain.

8.1 SINGLE INDENTATION TEST ANALYSISThe basic procedure for performing nanoindentation analysis is given below. The test that is being analyzed in this

section is a fused quartz sample. The following procedure can be used to calculate reduced modulus and hardness

from a bulk ceramic, metal, or hard polymer. Analysis for softer polymers (polymers with large amounts of creep or

adhesion), films, or other sample types will require different testing parameters and analysis routines and the user

should contact Hysitron for further support.

OPEN THE NANOINDENTATION CURVEOpen the nanoindentation curve to analyze from the Analysis tab Quasi sub tab Quasi sub tab by using the

Open button or File menu Open menu. The curve will be plotted in the software. If the test is a nanoDMA III data

file the associated nanoDMA data will automatically be loaded in the nanoDMA sub tab as well.

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Figure 8.1 Nanoindentation curve

displayed in Quasi sub tab

EVALUATE THE VALIDITY OF THE CURVEBefore analyzing the curve the user should evaluate the validity of the curve. The validity of the curve will depend on

many factors that are sample, probe, and test specific. However, evaluating the validity of the curve will typically

include verifying the following:

1. Proper lift segment (Figure 8.2). Verifying the curve has a flat lift segment (indicating the probe was able to start the test out of contact with the sam-ple). If the lift segment is not flat the test may need to be performed with a larger lift segment. Open loop tests will not have a lift height and the probe will start in-contact with the sample.

2. Correctly identified origin (Figure 8.2). Verifying the curve origin is at the point where the force starts to increase (indicating the probe has contacted the sample). If the curve is not at the correct origin point the Force and/or Displacement Offset buttons should be used to correctly orient the curve.

Figure 8.2 Verifying lift segment and

correct origin of curve

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3. No evidence of dirty sample, dirty probe, or poorly mounted sample (Fig-ure 8.3). This will typically be presented as s large increase in displacement at the beginning of the test with very little increase in force. If this is observed the sample and probe should be cleaned. If it continues the sample should be remounted.

Figure 8.3 Identifying dirty sample, probe,

or poorly mounted sample

4. Drift rate is reasonable (Figure 8.4). The drift rate can be viewed from the Editbutton, however, incorrectly measured or excessive drift would be indicated by an unexpectedly poor nanoindentation curve or a negative displacement measured during the hold (dwell) segment. Using a shorter hold time during the test may reduce the effects from a large or unstable drift rate.

Figure 8.4 Incorrectly measured or

excessive drift rates

5. Sample creep is minimal (Figure 8.5). For samples exhibiting creep behavior the load function should be performed with an adequate hold (dwell) time to allow for creep to settle before removing the maximum load. A bow shaped unloading curve is a good indication that the hold time is not adequate for the sample/test.

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Figure 8.5 Hold time is not adequate for

sample creep

6. Loading curve is free from dislocations and fractures (Figure 8.6). A loading curve showing sudden jumps in displacement or load would indicate the sample is fracturing or there are dislocations. Curves showing dislocations or fractures are typically relevant for the events and not the fitted reduced mod-ulus and hardness values.

Figure 8.6 Dislocations or fractures in

loading curve

VERIFY THE FITTING PARAMETERSThe fitting parameters that determine the calculated reduced modulus and hardness values are located in the bottom

right of the Analysis tab Quasi sub tab Quasi sub tab (Figure 8.7).

1. Verify the Upper Fit % and Lower Fit % produces a reasonable fit to the tan-gent of the initial unloading portion of the final segment. The default values will fit well for most ceramics, metals, and hard polymer samples.

2. Verify the Unloading Segment is set to the number of the unload segment in the test performed. Selecting the Auto check box will automatically fit the final segment (typically the unload segment for most tests).

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3. Verify the test origin (where the probe contacts the sample and force begins to increase) is at the zero force and displacement point. If the test is not at the zero force and displacement point the Force and Displacement Offset but-tons and associated parameters may need to be tuned.

4. Verify the Area Function pull-down menu is set as desired. If the From Tip Area Tab is selected the user must be certain the correct area function is loaded into the Calibration tab Tip Calibration sub tab Define sub tab.

Figure 8.7 Nanoindentation fitting

parameters

EXECUTE THE FITAfter verifying the curve is valid and the correct fitting parameters are being used the final step is to click the Execute

Fit button (at the bottom right of the Analysis tab Quasi sub tab Quasi sub tab) and record the reduced modulus

and hardness values (as well as other values such as contact depth, contact stiffness, etc...) given in the top right of the

Analysis tab Quasi sub tab Quasi sub tab. If the fit is not satisfactory, the user can adjust the fitting parameters

and click the Execute Fit button again.

8.1.1 PLOT MULTIPLE CURVESThe Plot Multiple Curves and the Multiple Curves Analysis options are available from the Analysis tab Quasi sub

tab Quasi sub tab Analysis menu. These two features will allow the user to plot and analyze (or just analyze)

multiple curves using the same fitting parameters defined on the Analysis tab Quasi sub tab Quasi sub tab.

These two commands can be useful when comparing samples or trying to fit and export multiple files.

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Following a Multiple Curve Analysis a single, tab-delimited text file will be created with a row for each data file and

a column for each fitted parameter given on the Analysis tab Quasi sub tab Quasi sub tab.

8.1.2 PARTIAL UNLOAD ANALYSISHysitron instruments have the capability to perform a partial unload test where a small force is applied by the

nanoindentation probe, withdrawn and then a slightly higher force is applied, withdrawn, and so on for a prescribed

number of cycles. Because a partial unload load function consists of several unloading segments, an alternate analysis

routine is required to properly extract data from this type of test.

Partial unload tests are normally created from the Load Function Generator which can be accessed from the Load Function tab Indentation sub tab Load Func. Gen. button.

To analyze a partial unload data file, right-click the Execute Fit button on the Analysis tab Quasi sub tab Quasi

sub tab. A window will prompt the user if they would like to update the graph after each fit (Figure 8.8). Selecting Yes

will take longer but display the real-time fit for each unloading segment.

A window will prompt the user to select which segments to analyze (Figure 8.9). Enter the number of the first

unloading segment (typically 2 or 3) and click OK.

All partial unload analysis data is saved as a *.txt file (with the same name as the *.hys but different extension) and is

displayed in the standard hardness/reduced modulus versus contact depth plot. The data will automatically be opened

in the hardness/reduced modulus versus contact depth plot upon clicking Save.

Figure 8.8 Update graph after each fit

prompt

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Figure 8.9 Select segments to analyze

prompt

There are also two options for analyzing multiple partial unload curves from the Analysis tab Quasi sub

tab Analysis menu Multiple Curve Analysis Partial Unload FMT 1 or Multiple Curve Analysis Partial

Unload FMT 2. Format 1 produces standard hardness and reduced modulus values whereas format 2 produces

hardness and Young’s or indentation modulus values but requires that the user know Poisson’s ratio for the sample.

Both formats will prompt the user to select files to analyze and prompt the user to enter which segments to analyze

(similar to Figure 8.9)

8.2 XPM ACCELERATED PROPERTY MAPPING ANALYSISXPM (accelerated property mapping) test results are loaded through the Analysis tab Quasi sub tab Quasi sub

tab OR Analysis tab Quasi sub tab XPM sub tab. A result will be displayed in the Quasi sub tab AND XPM sub

tab. Analysis for XPM test results should only be performed in the XPM sub tab because the Quasi sub tab will not be

able to properly offset each test or fit all segments. An example of what the Quasi sub tab would display with a

standard XPM test is given in Figure 8.10.

To properly offset the data and to fit the multiple segments XPM test result analysis should only be performed in the XPM sub tab.

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Figure 8.10 Quasi sub tab result after

loading XPM test

To load the XPM test in the XPM sub tab select the File Select File for Analysis. The user will be prompted to

select a Number of Segments for Each XPM Load Function (usually three), Segment Offset (usually zero unless

additional indentation segments are added prior to the XPM portion of the test), and Preload Used for XPM (usually

setpoint preload unless otherwise selected).

Selecting the Analyze Current File button on the XPM sub tab will perform the same function as the Select File for Analysis command.

Figure 8.11 XPM Analysis Parameters

window

The data file will be loaded after selecting OK on the XPM Analysis Parameters window (Figure 8.12). Individual

XPM segments can be removed from the plotted data with the Remove button at the bottom of the XPM sub tab and

the XPM plots (temperature maps) can be saved from the File menu as *.BCRF files for analysis in TriboView.

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Figure 8.12 XPM test result

8.3 NANOSCRATCH ANALYSISAccess the Scratch Data Analysis window by selecting Analysis tab Scratch sub tab. The resulting window

contains four graphs and is shown in Figure 8.13. Normal force, normal displacement, lateral force, and lateral

displacement are all plotted as functions of time. The normal force versus time and lateral displacement versus time

graphs should match the plots that were defined by the user in the Scratch load function sub tab.

The red indicator bars relative and absolute positions are given in the upper right portion of the Scratch Data sub tab

and can be used to measure distance to or between delamination points on films or other events. The indicator bars

can be moved by left-clicking and dragging the mouse on any of the four plots. The indicator bars will move to the

same time location on all plots.

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Figure 8.13 Scratch Data analysis tab

The measured Z-axis displacement is a combination of the probe moving into the sample and the tilt of the sample.

This sample tilt can, and should be removed, so that only the displacement of the probe into the sample is plotted on

the Z-displacement graph. Because the first segment of a scratch traces across the sample surface along the same axis

as the scratch (at the setpoint force), this segment can be used as a measurement of the slope of the sample along that

same direction. This measurement can be used to remove the tilt effects from the final scratch data.

The tilt correction process (using the Tilt Correction button) is described in the following steps and corresponding

Figure 8.14:

1. Perform a valid nanoscratch test with a segment designed for performing tilt correction. This is typically a very light scratch (near the setpoint value) per-formed from the origin position of the probe to the beginning location of the scratch.

2. Open the valid nanoscratch test in the Analysis tab Scratch sub tab Scratch Data sub tab.

3. Left-click and drag the two red indicator bars on any visible plot so that one is positioned at the beginning of the tilt correction segment (usually the first segment of the test) and the other is positioned at the end of the tilt correc-tion segment.

4. Click the Tilt Correction button. The segment normal displacement will be lin-earized and the remainder of the normal displacement data for the scratch test will be adjusted to remove the tilt of the sample.

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The tilt correction is not saved with the data file and must be performed each time the file is opened.

Figure 8.14 Tilt correction process

The coefficient of friction can be automatically computed by clicking the Friction button located halfway down on

the right side of the Scratch Data sub tab (Figure 8.15). This will open the coefficient of friction versus time plot

(Figure 8.16).

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Figure 8.15 Location of Friction button

Figure 8.16 Coefficient of Friction vs. Time

plot

The coefficient of friction versus time plot, given in Figure 8.16, represents all segments of the scratch load function.

Typically, the first and last two or three scratch segments are used for positioning the probe and the only segment of

interest is the segment that performs the scratch. To view only the segment that performs the scratch, select the

Segment Plotted pull-down menu (Figure 8.17) and select the scratch segment. If the Friction button is selected now,

only the segment of interest will be plotted (Figure 8.18).

Figure 8.17 Segment Plotted pull-down

menu

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Figure 8.18 Coefficient of Friction vs. Time

plot of scratch segment only

SCRATCH DATA ANALYSIS TIPS• Periodically check the Lateral Axis calibration. The ESF and plate spacing can

change based on temperature or humidity differences.

• Averaging of the data is possible by either clicking on the Edit icon on the Scratch Data sub tab or by going to File Edit File Constants and changing the # to Average value at the bottom of the dialogue box.

• The data can be exported as a tab delimited ASCII text file by clicking the Export Text File button on the Scratch Data Analysis toolbar or by selecting File Export Text File. The file exported is identical to the currently displayed *.hys file. It will create a new text file with the same name, in the same directory as the currently open file with a *.txt extension.

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CHAPTER 9 IN-SITU SPM IMAGING ANALYSIS

Hysitron TI series systems include TriboView in-situ imaging analysis software. TriboView is a 2D and 3D *.hdf

image viewer that can be used to apply background subtractions, measure surface properties and save images as other

formats.

TriboView is accessed from the Analysis tab Image sub tab or by accessing the C: Program

Files Hysitron TriboView.

Due to software conflicts and system resources, TriboView may not be accessed from the Analysis tab Image sub tab while TriboScan is performing an in-situ SPM image. Withdraw the probe from the sample to access TriboView or access TriboView from the windows directory listed above while performing an in-situ SPM image.

This user manual is written with TriboView 5.9. If the instruction in this user manual does not match your version of

TriboView contact Hysitron for a software upgrade or an alternate user manual that more closely follows your version

of TriboView.

To view previously saved *.hdf (legacy in-situ image) or *.bcrf (SPM+ in-situ image) files, select the directory that

the images have been saved in by clicking File Choose Image Folder or by clicking the blue colored file path

from the Image Browser (TriboView main window). If the user wishes to open only a single image, this may be

performed by selecting Open… instead of Select Image Directory. The window in Figure 9.1 will open.

Figure 9.1 Select Image Directory window

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From this window, the directory that contains the desired images can be selected. The images do not need to be

individually selected, but they should be located in the selected directory. When the appropriate directory is selected,

click Done.

The Image Browser window will show thumbnails the images from the selected directory, and will look similar to

Figure 9.2. From this window, the individual images can be opened for viewing by double clicking on the thumbnail

of the desired image.

Figure 9.2 Image Browser

When the mouse pointer is placed over an image, the details (file name, time and date created) of the file are given in

a pop-up box (Figure 9.3). Double left-clicking on an image from the Image Browser will open the image in the

Image window. The Image window is where the image manipulation is performed and is shown in Figure 9.4. The

image is displayed as a separate window, and can be manipulated using the different functions available in the tabs of

the Image Browser window.

Figure 9.3 Information available by

hovering the mouse over an image thumbnail

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Figure 9.4 Image window

The tabs of the TriboView software are discussed below.

Browser The Browser tab is where the image files can be selected for analysis and manipulation. Double left-click on an image thumbnail to open the image for further analysis.

Section The Section tab is where the cross-section line information is displayed. A cross-section is created by left-clicking on the image. Red and green indicators can be placed on the cross-section by selecting the points on the Section tab (a corresponding red and green indicator will appear on the image).

To view cross-section information (after selecting a cross-section) go to the Info tab and select Section Analysis from the pull-down menu.

Figure 9.5 Section tab

Histogram The Histogram tab gives a plot representing the distribution of the Z range in the image. The color of the image can be adjusted by moving the blue slider bar or adjusting the Minimum Value and Maximum Value parameters; the Brightness and Contrast can be adjusted with the coresponding parameters.

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Figure 9.6 Histogram tab

Background Subtraction

The Background Subtraction tab is where the user can select from the different imagie flattening options. Four choices are given for different types of background subtraction:

• None• Linear Regression• Average Plane• Zone

Figure 9.7 Background Subtraction tab

Background subtraction helps to account for any tilt that may be present on the surface of the sample. If None is selected the image will appear just as the sample was originally imaged. If there is too much tilt, the colors in the image may become saturated from the elevation change from one side of the sample to the other. This can hide many features on the surface of the sample. Background subtraction removes this tilt and allows surface characteristics to be more easily viewed.

Linear regression will remove the tilt from the sample on a line-by-line basis. Average plane will remove the tilt by considering the entire image and then perform the tilt removal. Zone subtraction will remove tilt based on two zones assigned by the user. Usually linear regression or average plane will result in a more balanced image. The different background subtraction routines available from TriboView are given in Figure 9.8. Linear regression, zone, and none are the background subtraction routines available in real-time while performing an in-situ SPM image in TriboScan. Average plane is only available in TriboView.

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Figure 9.8 Background subtraction routines

available from TriboView

Color Table The Color Table tab gives a list of available color scales to apply to the image. The default color scale is Brown.

Info The Info tab displays information about the image. The option sin the pull-down menu on the Info tab are given below.

• Image Info Basic image information.

• Roughness Analysis Image rougness information can be viewed under this pull-down menu by first selecting Tools Roughness Whole Image or Sub Image.

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• Section Analysis Section analysis information can be viwed under this pull-down menu by first selecting a section on the current image.

• File Header The file header infomration is given for *.bcrf (SPM+) image files only.

Figure 9.9 Info tab

There are several menu items available from the TriboView software. Some menu items have cooresponding tab

selections (discussed above). The menu items will be discussed below.

File The File menu contains the commands to open, save, and print the image files.• Open: Open a single image file• Choose Image Folder: Open multiple images in image browser• Browse Current Image Folder: Returns to Browser tab• Recent Folders: Displays the most recently accessed folders• Save Image As: Saves current image as *.TIF, *.BMP, *.PNG, *.TXT, *.BCRF• Save Profile as ASCII:. Saves current cross-section to *.TXT• Print Image: Prints current image to availble printer• Print Info Text: Prints current Info tab• Exit: Exits TriboView software

Edit The Edit menu contains commands to copy the image or image information.• Copy Image to Clipboard: Copies current image to computer clipboard• Copy Image with Scale Bar to Clipboard: Copies current image with scale

bar information to computer clipboard• Copy Plot to Clipboard: Copies current plot in Section tab to computer

clipboard• Copy Info Text to Clipboard: Copies current Info tab to computer clipboard

View The View menu contains commands for adjusting the image size and cursor preferences.

• View Section Analysis: The View Section Analysis command displays the Info tab Section sub tab next to the Section tab

• Zoom: The Zoom command adjust the image size• Cursor Color: The Cursor Color command changes the color of the section

line and remove lines cursor

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Tools The Tools menu contains commands to edit and analyze the image.• Remove Lines: While imaging a sample, an occasional bad scan line is

possible due to surface debris or external noise. These scan lines can be removed by blending adjacent scan lines. The pointer can be used to maneuver a bar of the desired size over the line(s) to be removed. Left-clicking on the bad scan lines in the image will cause them to blend into the adjacent lines.

• Roughnes: Roughness information can be obtained for the entire sample or for a small, user defined, sub sample. If Sub Image is selected, left-clicking on the sample image and dragging it will create a user defined sub image. Information regarding the whole or sub image will be displayed in the Info tab. The data displayed includes Projected Area, RMS Roughness, Average Roughness, Mean Height, Maximum Height, Minimum Height, and Peak-to-Valley.

• 3D Plot: The 3D Plot command opens the 3D Plot window. The options in the 3D Plot window will be discussed in the next section.

Window The Window menu contains commands relating to the behavior of the TriboView windows.

• Always on Top: The Always on Top command forces the TriboView window to be on top of all opened image files

• Image Selection: The Image Selection displays the current opened image files for easy access

Help The Help menu displays information about TriboView.

9.1 3D PLOT WINDOWThe 3D Plotting feature will generate a 3D presentation of the currently displayed 2D image. The 3D plot is accessed

from the image window by selecting Tools 3D Plot. The 3D Plot window will appear similar to Figure 9.10

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Figure 9.10 3D Plot window

Because of the increased computer processor requirements with the 3D plotting, it is convenient to position and

modify the image in low-resolution mode, and then switch to high-resolution mode to save the 3D image. Switching

between high and low resolution is performed by checking or un-checking the High Resolution Image box in the

lower right corner of the 3D Plot window (Figure 9.11).

Figure 9.11 High Resolution Image check-

box location

The movement of the 3-D image is controlled using the mouse as described below. These controls are also listed on

the bottom left side of the 3D Plot window for quick reference.

Rotate Left-click and move the mouse

Zoom CTRL + left-click and move the mouse

Pan SHIFT + left-click and move the mouse

Properties Right-click to adjust image properties

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After the image has been manipulated as desired, it can be saved as a *.tif file or printed. These options are available

by selecting File Save Image As or File Print, respectively.

Some settings used in the image, as specified in the Properties window, can be saved as the defaults for the 3D Plot.

This option is selected by clicking Config Save Current Window Properties as Default. Various property

configurations can be saved and loaded individually by selecting Config Save Window Properties and

Config Load Window Properties, respectively.

The 3D Plot Properties window can be accessed by right-clicking on the image. In the Properties window, there are

five tabbed sections which can be used to manipulate the image. These sections are Control, 3D, Axis, Lighting, and

Plots.

The Control tab is shown in Figure 9.12. This window controls the color of the background, which can be selected by

clicking the colored square next to Background Color. The Pan, Zoom, and Rotate functions using the mouse can be

disabled or enabled and the speed of the respective functions can be specified by checking and un-checking the

appropriate boxes. The size of the image within the window can be adjusted by changing the values in the Position

and Size parameters. A label can be added above the image by typing it in the white box marked Label. The label

style can be changed by clicking the Label Style button.

Figure 9.12 3D Properties Control tab

The 3D tab is shown in Figure 9.13. This window controls the type of drawing, the axis, and the viewing angle. In the

Drawing box, the drawing type can be changed from Orthographic to Perspective and the Plot Area of each axis can

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be determined. In the Axis Grid Planes box, the axis and grids can be enabled and disabled as well as selecting the

color for the components. In the Viewing Position box, a specific plane or any user-defined direction can be selected

for viewing.

Figure 9.13 3D Properties 3D tab

The Axis tab is shown in Figure 9.14. This window controls the names and labels of each axis. If the Name field in the

Axis Name box is filled and Visible is checked, the name will appear along the appropriate axis. Axis Labels are the

numerical values associated with the points along the axis. Ticks on the axis are used to show the placing of the labels

more precisely. The Attributes box contains additional parameters.

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Figure 9.14 3D Properties Axis tab

The Lighting tab is shown in Figure 9.15. This window controls the type and amount of lighting. From the General

box, the Lighting can be enabled and disabled and an Ambient Color can be selected. From the Positional Lights box,

up to four separate lights can be individually defined. The color, placement, and intensity factors for each light can be

specified. The light can be defined as a spotlight if the user wishes.

Figure 9.15 3D Properties Lighting tab

The Plots section is shown in Figure 9.16. This window controls the way that the surface is plotted onto the 3D

image. One of three Color Schemes can be chosen for the image. These schemes show color change with change in

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elevation. In the Plane Projections box, different plane projections can be chosen. These are two-dimensional

projections of the 3D image onto the specified planes. The value in the Points Size box determines how large each of

the points on the image is. The default value of zero gives the sharpest image. Using a wire style from the Wire box

forces the image to appear as a wire-frame model of the surface and can be useful in seeing peaks and valleys. A

surface style can be selected from the Surface box. The surface style forces the image to appear similar to the actual

sample.

Figure 9.16 3D Properties Plots tab

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SECTION | NANODMA• Dynamic (nanoDMA) option installation, connections, and calibrations for

nanoDMA option• Dynamic (nanoDMA) test creation and analysis• Setting parameters for modulus map testing (upgraded feature)

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This section of the user manual is intended for users with a system capable of nanoDMA testing (with the option to

upgrade to Modulus Mapping). If you are unsure if your system has nanoDMA testing contact Hysitron for additional

information. Due to numerous similarities, some portions of this section will refer to the TriboIndenter base portion

of this user manual.

This section of the user manual assumes the user has read and is familiar with the TriboIndenter base user manual and

the following calibrations have been satisfactorily performed:

• Optic-Probe Offset (H-pattern) calibration• Probe area function• Tare value verification• Indentation Axis calibration

The system must be set up and the calibrations listed above performed before continuing with the nanoDMA section


HISTORY OF NANODMAThe nanoDMA and modulus mapping technique has been developed at Hysitron for the purpose of augmenting the

indentation capabilities of the Hysitron transducer. This testing method utilizes sinusoidal loading concurrent with the

quasi static indentation loading to provide the ability to perform a wide array of new tests. The applications range

from ceramics to polymers and from thin films to bulk samples. Any sample that can be characterized using the quasi

static indentation testing method can be tested using nanoDMA to obtain much more information about the sample.

Modulus mapping, similar to nanoDMA testing, involves performing hundreds of dynamic tests over the sample

surface while obtaining an in-situ image. nanoDMA is required to operate modulus mapping on a system but is not

included in the base purchase of the nanoDMA package.

The dynamic testing technique was developed primarily in response to the insufficiencies of quasi static indentation

testing for materials that display significant time-dependent deformation and recovery. For viscoelastic materials, it is

very difficult to obtain meaningful and accurate data using quasi static indentation testing due to the large effect that

the choice of the loading function and the type of probe utilized will have on the measured properties due to creep and

strain rate effects. Additionally, in the case of viscoelastic materials, it is desirable to have the capability to

characterize both components of the complex moduli: the storage and the loss modulus. It is very challenging and

time consuming to accurately quantify the complex modulus of polymeric materials using quasi static indentation

techniques, requiring numerous tests and copious amounts of analysis.

Standard analysis methods of quasi static nanoindentation load vs. displacement data assume purely elastic/plastic

material behavior, particularly during the loading and unloading portions of the test. This assumption ignores

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viscoelastic effects that exist throughout the entirety of the indentation test. The most commonly accepted quasi static

indentation analysis measures stiffness by calculating the slope of the initial portion of the unloading curve. This

analysis assumes that all recovery observed during the unloading is elastic recovery, which is true for most ceramics

and metals. However, many polymers show strong viscoelastic behavior, which implies a time dependent recovery.

Therefore, the unloading portion of the load/displacement data is a convolution of elastic and viscous recovery,

rendering it nearly impossible to calculate a true indentation modulus.

Historically, the primary method of characterizing the mechanical properties of viscoelastic materials has been

through dynamic mechanical analysis, commonly referred to as DMA. DMA has developed into a versatile technique

with the capability of applying cyclic stress and strain to polymer specimens of various configurations in tension,

compression and shear. DMA has the capability of testing frequencies over several orders of magnitude, beginning in

the milli-hertz range and going well into the hundreds of hertz. Numerous discussions with experienced DMA users

have suggested that DMA is most successful at accurately characterizing materials under 50 Hz.

DMA is designed for, and has been successfully proven effective for, testing on the macroscopic scale, typically with

specimens on centimeter size scales. The most typical method of testing dynamic properties of materials has been by

using a parallel plate test fixture. A specimen is placed between the parallel plates as shown in Figure 10.1.

Figure 10.1 Parallel plate DMA testing

This technique measures a shear modulus as the plates are rotated at different angular frequencies and with different

rotational amplitudes. The effects of the testing frequency can be observed by the amount of force that is necessary to

accomplish the rotation desired.

Alternatively, and more similar to the proposed nanoindentation technique, a sample can be tested uni-axially through

a tension test, as in a typical dog-bone tensile test. A cyclic tensile load is applied to the sample at a given frequency

or range of frequencies, which also allows observation of the frequency dependent properties of the sample.

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Figure 10.2 Uni-axial DMA testing

Characterization of the viscoelastic properties of polymers requires quantifying a complex modulus, which is ignored

by quasi static indentation testing, as discussed previously. The complex modulus is comprised of two moduli, a

storage modulus and a loss modulus, which are each representative of two different components of the material’s

behavior. A common model for polymers describes the material as a system of a spring and a dashpot in parallel. A

simple example is given in Figure 10.3, where [k] and [C] are the stiffness and the damping of the polymer,

respectively.

Figure 10.3 Kelvin model for polymeric

systems

The storage modulus relates to the stiffness of the material, or the in phase response of the material to the applied

force. This modulus relates the elastic recovery of the sample, which is the amount of energy recovered from the

sample subsequent to a loading cycle. The storage modulus is proportional to the ratio of the applied force amplitude

to the displacement amplitude that is in phase with the applied force. The loss modulus relates to the damping

behavior of the material and is observed by the time lag between the maximum force and the maximum displacement.

This damping is the amount of energy put into the sample during the indentation that is dissipated by various

processes that facilitate energetic losses, primarily heat generation.

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IMPROVEMENTS WITH NANODMA IIIThe next generation of nanoDMA testing (nanoDMA III) was introduced by Hysitron in September 2011.

nanoDMA III includes new features such as:

• Updated transducer electronics• Updated Hysitron control unit electronics• Increased user-customizable software• Continuous measurement test (CMX)• Reference frequency analysis• Multiple nanoDMA data file plotting• Lower frequency range (0.1 Hz - 300 Hz)• Amplitude defined more commonly as center-to-peak, not peak-to-peak

nanoDMA III is an upgraded feature from nanoDMA II and requires a system running a performech or digital control

unit with TriboScan 9.2.12 or higher.

CHAPTER 10 NANODMA HARDWARE

The nanoDMA option requires the hardware discussed in the TriboIndenter base section of this user manual be

installed and calibrated. The probe, transducer, and piezo scanner are installed identically to the information

presented in the TriboIndenter base section of this user manual. The nanoDMA option has some unique hardware

installation and connection requirements that are not covered in the TriboIndenter base section.

10.1 INSTRUMENT CONNECTIONSMost TriboIndenter systems utilize an updated Hysitron control unit firmware that includes a DDLA (Dual Digital

Lock-in Amplifier). No additional instrument connections are required for new TriboIndenter systems (with the

exception of installing the nanoDMA-compatible transducer). This section is only relevant for prior revision systems

being upgraded that may utilize an external SRS 830 lock-in amplifier. Functionality and specifications with the

DDLA and external SRS 830 lock-in amplifier is identical.

The connection diagram for systems running nanoDMA III using an external SRS 830 lock-in amplifier is given in

Figure 10.4.

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Figure 10.4 nanoDMA connection diagram

The Hysitron DSP-based control unit is connected to the SRS 830 lock-in amplifier with four BNC connections. The

BNC cables are connected as given:

• Hysitron control unit ADC 2 SRS lock-in amplifier Sine Out• Hysitron control unit ADC 3 SRS lock-in amplifier Ch 1 Output

(amplitude)• Hysitron control unit ADC 4 SRS lock-in amplifier Ch 2 Output (phase)• Hysitron control unit DAC 3 SRS lock-in amplifier A/I

Additionally, the SRS 830 lock-in amplifier is connected to the data acquisition computer through a USB-GPIB

adaptor.

! DO NOT connect or disconnect any cables while the transducer controller or computer is powered on as serious damage may occur to the electronics.

10.1.1 INSTALLATION OF COMPONENTSThe following procedure should be used to install the nanoDMA III components. Typically, a qualified service person

from Hysitron will perform the initial installation so many portions of this procedure may already be completed.

Portions of this procedure can be used by the user if the system is disconnected for any reason.

1. Power off all components of the system.

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2. Connect the National Instruments USB-GPIB adapter between the lock-in amplifier and the computer.

3. Connect four BNC cables between the Hysitron control unit and lock-in amplifier as labeled:

•ADC 2 Sine Out•ADC 3 Ch 1 Output•ADC 4 Ch 2 Output•DAC 3 A/I

4. Power on the lock-in amplifier.

5. On the front panel of the lock-in amplifier, press the Setup button in the lower right corner until the Address light is selected. Verify that the address is set to [1]. If not, use the large knob to the right of the display to set the address.

6. Power on the computer.

7. If the software has already been installed for the GPIB interface, the installation is complete.

8. If the software has not been installed, install the software from the CD labeled NI 488.1. Follow the on-screen instructions to set up the GPIB interface and verify communication with the lock-in amplifier.

9. Install nanoDMA software using the CD that was provided. Depending on the specific system, the software may require a licensing key. Contact a Hysitron service engineer for licensing information.

10.1.2 LOCK-IN AMPLIFIER CONFIGURATIONFollowing the initial set up, the lock-in amplifier is completely controlled by the computer. The following settings on

the lock-in amplifier need to be verified by the user prior to running a nanoDMA or modulus map test.

On the front of the lock-in amplifier (Figure 10.5) press the Setup button until the indicator light is next to the desired

item (Table 10.A), and verify that the displayed value is set correctly. If the item requires adjustment, use the

Adjustment Knob to properly set the items. Leave the indicator light set to GPIB/RS232 after the settings have been

verified.

Figure 10.5 Location of amplifier settings

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Table 10.A Values for lock-in amplifier

settings

The remainder of the lock-in amplifier settings are controlled by the software. No direct user interaction with the

lock-in amplifier is required during a nanoDMA or modulus mapping test.

Upon starting the lock-in amplifier several self-diagnostic tests are performed. If any of these startup tests fail refer to either the lock-in amplifier user manual, or contact a Hysitron service engineer before proceeding.

CHAPTER 11 NANODMA OPERATION

The calibrations discussed in the base section of this user manual should be completed prior to calibrating or testing

with the nanoDMA option.

Prior to using the nanoDMA III features, users should be familiar with standard Hysitron software operation and all

calibration/testing procedures for indentation testing.

! Before performing any nanoDMA testing all necessary system calibrations should be performed. This may include but is not limited to the Transducer Indentation Axis calibration and the Optic-Probe Offset calibration.

For systems upgrading from nanoDMA II there will be an additional Legacy nanoDMA sub tab for analyzing previously collected nanoDMA II data files.

! For systems upgrading from nanoDMA II there will be an additional nanoDMA mode from the Modepull-down menu and nanoDMA sub tab under the Load Function tab. Running tests from the Load Function nanoDMA sub tab or with the nanoDMA mode selected, even with nanoDMA III hardware, will result in nanoDMA II data files with nanoDMA II correction and fitting parameters.

Lock-In Amplifier Settings

Item Value

GPIB/RS232 GPIB

Address 1

Baud 9600

Parity none

Queue 300A

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11.1 NANODMA CALIBRATIONSThe calibrations discussed in this section are specific to the nanoDMA option. This section is intended as a

supplement to the System Calibrations section presented earlier in this user manual.

! Calibrations in the earlier presented System Calibrations section must be completed and/or verified before performing sample testing.

11.1.1 VERIFY THE TRANSDUCER CONSTANTSnanoDMA III testing requires the use of a nanoDMA III capable transducer. The calibration constants for the

nanoDMA III transducer are located within the Calibrations tab System Calibrations sub tab (Figure 11.1).

Figure 11.1 System Calibrations sub tab

The transducer constants should be entered as listed on the transducer constants data sheet that was provided with the

transducer. The parameters listed under the Transducer Constants heading are static values for the transducer; the

parameters listed under the Transducer Calibrations heading will be calculated and may vary from calibration to

calibration.

Most of the parameters in the System Calibration sub tab are defined in the base section of this user manual.

Parameters specific to nanoDMA testing are defined as follows:

Spring Constant The Spring Constant is a property of the nanoDMA transducer and is modified during the Dynamic calibration. The default starting value is 350 N/m.

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Mass The Mass is a property of the nanoDMA transducer and is modified during the Dynamic calibration. The default starting value is 500 mg.

Damping The Damping is a property of the nanoDMA transducer and is modified during the Dynamic calibration. The default starting value is 0.06 kg/s.

Load Amplitude Attenuation

The Load Amplitude Attenuation setting will be available only with instruments equipped with nanoDMA III and Modulus Mapping (this parameter is only used for Modulus Mapping). The Load Amplitude Attenuation is a gain setting for the lock-in amplifier, 100 is the default and works for most testing routines. The Load Amplitude Attenuation should be lowered when the lock-in amplifier channels have been saturated during a test.

Lock-in Input Gain The Lock-in Input Gain parameter determines the gain on the AC signal being input into the lock-in amplifier. The default setting is 100, if the AC signal displacement amplitude is greater than about 300 nm, this gain should be set to 10. If the first point in the nanoDMA test is greater than about 300 nm, the gain will automatically adjust to 10 for the duration of the test.

Modulus Mapping Low Pass Filter

The Modulus Mapping Low Pass Filter is an electronic filter intended for use while performing a Modulus Mapping test to reduce noise between the piezo and transducer. This should be set to Disable when performing nanoDMA testing.

11.1.2 PROBE AREA FUNCTION Before nanoDMA III testing begins, the probe and transducer intended to be used for the nanoDMA III testing should

be used in Indentation mode to generate a probe area function. The procedure for calibrating the probe area function

is located within the base section of this user manual.

The calculated probe area function file can be loaded into the probe area function panel from the Calibration

tab Tip Area Function sub tab Open or the values can be entered manually into the corresponding fields.

Similar to quasi static indentation tests, the probe area function loaded in this window at the time the test is performed

will be stored with the data file and used for the analysis.

The probe area function can also be performed with a nanoDMA III CMX test. More information regarding this procedure can be found later in this section of the user manual.

11.1.3 INDENTATION AXIS CALIBRATIONThe Indentation Axis calibration is used to calculate the Electrostatic Force Constant (ESF) and Plate Spacing of the

transducer. The Indentation Axis calibration must be performed identically to the method presented in the base

section of this user manual.

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Because of the stiffer springs associated with the nanoDMA transducers (and the load scale factor set to about

0.5 mV/mg), a maximum force of about 1200 μN during the Indentation Axis calibration will be required to actuate

the transducer to a high enough displacement to achieve a reasonable calibration. The TriboScan software should

automatically apply the larger force during the calibration process.

During the Indentation Axis calibration the transducer should actuate 3.5 – 4.5 μm. If the normal displacement is less than 3.5 μm consider performing the Indentation Axis calibration at a higher maximum force.

11.1.4 DDLA LOCK-IN AMPLIFIER CALIBRATIONSystems that have a Hysitron control unit with DDLA (Dual Digital Lock-in Amplifier) and do not have the external

SRS 830 lock-in amplifier requires an additional Lock-in Amplifier calibration. The Lock-in Amplifier calibration is

only required to be performed if the instrument hardware configuration changes and is often performed at the time of

the installation and is not required unless instructed by a Hysitron service engineer.

To perform the Lock-in Amplifier calibration select the Calibration tab System Calibrations sub tab LIA Cal

button (under the System Parameters heading). The Lock-in Amplifier calibration results window is given in

Figure 11.2.

Results will be given in the Lock-in Amplifier calibration window for each of the installed data acquisition boards.

The Sense X Gain, Sense Y Gain, Mirror X Gain, and Mirror Y Gain should all be between about 1.8-2.2. All Offset

values should be between 0.0 and 0.4 V.

If the result is satisfactory click the Close button and accept the updated values to be used for the system.

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Figure 11.2 Lock-in Amplifier calibration

results window

11.1.5 DYNAMIC CALIBRATIONThe Dynamic calibration is to be performed out of contact with any sample with the probe that will be used for the

testing. It is important that the correct transducer constants are loaded or entered into the Calibration tab System

Calibrations sub tab before proceeding. The following procedure assumes that the Indentation Axis calibration and

Optic-Probe Offset calibration has been successfully performed.

The Dynamic calibration should be performed about once a week or whenever the probe or transducer has been

removed, replaced, or modified.

1. With the probe out of contact, click the Calibrations tab System Calibrations sub tab.

2. Verify the proper transducer constants are loaded and reset any values to the default values as necessary.

3. Select the Calibrate button under the Transducer Calibrationsheading nanoDMA sub heading (Figure 11.3).

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Figure 11.3 Dynamic calibration button

4. The Dynamic calibration load function will open in the Load Function tab Indentation sub tab (Figure 11.4). Do not change any parameters on this window.

5. Click the nanoDMA Air Cal button and the system will perform a nanoDMA test in the air over the defined range of forces and frequencies to solve for the dynamic compliance of the system. This test takes approximately 7 minutes to complete.

Figure 11.4 Dynamic calibration load

function

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6. Following the test a plot (similar to Figure 11.5) will be displayed and the user will be prompted if they would like to use the Dynamic calibration result. The user should select Yes if the fit is satisfactory in the Dynamic Compliance vs. Frequency plot and the Stiffness RMSE is less than 0.1 μN/nm and the Phase RMSE is less than 1.0 deg. The RMSE values can be found in the upper right of the nanoDMA Calibration window.

7. The Stiffness, Mass, and Damping for the transducer are automatically calibrated and given in the upper right of the nanoDMA Calibration window.

8. Click the Close button in the lower right of the nanoDMA Calibration window to exit and save the defined calibration values.

9. The user can review past calibration results by opening the calibration file in the Analysis tab nanoDMA sub tab File menu Dynamic Calibration.

Figure 11.5 Satisfactory Dynamic calibration

result

Many times a poor calibration can be caused by debris on the probe or a poorly installed probe. If the RMSE values

are not within the desired range the user should attempt to remove the transducer and probe and perform the

calibration with no probe installed. If the calibration result is satisfactory with the probe removed the user can attempt

to reinstall the probe and run the calibration again.

If the issue persists the user should contact Hysitron for further assistance.

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PHASE ERRORThe Phase Error can be viewed by selecting the Show Details button on the nanoDMA Calibration window.

The plots located under the Show Details button are provided only for user information and troubleshooting purposes

and are not required for the calibration process. The Phase Error vs. Frequency plot is a plot of the accuracy of the

Dynamic calibration fit. The Residual Phase vs. Frequency plot, for a properly functioning system, should have a

Residual Phase of less than approximately 3˚, however, if this is not met the system will fail with the earlier defined

Phase RMSE specification.

11.2 NANODMA III TESTINGThe nanoDMA III load function is constructed within the Load Function tab Indentation sub tab. Within the

Indentation sub tab there is a nanoDMA side tab that will be used for constructing the nanoDMA segments within the

load function.

With the nanoDMA III capabilities incorporated into the quasi static indentation load function editor different colored

segments represent different modes:

• Red Currently selected segment• Black Quasi static indentation segment• Green nanoDMA III segment• Blue Reference segment (discussed later in this user manual)

Before discussing the nanoDMA III load function parameters there are two very important menu items on the Load

Function tab Indentation sub tab that the user must be aware of: Standard Load Functions (Figure 11.6) and User

Mode (Figure 11.7).


functions including a basic quasi static trapezoid indentation test, CMX (Continuous Measurement of X) dynamic

tests (that will be discussed later in this user manual), and a standard frequency sweep dynamic test.


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function. Because of the increased number of user-tunable parameters within the nanoDMA III software the User

Mode is more important than in other testing modes.



The Custom mode will give the user access to all parameters and can be more complicated for users who are

unfamiliar with the capabilities of the nanoindentation system. This nanoDMA III user manual is written while in

Custom mode so all parameters will be discussed.


The nanoDMA III user manual is written with the User Mode set to Custom so that all parameters will be discussed. If parameters discussed in this user manual are not present in the instrument software the user should verify the User Mode is set to Custom.

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11.2.1 NANODMA SIDE TABThe nanoDMA side tab (Figure 11.8) is the primary area where the user can create, edit, and modify the load function

nanoDMA III segments. The user must select a segment from the load function plot before modifying the parameters

given in the nanoDMA side tab. A discussion of the parameters is given below.

Figure 11.8 nanoDMA side tab

Segment Type The Segment Type parameter allows the user to choose the type of segment for the currently selected segment on the load function plot. The options include quasi static (indentation), nanoDMA (frequency or load sweep), or reference (which will be discussed later in this user manual).

Frequency The Frequency parameter allows the user to set the frequency for the nanoDMA segment(s). The frequency can be set from 0.1 Hz up to 300 Hz.

Dynamic Load Scaling The Dynamic Load Scaling parameter allows the user to choose how the dynamic load is scaled with respect to the quasi static load.

• Variable Dynamic Load: The Variable Dynamic Load option will scale the dynamic load proportional to the square root of the quasi static load. This option usually results in the most constant dynamic displacement amplitude, which is typically most desirable, and because of that this option is the most common dynamic load scaling option.

• Constant Quasi/Dynamic Ratio: The Constant Quasi/Dynamic Ratiooption will scale the dynamic load proportional to the quasi static load.

Figure 11.9 Representation of Variable

Dynamic Load and Constant Quasi/Dynamic Ratio scaling

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• Constant Dynamic Load: The Constant Dynamic Load option will hold the dynamic load constant for the segment.

Figure 11.10 Graphical representation of

Constant Dynamic Load scaling

Figure 11.11 Dynamic Load Scaling options

Note that the Dynamic Load Scaling parameters have no effect if the load function segment is a hold segment (same starting and ending quasi static load).

For tests where the starting load is zero and the Dynamic Load Scaling is not set to the Constant Dynamic Load option, the load will be scaled based upon the segment dynamic force and the preload value. This will be the case even if the dynamic load is not applied during the preload.

Begin Load Amplitude

The Begin Load Amplitude parameter defines the starting dynamic load for the defined segment. This parameter is defined as a center-to-peak value, not peak-to-peak that users upgrading from nanoDMA I or nanoDMA II may be familiar.

End Load Amplitude The End Load Amplitude parameter is automatically generated by TriboScan based on the Dynamic Load Scaling selection and the quasi static starting/ending loads of the segment.

Lock-In-Time Constant

The Lock-In Time Constant parameter is a moving average that allows the user to define the length of time to average data. Small Lock-In Time Constant values may be

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noisier and less stable while larger values average more data but short events may be averaged out. The default setting is Auto/Lookup Table which will use time constants based on the rules defined in the Time Constants window.

Time Constants Lookup Table button

The Time Constants Lookup Table button opens the Time Constants window (Figure 11.12). The Time Constants Lookup Table allows the user to define the time constants that are used based upon the frequency of the test at any given time. When the user selects the Auto/Lookup Table option from the Lock-In Time Constant parameter the table in the Time Constants window is used. The Time Constantswindow is also used by the nanoDMA segment generator to set the time constants on the inserted segments and to define the segment length based upon the Number of Time Constants (Delay) parameter.

The user can edit, remove, or restore the lookup table default values from the Time Constants window (Figure 11.12). Each rule consists of a lock-in amplifier time constant setting and a maximum frequency for use. If no rule has been defined up to the maximum frequency allowed (300 Hz) the final rule will be used for the remainder of the frequency range.

Figure 11.12 Time Constants window

The user can also choose to select a time constant from the pull-down list and use this time constant for the selected segment.

The Roll Off Time Constants parameter can be thought of as settle time prior to each dynamic segment. This value is multiplied by the Time Constant Setting corresponding to the segment frequency to yield the settle (hidden/uncollected data)

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time prior to the dynamic segment. It is important that the Number of Time Constants (Delay) in the Dynamic Sweep Generator window is set larger than the Roll Off Time Constants or no data will be collected for that segment. Likewise, if the user is creating a load function from the Load Function tab the segment time must be longer than the Roll Off Time Constant multiplied by the Time Constant Setting for the segment frequency or no data will be collected for that segment.

No data collected? Check the Roll Off Time Constant, segment frequency, and Time Constant Settingparameters.

All buttons Any button labeled All will force the entire load function to match the current segment parameters (as much as is possible based on the load function set up).

The All buttons for the dynamic loads will change the loads of the other segment based upon the quasi static load and the dynamic load scaling (allowing for a smooth transition between segments). The All button for the segment types will not change Reference segments to nanoDMA segments if the button is clicked when a nanoDMA segment is selected. The All buttons for the dynamic load and the time constant will also affect the preload dynamic properties.

Reference Frequency The Reference Frequency parameter is the frequency of the reference segments to be performed during the test (if any reference segments have been defined).

Typically the reference segments are created automatically within the nanoDMA Segment Generator window and the Reference Test Parameters (Frequency, Modulus, and Modulus From) are only used if the user needs to modify individual segments.

When the Reference Frequency option is used, the modulus throughout the test is ‘referenced’ (compared) to the first reference segment in the test and then compared with future reference segments to reduce the effects of drift or sample creep in the sample result. Alternatively, the user can define the modulus for the reference segments, however, this value is typically unknown so this is not the preferred method.

Reference Modulus The Reference Modulus parameter allows the user to define a modulus of the sample at a given frequency (if known). If the modulus of the sample is unknown, the Auto/From First Ref. Segment option should be selected from the Reference Modulus Fromparameter.

The modulus used for the reference value is always a storage modulus.

Reference Modulus From

The Reference Modulus From parameter defines where the system obtains a reference value.

• Auto/From First Ref. Segment will obtain the reference modulus from the first reference segment.

• User Defined Value uses the value defined by the user in the Reference Modulus parameter.

Lock-In Sensitivity The Lock-In Sensitivity parameter allows the user to set a gain on the signal input for the lock-in amplifier. This parameter also affects the magnitude of the output signals from the lock-in amplifier.

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A Lock-In Sensitivity that is too high will overload the lock-in amplifier and/or overload the input signal going back to the Hysitron control unit.

A Lock-In Sensitivity that is too low may result in more noise in the data. It is important to note that the noise in the system is also affected by the Lock-In Input Gain on the Calibrations tab System Calibration sub (which is also a gain on the signal going to the lock-in amplifier).

Typical settings for the Lock-In Sensitivity parameter are given below:

Table 11.A Lock-In Sensitivity settings

Filter Slope The Filter Slope parameter is a digital filter that reduces data at frequencies that the lock-in amplifier is not concerned with regarding the current measurement signal. Increasing the Filter Slope parameter will reduce the noise measured by the lock-in amplifier, however, this may result in a longer roll-off time (the time required between frequency adjustments for the lock-in amplifier to stabilize). The default setting is 18 dB/oct. For more details consult the SRS lock-in amplifier user manual.

Reserve The Reserve parameter is a ratio of the largest tolerable noise to the full scale signal without the lock-in amplifier sensing an overload (how well the lock-in amplifier is able to filter out the non-signal frequencies). A High reserve would indicate very effective filtering at a cost of resolution. A Low reserve would include more electronic noise from the lock-in amplifier but higher resolution. The default setting is Normal. For more details consult the SRS lock-in amplifier user manual.

nanoDMA Segment Generator button

The nanoDMA Segment Generator button will open the Dynamic Sweep Generator window (or if the User Mode is set to Standard this button will open either the Dynamic Frequency Sweep Generator window [for a hold segment], or the Dynamic Load Sweep Generator window [for a load/unload segment]). All of these windows are similar with the Dynamic Sweep Generator window containing all parameters and the other two windows containing limited parameters.

11.2.2 DYNAMIC (FREQUENCY OR LOAD) SWEEP GENERATOR WINDOWThe Dynamic Sweep Generator window (accessed from the nanoDMA Segment Generator button on the nanoDMA

side tab) is shown in Figure 11.13. The Dynamic Sweep Generator window assists the user to create more complex

dynamic load functions. The parameters given in the Dynamic Sweep Generator window are given below.

If parameters discussed in this section are not present in the instrument software the user should verify the User Mode is set to Custom.

Lock-In Sensitivity Settings

Value Recommended Dynamic Amplitudes

50 mV/nA Default setting

100 mV/nA 1-2 nm

500 mV/nA >2 nm

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Figure 11.13 Dynamic Sweep Generator

window

Segment Number The Segment Number is defined as the current indentation segment that is being replaced by the dynamic segment defined in the Dynamic Sweep Generator window. This parameter is given for user information and cannot be modified unless the user selects an alternate segment from the Load Function tab.

Start Frequency The Start Frequency is defined as the starting frequency that the dynamic portion of the currently selected segment will oscillate the probe. The Start Frequency cannot be less than 200 Hz when performing a nanoDMA test in load control mode.

End Frequency The End Frequency is defined as the ending frequency that the dynamic portion of the currently selected segment will oscillate the probe. The End Frequency cannot be less than 200 Hz when performing a nanoDMA test in load control mode.

Number of Steps The Number of Steps parameter allows the user to define how many increments are used during the segment to move from the Start Frequency to the End Frequency.

Frequency Scaling The Frequency Scaling pull-down menu allows the user to toggle between a linear and logarithmic variation in frequency from the Start Frequency and the End Frequency.

Randomize Frequency Order

The Randomize Frequency Order check box allows the user to perform the frequency sweep test in a random frequency pattern in decouple the effects of drift or sample creep from sample frequency dependence.

Include Reference Frequency

The Include Reference Frequency check box will place a reference frequency segment (with the frequency defined in the following parameter) between each step in order to use a reference modulus (as opposed to the measured contact depth) when performing the analysis.

When the Reference Frequency option is used, the modulus throughout the test is ‘referenced’ (compared) to the first reference segment in the test and then compared with future reference segments to reduce the effects of drift or sample creep in the sample result. Alternatively, the user can define the modulus for the reference

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segments, however, this value is typically unknown so this is not the preferred method.

Reference Frequency The Reference Frequency parameter is the frequency for all reference frequency segments to be performed.

Quasi Static Dwell Time

The Quasi Static Dwell Time is a parameter that allows the user to define a hold time prior to starting the dynamic segment to allow for sample creep to settle.

Start Load The Start Load parameter allows the user to define the starting load for a dynamic load sweep test. If the start and end loads are not the same a non-zero Loading Ratemust be defined.

End Load The End Load parameter allows the user to define the ending load for a dynamic load sweep test. If the start and end loads are not the same a non-zero Loading Rate must be defined.

Loading Rate The Loading Rate parameter allows the user to define the loading rate for a dynamic load sweep test. If the start and end loads are not the same a non-zero Loading Ratemust be defined. If the start and end loads are the same the Loading Rate must be zero.

Begin Load Amplitude

The Begin Load Amplitude parameter defines the starting dynamic load for the defined segment. This parameter is defined as a center-to-peak value, not peak-to-peak that users upgrading from nanoDMA I or nanoDMA II may be familiar.

Load Amplitude Scaling

The Load Amplitude Scaling parameter defines how the Load Amplitude value will adjust as the quasi static load varies during the test. This parameter was discussed thoroughly in the nanoDMA side tab section of this user manual (previous section).

Number of Time Constants (Delay)

The Number of Time Constants (Delay) is defined as the number of time constants that each segment will last. The Roll Off Time Constants parameter (in the Time Constants lookup table) is subtracted from the Number of Time Constants (Delay) parameter to yield the actual number of time constants the segment will last.

The Number of Time Constants (Delay) parameter will determine the time for each segment in the Dynamic Sweep Generator and it must be larger than the Roll Off Time Constants parameter given in the Time Constants lookup table or no data will be collected.

Segment Additional Fixed Delay Time

The Segment Additional Fixed Delay Time is a parameter the user can initiate to add an additional fixed delay time to each segment.

Minimum Segment Time

The Minimum Segment Time is the minimum allowable time permitted for any segment during the test. If the Number of Time Constants (Delay) and Segment Additional Fixed Delay Time are defined to present a segment less than the defined Minimum Segment Time, the Minimum Segment Time will be used for the segment instead. This parameter should be set to a value to avoid synchronization issues with extremely short segments.

Lock-In Time Constant

The Lock-In Time Constant parameter is a moving average that allows the user to define the length of time to average data. Small Lock-In Time Constant values may be noisier and less stable while larger values average more data but short events may be

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averaged out. The default setting is Auto/Lookup Table which will use time constants based on the rules defined in the Time Constants window.

Time Constants Lookup Table button

The Time Constants Lookup Table operates the same as the Time Constants Lookup Table button located on the nanoDMA side tab (discussed in the previous section).

Data Acquisition Rate The Data Acquisition Rate parameter defines the acquisition rate for the entire test. The Data Acquisition Rate can also be modified from the Load Function tab.

Total Segment Time The Total Segment Time is generated based on the parameters defined within the Dynamic Sweep Generator window. This parameter is presented for informational purposes and cannot be modified.

11.3 DYNAMIC TEST TYPESThere are four basic types of dynamic tests that the nanoDMA III software has been designed to perform. The

software is very open and versatile so as users become more experienced they will likely begin to develop their own

routines, however, this user manual will cover the configuration and performance of these basic tests.

The four types of tests are:

• Variable Frequency: Variable frequency with constant load.• Variable Load: Variable load with constant frequency.• CMX: Continuous Measurement of X (where X is modulus, hardness, stiffness,

etc...)• Reference Creep: A creep test using reference frequencies to allow for longer

test times.

nanoDMA tests performed in Load Control Feedback may not be performed at frequencies less than 200 Hz.

Some nanoDMA III Standard Load Functions are created in Open Loop Feedback mode with a force lift segment (load function plot that has an initial segment that goes to a negative force). Tests with a negative force segment cannot be performed in Load Control Feedback mode (the standard Lift Height and other parameters should be used).

Testing is performed similarly to the three-plate capacitive indentation testing (either with the Perform Indent button

from the Indentation sub tab or the Test button from the in-situ SPM Imaging tab). Because of the test times

associated with nanoDMA testing, it is suggested to perform testing only after having the probe in-contact for a

sufficient amount of time to minimize drift.

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11.3.1 VARIABLE FREQUENCYDuring a variable frequency test, the frequency is varied in each progressive step. During this type of test, a fixed

quasi static load is chosen, as well as a fixed dynamic load amplitude. An example of this type of test is given in

Figure 11.14.

Figure 11.14 Force vs. time plot for variable

frequency test

Mechanical properties of viscoelastic materials often vary when tested at different frequencies. A ramping frequency

test is used to determine mechanical properties as a function of frequency. This is the typical type of test performed

by a DMA (dynamic mechanical analysis) instrument at macro scale.

The frequencies may be ramped from 0.1 Hz up to 300 Hz. When testing at lower frequencies (below 10 Hz) the test

can take a very long time, so it is recommended that lower frequency tests utilize the reference frequency functions to

minimize drift effects. When testing is performed over 200 Hz, the amplitude can become quite small, and it may be

difficult for the lock-in amplifier to measure the phase and amplitude of the displacement signal. The user must be

sure that the amplitude is large enough at higher frequencies to ensure quality data.

The easiest way to create a variable frequency test is to go to the Load Function tab Indentation sub

tab Standard Load Function menu Frequency Sweep. This will open the Dynamic Sweep Generator window

(Figure 11.15).

Figure 11.15 Dynamic Sweep Generator

window

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Within the Dynamic Sweep Generator window the user should enter a Start and End Frequency for the desired

variable frequency test. The Number of Steps will determine the number of divisions taken to move from the Start to

End Frequency.

• The user may want to use the Logarithmic option from the Frequency Scaling pull-down menu for testing ranging from very low to high frequencies (to produce more desirable results at low frequencies).

• The user may want to use the Reference Frequency check box for low frequency testing to reduce possible effects from sample creep or drift.

An example of a variable frequency result is given in Figure 11.16. Notice that the result in Figure 11.16 has the

following options selected:

• X axis set to frequency and logarithmic (as the test was performed with Frequency Scaling set to Logarithmic). The X axis can be set to Log by double left clicking on any axis and adjusting the Axis Settings.

• Left Y axis set to storage modulus.• Right Y axis set to loss modulus.• Hide Reference Frequency selected.

Figure 11.16 Variable Frequency test result

11.3.2 VARIABLE LOADWith the release of the nanoDMA III software Hysitron has introduced the CMX testing mode (discussed in the next

section) which is an improved method of variable load test and should be used for most variable load situations. The

traditional variable load test is still possible to perform in nanoDMA III software but not the preferred method.

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During a ramping quasi static load test, the quasi static load is varied with each progressive step. During this type of

test, a fixed frequency is chosen and the dynamic load amplitude can be held constant or varied with the quasi static

load.

A variable load test can be set up by starting with a basic quasi static trapezoid load function (from the Standard Load

Functions menu). Select the hold segment and click the nanoDMA Segment Generator button to adjust the Start and

End Loads while keeping the frequency constant.

11.3.3 CMXThe addition of CMX (Continuous Measurement of X) capabilities is one of the major improvements implemented

with the nanoDMA III software release. There are two types of CMX load functions available from the Standard

Load Function menu:

• Constant Strain Rate CMX• Linear CMX

Both types of tests will perform continuous measurements of various parameters (at the defined data acquisition rate)

but the loading segment will vary as either exponential increasing load or linear increasing load.

It is important to note that the constant strain rate test, similar to the indentation constant strain rate, is an exponential

that imitates a constant strain rate. The test is actually multiple linear segments arranged in an exponential loading

arrangement. The exponential function used is discussed in the Partial Unload & Constant Strain Rate section of the

instrument primary user manual.

An example of the Constant Strain Rate CMX test is given in Figure 11.17.

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Figure 11.17 Constant Strain Rate CMX test

To modify the load the user should adjust the Peak Force parameter. To modify the dynamic load amplitude the user

should set the Load Amplitude Scaling (as desired, typically Variable Dynamic Load) then choose a nanoDMA

segment from the load function (Figure 11.17 has the first segment of the constant strain rate selected) and enter the

desired Begin Load Amplitude. To update all segments with regard to the Load Amplitude Scaling selected click the

All button next to the Begin Load Amplitude parameter.

The All button must be selected in order to updating the scaling for the entire load function based on the scaling and load amplitudes entered by the user.

An example result window from a constant strain rate CMX test is given in Figure 11.18.

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Figure 11.18 CMX test result

USING A CMX TEST TO CALCULATE A PROBE AREA FUNCTIONIt is possible to use a CMX test on fused quartz to calculate a probe area function (as opposed to performing multiple

nanoindentation tests at various loads on the fused quartz sample). To use a CMX test to calculate a probe area

function the following procedure should be used:

1. Install the fused quartz sample, define the boundary, and approach the sample to start imaging the surface.

2. Go to the Load Function tab Indentation sub tab Standard Load Function menu Constant Strain Rate CMX.

3. Set the Peak Force to the maximum force that is desired for the calibration (typically around 9-10 mN). It is important to note the maximum force of the transducer (given on the Calibration tab System Calibration sub tab Indentation Axis heading) is the maximum indentation with dynamic component. With the Peak Force set to 9-10 mN the Begin Load Amplitude (with the scaling set to Variable Dynamic Load) will be calculated to forces that will work well on the fused quartz sample so no additional modifications are required for this load function.

The Peak Force of the load function plus the Load Amplitude at the peak force cannot exceed the Maximum Force defined on the Calibration tab System Calibration sub tab Indentation Axisheading.

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4. Run the test at a minimum of four locations to confirm the result is similar. The first test may have more influence from drift but the final two tests should be very similar. This is important because the probe area function is being solved from one test and if that test has influence from drift or sample movement the calibration may be invalid.

5. When a satisfactory test has been completed, go to the Calibration tab Tip Calibration sub tab Calculate sub tab File menu Open menu option File of Type pull-down menu (Figure 11.19) and select the nanoDMA III data file performed from step 3.

Figure 11.19 Using a nanoDMA III data file for

a probe area function

6. The data will plot and fit identical to the standard indentation probe area function calculation.

11.3.4 REFERENCE CREEPA dynamic reference creep test is similar to a creep test performed with the three-plate capacitive indentation,

however, with the use of reference frequencies the test time can be much longer and because of the dynamic

components (in combination with the CMX capabilities) the test will continuously measure hardness, stiffness,

modulus, etc...

An example of dynamic reference creep test is given in Figure 11.20. A reference creep test is a test with an initial

reference frequency segment followed by a long constant force dynamic segment. The first reference frequency

segment will be used to calculate the contact area and the second (longer) reference frequency segment will be

analyzed as the creep segment.

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Figure 11.20 Reference Creep test

An example result from a reference creep test is given in Figure 11.21. When analyzing reference creep tests the Hide

Reference Segments must be unchecked (as all nanoDMA segments are reference segments). A typical reference

creep test will plot Reference Hardness and Reference Contact Depth vs. Time (as shown in Figure 11.21).

Figure 11.21 Reference Creep test result

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11.4 NANODMA TESTING SUGGESTIONSThe optimal displacement amplitude for most dynamic tests is 1-2 nm. The Load Amplitude that is chosen will affect

the measured displacement amplitude. One or two tests may need to be conducted on a sample to determine the

optimal Load Amplitude before automated testing is performed.

During the drift correction process, there is no control over the force on the sample caused by the drift. If the

Maximum Drift Time is set for a very long time, the probe may lose contact with the sample during the drift check,

causing a bad drift measurement. If the drift is in the positive direction, then the preload will increase, causing an

error in the displacement during a test. To minimize either of these effects, it is recommended that the maximum drift

time is kept to less than 20 seconds.

Because of the longer time associated with nanoDMA testing it is recommended that most nanoDMA testing be

performed from imaging (perform an in-situ SPM image of the sample, locate the area of interest and perform the

test). It is recommended, when possible and if available, to perform nanoDMA tests with either automated methods

or piezo automations. This will lower the drift in the system and produce better results.

The probe area function for the probe being used in an experiment should be defined before the test is started. It is

much more difficult to change this in the files after the data has been acquired.

For low displacement amplitude testing (such as when working at shallow contact depths) the user may want to

increase the Lock-in Input Gain from the Calibration tab System Calibrations sub tab nanoDMA Settings

heading to 100 to increase the signal-to-noise ratio.

11.5 NANODMA DATA ANALYSISThe nanoDMA III analysis tab is located under the Analysis tab nanoDMA sub tab (Figure 11.22). nanoDMA III

data files have a *.tdm extension. Whenever a nanoDMA III data file is saved there will be an associated *.hys

(indentation file) saved as well. Whenever the nanoDMA III data file is opened the associated indentation curve will

also be loaded in the Analysis tab Quasi sub tab.

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Figure 11.22 nanoDMA sub tab

The nanoDMA sub tab has multiple menu items, tabs, and buttons that will be discussed in this section of the user

manual.

Similar to the load function section of this user manual, this section is written with the software in Custom mode

(from the User Mode menu item). If features discussed in this section are not present the user should verify that the

User Mode from the nanoDMA sub tab is set to Custom.

MENUSThere are three menus on the nanoDMA sub tab:

• File• Plot• User Mode

The File menu has several options discussed below:

Open Single File The Open Single File option allows the user to load a single nanoDMA III data file. There is also an Open Single File shortcut button.

Open Multiple Files The Open Multiple Files option allows the user to load multiple nanoDMA III data files. There is also an Open Multiple File shortcut button.

Add File(s) The Add File(s) option allows the user to load additional files to the already opened nanoDMA III data files. There is also a Add File(s) shortcut button.

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Edit File The Edit File option opens the Edit File Parameters window where the user can view and modify many parameters. Only advanced users should access and modify parameters within this window. There is also a Edit File shortcut button.

Rename .tdm File The Rename .tdm File option allows the user to change the name of the currently open nanoDMA III data file.

Dynamic Calibration The Dynamic calibration option opens the nanoDMA Calibration window with the currently loaded nanoDMA III data file as the data to be used for the calibration.

Export to ASCII The Export to ASCII option exports the currently loaded nanoDMA III data file to an ASCII file. Upon selecting this option the data file is automatically created in the same directory with a *.txt extension. There is also an Export to ASCII shortcut button.

Export to ASCII Options

The Export to ASCII Options allows the user to determine which portions of the data file are exported. The different portions include quasi static data, dynamic data, average/standard deviation data, and reference frequency data. After selecting the desired data to export the user must select OK and then go back to the Export to ASCIIoption to export the desired data. There is also a Export to ASCII Options shortcut button.

Update Multiple Files The Update Multiple Files option allows the user to update files based on the values entered in the Calibration tab System Calibration sub tab. Upon selecting the Update Multiple Files option the user will be prompted to select the files for updating then a window will open asking which parameters to update. This option should be used with caution as it will update parameters from the System Calibration sub tab which may be different for different data files.

Multiple File Re-Zero Offsets

The Multiple File Re-Zero Offsets option allows the user to offset the data files to a new origin position (similar to the offset options available with indentation tests). Upon selecting the Multiple File Re-Zero Offsets option a window prompts the user if they would like to perform a load and/or displacement offset. Offsets can be performed in the nanoDMA or Quasi sub tab and the results will be reflected in both tabs.

The Plot menu has several options discussed below:

Plot Label The Plot Label option allows the user to modify the text and font style for the nanoDMA plot title.

X Axis The X Axis option allows the user to modify the text and font style for the nanoDMA plot X axis.

Left Y Axis The Left Y Axis option allows the user to modify the text and font style for the nanoDMA plot left Y axis.

Right Y Axis The Right Y Axis option allows the user to modify the text and font style for the nanoDMA plot right Y axis.

X-Y Axes The X-Y Axes option allows the user to modify the font style for the X and Y axes.

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Zoom Mode The Zoom Mode allows the user to select a zoom mode for modifying the nanoDMA plot. Options include Around Point, Rectangle, X Axis, and Y Axis. Each of these zoom options also have a corresponding shortcut button. To use the zoom options, the user must select the desired zoom then hold the CTRL key while selecting the zoom area with the mouse. The nanoDMA plot also has the option (like all other plots within TriboScan) to zoom in and out by holding the CTRL key and left and right clicking, respectively.

Any plot can also be double left-clicked to open the Axis Settings window which will allow the user to set the scaling (or return the plot back to auto scaled).

The User Mode menu has two options (Standard and Custom). Standard mode is an abbreviated version of Custom

mode with the most commonly used options and features active in order to present a simpler user interface.

BUTTONSThere are several buttons on the nanoDMA III Analysis sub tab. Each of the menu buttons given in the list below also

appear as functions in the menu bar and have been discussed in the previous section (Menus). The buttons include:

• Open Single File• Open Multiple Files• Add File(s)• Edit File• Export to ASCII• Export to ASCII Options• Auto Scale Axes• Zoom Around Point• Zoom Rectangle• Zoom X Axis• Zoom Y Axis

There is also three buttons below the tabs inside the nanoDMA sub tab:

• Graph to Clipboard: Saves the current plot to the clipboard to be pasted into other programs as an image.

• Toggle Grid: Toggles an X, Y, or X & Y grid on the displayed plot.• Show Legend: Displays a legend of the currently loaded data files.

TABSThere are three tabs within the nanoDMA sub tab that are used to determine the values plotted, plotting styles, and

other parameters. The tabs include:

• Data Selection• Data Point Values• Multiple Files

To the right of the three tab options there is a >> button. This button will collapse the tabs to allow for a larger view

of the current plot. Click the << button to expand the tabs after they have been collapsed.

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Data Selection The Data Selection tab allows the user to select the value(s) to plot on the X, YL (left), and YR (right) axes (Figure 11.23). Only one value can be selected for each axis.

Figure 11.23 Data Selection tab

There is a Data Plotted pull-down menu within the Data Selection tab that allows the user to define the range of data plotted. Options include:

• Plot All Data Points: All data is plotted• Plot Selection of Data Points: Two additional parameters will appear to allow

the user to set a From and To time to be plotted.• Plot Per-File Selection of Data Points: With this option the user must set plotted

time ranges from the Multiple Files tab.• Plot Averaged Data Points: With this option the user will see the average data

with associated error bars.

The Hide Reference Segments check box at the bottom of the Data Selection tab will hide all reference frequency segments (if the exist) in the plotted data. This is typically desirable as the reference frequency data is not usually used for the analysis.

Data Point Values The Data Point Values tab (Figure 11.24) displays the calculated and measured values for the currently selected point on the plot. The Index parameter indicates which point is currently selected.

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Figure 11.24 Data Point Values tab

Multiple Files The Multiple Files tab (Figure 11.25) displays plotting options for each of the loaded nanoDMA data files. The Multiple Files tab allows the user to modify the plot color, style, name, time plotted, etc... Many of the parameters within the Multiple Files tab are editable, however, to return to software defaults the data file will need to be reloaded. Some parameters such as font size/style will require a software restart to return so the software default values.

There are three buttons on the Multiple Files tab to add, remove, and clear files. The buttons are Add File(s) (the same as the Add File(s) menu button), Remove File, and Clear List.

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Figure 11.25 Multiple Files tab

11.5.1 NANODMA DATA ANALYSIS DETAILSDuring a nanoDMA test, an indentation force (quasi static) and a much smaller dynamic load at a user prescribed

frequency is applied to the sample with the nanoindentation probe using a lock-in amplifier. The resulting signal is

analyzed using the lock-in amplifier to measure the displacement amplitude and phase shift. A graph of the measured

dynamic displacement (d), applied dynamic force (F), and phase shift (φ) is given in Figure 11.26.

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Figure 11.26 Dynamic signals

The nanoDMA analysis is performed with some information entered from the user (such as the probe area function

that relates contact area to contact depth) and the following equations.

The sample damping (Cs) is calculated by the following equation:

where the [ACActForce] is the dynamic actuation force, [ACDisplacement] is the dynamic displacement, ϖ is the

radial frequency, and CT is the transducer damping.

The storage stiffness (kstorage) is calculated by the following equation.

where kstorage is defined as the storage stiffness, mT is defined as the mass of the transducer, and kT is defined as the

stiffness of the transducer.

The loss stiffness can be expressed as the following equation:

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The complex stiffness (kcomplex) can be expressed as:

where [MC] is defined as the system machine compliance.

The tan delta is a useful parameter used to define viscoelastic sample behavior. The tan delta is not dependent on the

area function of the probe and is expressed as the ratio of the loss to storage modulus values.

The contact displacement (hc) for the nanoDMA III analysis is calculated slightly different from the standard method

the user may be accustomed to:

where h is the maximum displacement, ϵ is defined as a geometric constant related to the probe (default value is 0.75

but is editable from the Edit File window), P is the maximum force, and k is the stiffness (hard-coded to storage

stiffness).

The contact area (Ac) is defined similar to the standard indentation analysis. With the nanoDMA III analysis an offset

factor (B) has been introduced that allows the area function fit to deviate from a fit through the origin. The offset

factor can be very useful when using a flat-ended probe (where the user would set the C0 - C5 to zero and set B to the

area of the flat-ended probe).

The modulus (E) (storage, loss, and complex) can be solved with the following equation:

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where k is given as the storage, loss, or complex stiffness to obtain the respective modulus value.

Hardness can be solved for with the maximum force (P) and contact area (Ac):

If the nanoDMA III tests are being performed with reference frequency segments the contact area (Ac) is calculated

differently:

where k is stiffness (hard-coded to storage stiffness) and Ereference is the reference modulus as defined by the user or

as measured with the first reference frequency segment (depending on the load function set up).

11.5.2 NANODMA DATA ANALYSIS PROCEDUREThe nanoDMA III data analysis window is displayed after completion of a nanoDMA test and can be accessed by

selecting the Analysis tab nanoDMA sub tab.

The user can select the plots to display by the check boxes on the left side of the nanoDMA sub tab. The results have

been calculated based on the currently loaded area function and transducer constants. If needed, the area function and

transducer constants parameters can be changed from the Edit File window in order to modify the saved data files.

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Figure 11.27 nanoDMA III data analysis

(nanoDMA sub tab)

When the nanoDMA III data file is loaded, the associated indentation data file is also loaded in the Analysis

tab Quasi sub tab. The indentation data file can be treated similar to a standard indentation plot and be analyzed (if

desired).

More detailed analysis descriptions for specific testing methods is discussed in previous sections of this user manual.

Some information to remember while analyzing and/or modifying the nanoDMA III data files:

• Force and displacement offsets performed in the Quasi sub tab will affect the nanoDMA sub tab. Force and displacement offsets performed in the nanoDMA sub tab will not affect the Quasi sub tab.

• Area function changes performed in the Quasi sub tab will affect the nanoDMA sub tab. Area function changes performed in the nanoDMA sub tab will not affect the Quasi sub tab.

• Area function changes performed in the Quasi sub tab will not affect any pre-defined B (offset) value that has been entered on the nanoDMA sub tab.

• The nanoDMA sub tab will use always use the area function that was saved on the system when the test was performed. To change the area function the Edit File window must be updated. The Area Function pull-down menu on the Quasi sub tab will not affect the nanoDMA sub tab.

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• Machine compliance changes performed in the Quasi sub tab will affect the nanoDMA sub tab. Machine compliance changes performed in the nanoDMA sub tab will not affect the Quasi sub tab.

• No other parameters (such as the load scale factor or displacement scale factor) will update between the two data files when changes are made.

• nanoDMA III data files are analyzed with the area function that was saved on the system at the time of the test. The area function must be updated from the Edit File window in order to apply a new area function.

11.6 MODULUS MAPPINGThe TI series systems can be upgraded to include modulus mapping capabilities. Modulus mapping is a software only

upgrade to a system with nanoDMA installed. If the user is unsure if the system has modulus mapping capabilities

contact Hysitron for information.

During a modulus map test, the nanoindentation probe is scanned across the surface in a raster mode to image the

sample. The lock-in amplifier sends a dynamic signal to the drive plate of the transducer, causing the probe to

oscillate during the image. Because the oscillation is much faster than the feedback response of the piezo scanner, the

in-situ SPM image is not affected. The lock-in amplifier continuously analyzes the resulting signal from the

transducer and outputs the phase and amplitude to the TriboScan software producing plots of phase and amplitude as

the surface is imaged.

The software can analyze the phase and amplitude signals (as is done with nanoDMA testing) to find the stiffness and

damping. In order to calculate the storage and loss moduli from the stiffness and damping data, the projected contact

area between the probe and sample must be known. The contact area is calculated based on the radius of curvature of

the nanoindentation probe.

The modulus mapping software is divided into two parts: acquisition software and analysis software. During data

acquisition, the software is used to control the settings for the lock-in amplifier. The analysis software is used to

create the maps of the sample based on the properties found during the data acquisition.

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Figure 11.28 3D modulus map of ceramic

fiber within a matrix rendered in TriboAnalysis

11.6.1 ACQUISITION SOFTWAREThe data acquisition and analysis is performed within the TriboScan software suite. This section requires the use of

the system in-situ SPM imaging capabilities and the user should be familiar with the in-situ SPM imaging operation

and capabilities.

DATA ACQUISITION SOFTWAREA modulus map is essentially an in-situ SPM image being performed at the same time as a dynamic test. The modulus

mapping data acquisition software consists of a window to set the parameters of the lock-in amplifier and the Imaging

tab to collect the resulting in-situ image. Because the test is performed during the imaging process and a standard load

function is never created or used, the Lock-In Control window is, in essence, the load function creator for modulus

map tests. The Lock-In Control window is accessed by selecting the Imaging tab Lock-in Control icon in the

upper left corner (Figure 11.29).

Figure 11.29 Lock-in control icon

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The location of the Lock-in Control window may vary by software version, however, the icon will remain unchanged

and could be located on the nanoDMA Load Function sub tab (nanoDMA I or II) or Imaging tab.

MODULUS MAPPING SETUP WINDOWThe Modulus Mapping Setup window provides the user with real-time control of the lock-in amplifier. The Modulus

Mapping Setup window is shown in Figure 11.30.

Figure 11.30 Modulus Mapping Setup

window

A description of the controls available from the Modulus Mapping Setup window are listed below:

Frequency The Frequency parameter is the user defined frequency of the oscillation applied to the probe during imaging. The range is 1 Hz to 300 Hz. The default setting is 200 Hz. If the frequency is set to a lower value the scan rate will also need to be reduced to allow for adequate data collection.

Load Amplitude The Load Amplitude parameter is the user defined amplitude of the dynamic force that is applied to the probe during imaging. The range is 0.001 μN up to the maximum force allowed by the transducer. The default value is 2 μN and typical values range from about 0.5 μN up to 10 μN.

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Lock-In Time Constant

The Lock-In Time Constant parameter is the user defined time constant, or the length of time the lock-in amplifier locks in on the signal before updating. For higher frequencies, smaller time constants can be used to obtain better resolution in the image. Larger time constants will average the data longer during the imaging, and can cause streaks in the images. Smaller time constants will improve the lateral resolution of the image, but will also increase the noise, because the data is not averaged as long. The default value is 10 ms and the typical setting is usually 10 ms or 3 ms.

Lock-In Sensitivity The Lock-In Sensitivity parameter is the user defined sensitivity, or range that is used by the lock-in amplifier for measuring the amplitude of the displacement signal. A larger sensitivity must be used for larger oscillations. For small oscillations, the resolution will be better when a smaller sensitivity is selected. The default value is 50 mV/nA.

Filter Slope The Filter Slope parameter is a digital filter that reduces data at frequencies that the lock-in amplifier is not concerned with regarding the current measurement signal. Increasing the Filter Slope parameter will reduce the noise measured by the lock-in amplifier, however, this may result in a longer roll-off time (the time required between frequency adjustments for the lock-in amplifier to stabilize). The default setting is 18 dB/oct. For more details consult the SRS lock-in amplifier user manual.

Reserve The Reserve parameter is a ratio of the largest tolerable noise to the full scale signal without the lock-in amplifier sensing an overload (how well the lock-in amplifier is able to filter out the non-signal frequencies). A High reserve would indicate very effective filtering at a cost of resolution. A Low reserve the would include more electronic noise from the lock-in amplifier but higher resolution. The default setting is Normal. For more details consult the SRS lock-in amplifier user manual.

Low Pass Filter The Low Pass Filter parameter allows the user to enable a low pass filter when performing a modulus map test. The low pass filter will prevent the piezo scanner from retracting or extending with the oscillation probe during the scanning process (thus producing an undesirable image). The low pass filter should be Enabled when performing a modulus map test and when the low pass filter is Enabled the Scan Ratefrom the Imaging tab will need to be reduced to produce a desirable image.

Low Pass Filter Order The Low Pass Filter Order parameter allows the user to toggle between a First and Second order low pass filter. The performance of the Second order low pass filter is typically more desirable and will usually be the preferred filter selection. A plot showing the response of the low pass filter based on the order selection is given in Figure 11.31.

Low Pass Filter Cutoff Frequency

The Low Pass Filter Cutoff Frequency parameter allows the user to determine what high frequency data will be filtered in the resulting modulus map test.

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Figure 11.31 Modulus mapping low pass filter

response

Start/Restart Button The Start/Restart button sets the lock-in amplifier to the desired settings listed in theparameters on the Modulus Mapping Setup window. After any changes to the parameters on the Modulus mapping Setup window the Start/Restart button must be selected for the changes to be effective.

Stop Button The Stop button stops all lock-in amplifier operation. The Stop button should be used when modulus map testing has been completed and the user would like to perform a standard in-situ SPM image or nanoindentation test.

Load Amplitude The Load Amplitude parameter will be updated with the current amplitude being measured by the lock-in amplifier whenever the Start/Restart button or Refresh Statusbutton is selected.

Dynamic Displacement

The Dynamic Displacement parameter will be updated with the current displacement being measured by the Hysitron control unit whenever the Start/Restart button or Refresh Status button is selected.

Phase Shift The Phase Shift parameter displays the difference, in degrees, between the oscillating load and the resulting oscillating displacement as measured by the lock-in amplifier. The Phase Shift is updated whenever the Start/Restart button or Refresh Status button is selected.

Lock-In Overload The Lock-In Overload indicator light will illuminate red colored if any settings (typically Lock-In Time Constant or Lock-In Sensitivity) are set too low and result in an overload signal to the lock-in amplifier. Adjust the parameters and click the Start/Restart button to resolve the issue.

THE IMAGING TABThe Imaging tab is identical to the standard Imaging tab with the exception of the Channel Selection window

(accessed from the Channel Selection button on the button bar or the Control Channel Selection menu. When the

system is licensed for modulus mapping, a Select Modulus Mapping button will appear in the Channel Selection

window (Figure 11.32). This button will automatically select the channels necessary to collect a modulus map.

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Figure 11.32 Modulus mapping imaging tab

options

11.6.2 ANALYSISWith SPM+ the modulus mapping analysis is performed in real-time and images are saved in *.BCRF format to be

opened in TriboView (5.9 or higher). For systems not equipped with SPM+ contact Hysitron for documentation

related to the stand-alone modulus mapping analysis program or information on upgrading to SPM+.

11.6.3 TESTING PROCEDUREThe following procedure is a general outline for setting up and completing a modulus map test:

1. Set the TriboScan software to Indentation mode: The Indentation mode is selected from the Mode pull-down menu on the Action Bar. The mode cannot be changed when the probe is in contact with a sample.

2. Select additional images to capture: In addition to obtaining a topographical and gradient image of the surface, additional images will also need to be captured. Select the Channel Selection button on the button bar and click theSelect Modulus Mapping button to select the appropriate images.

3. (Optional) Pre-scan the surface: Perform a quick (1-2 Hz) pre-scan of the surface so that the area of interest may be selected.

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4. Initialize the lock-in amplifier: Go to the Lock-In Control window (Lock-In Control button from the Imaging tab) and enter a frequency (10-300 Hz) at which to perform the test and click Initialize.

5. Begin scanning the sample surface: Begin scanning the sample surface at approximately 0.1 - 0.2 Hz. Slower scan rates may be needed for higher resolution imaging.

6. Set the lock-in amplifier: While scanning the sample surface, select an appropriate dynamic force, sensitivity and time constant from the Lock-In Control window and click Set.

7. Check the amplitude plot: An amplitude of about 0.3 - 1 nm is desirable (Figure 11.33), which may take some experimenting if the sample is unknown. To check the amplitude, select the amplitude in-situ image and view the scan line in the lower right corner of the Imaging tab.

Figure 11.33 Amplitude scan line during

modulus map

8. Adjust the dynamic load: Adjust the dynamic load in the Lock-In Control window (the Set button must be clicked after any adjustment in dynamic load) and check the scan line again until the amplitude is approximately 0.3 - 1 nm. Standard values for the lock-in amplifier control window are listed in Table 11.B. Of course, these values are only a starting point and will differ based on each materials unique properties.

Table 11.B Standard lock-in control window

values

9. Restart the image scan: After the appropriate amplitude has been found, restart the image scan and make sure an image base file name has been chosen and that the capture for the current image is turned on.

Standard Lock-In Amplifier Values

Generically Fused Quartz Porcelain Polycarbonate

Dynamic Load Yields ~0.4 nm amplitude 1-2 μN 0.5-1 μN 0.4-0.5 μN

Imaging Setpoint 2 μN 2-4 μN 1-3 μN 2-3 μN

Time Constant 3 ms 3 ms 3 ms 3 ms

Sensitivity 50 mV 50 mV 50 mV 50 mV

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ANALYSISModulus mapping files collected with SPM+ are saved as standard *.BCRF files and can be opened for further

analysis with TriboView. The images available for further analysis in TriboView are amplitude, phase, damping, loss

stiffness, storage stiffness, tan delta, loss modulus, and storage modulus.

Modulus map tests are heavily influenced by dirty probes. Because modulus mapping tests are typically only a few nanometers deep, any debris or contamination on the probe can greatly influence the calculated probe radius and thus the measured modulus values.

DETERMINATION OF PROBE RADIUSThe Measure Tip Radius Of Curvature command is an automated routine that examines the complex modulus image

and calculates the tip radius value that yields an average complex modulus of a defined value (typically 69.6 GPa for

the fused quartz sample). Because only a few nanometers of the probe are used during the modulus mapping test, the

calculated tip radius is typically much greater than measured from standard nanoindentation. After using the Measure

Tip Radius Of Curvature command, the software will inform the user what the calculated tip radius is and ask if the

value should be applied. The radius calculated will be saved on the system and applied to all modulus map tests until

the radius is recalculated.

The procedure for calculating the tip radius is given below.

1. Perform a modulus map on the fused quartz sample with the procedure defined in the previous section.

2. While performing the modulus map select the Control Tip Radius Calibration.

3. If the tip radius calibration is being performed on fused quartz leave the reduced modulus value as 69.6 GPa and click OK.

Modulus mapping tests are typically performed at very low displacements. Testing at very low displacements in

combination with the imperfect geometry of most indenter probes means that the measured tip radius can vary widely

depending on the displacement of penetration during a test. To further complicate this calculation, the displacement

of penetration will be dependent upon sample properties and is dependent on the setpoint force that is used in the

system imaging parameters.

Figure 11.34 illustrates how the apparent radius of a probe that has been flattened over time can vary with

displacement. Smaller displacements will generally require a larger radius. In order to calibrate the radius of a probe,

the Modulus Mapping radius of curvature (the procedure given in the above section) should be measured on fused

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quartz at a specific displacement. For the most accurate result, the displacement used during the probe radius

determination should be maintained on the unknown sample.

The Tip Radius parameter may not accurately reflect the measured tip radius from the area function calibration. This is normal as modulus mapping tests are performed at much smaller displacements the calculated tip radius will likely appear to be much larger. Typically, the user can expect the Tip Radius parameter to be around ten times the measured tip radius from the quasi static software.

Figure 11.34 Deep and shallow indentation

test showing different probe radius determination

The general procedure for finding an appropriate radius is outlined in the following steps:

1. Perform a modulus map on the unknown sample using the procedure given earlier in this section of this user manual.

2. Perform a nanoindentation test on the unknown sample (usually a load controlled test, around 20-50 μN peak force with a 10-20 nm lift height) to find the displacement during modulus map. Use the resulting force vs. displacement plot to locate the measured displacement at the setpoint force.

3. Perform a nanoindentation test on the fused quartz standard to find the setpoint force required to match the displacement measured in step 2 (above). A plot showing this step is given in Figure 11.35.

Because this procedure is working at very low displacements and forces, it is important that the plots used in step 2 and 3 are properly zeroed (illustrated in Figure 11.35).

4. Perform a modulus map on the fused quartz standard using the setpoint load determined from step 3 and the procedure in given earlier in this section of this user manual.

5. Use the Tip Radius Calibration procedure to find the tip radius used for the testing displacement.

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6. Use the Tip Radius found in the previous section and perform an new modulus map on the unknown sample (which will use the newly calculated tip radius).

Figure 11.35 Using TriboScan to measure the

displacement at a given force

Currently the tip radius value can not be updated in previously collected modulus map files.

The apparent tip radius may be influenced by probe wear, accumulation of debris, or surface features. It is important to check the tip radius calibration frequently

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SECTION | XPROBE TRANSDUCER• xProbe transducer option installation, connections, and calibrations• xProbe testing suggestions, limitations, and warnings

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This section of the user manual is intended for users with an xProbe transducer. If you are unsure if your system has

an xProbe transducer contact Hysitron for additional information. Due to numerous similarities, some portions of this

section will refer to the TriboIndenter base portion of this user manual.

The xProbe transducer is a MEMS-based rigid probe transducer that operates at previously unimaginable force and

displacement ranges. The xProbe transducer offers near AFM displacement and noise levels while preserving the

quantitative measurements of the standard Hysitron transducers.

This section of the user manual assumes the user has read and is familiar with the TriboIndenter base user manual and

the following calibrations have been satisfactorily performed:

• Optic-Probe Offset (H-pattern) calibration Alternate information will be discussed in this section

• Probe area function Alternate information will be discussed in this section

• Tare value verification• Indentation Axis calibration

Additional information will be discussed in this section

The system must be set up and the calibrations listed above performed before continuing with the nanoDMA section


CHAPTER 12 XPROBE TRANSDUCER

The xProbe transducer is a MEMS-based transducer that extends the characterization capabilities of Hysitron

instrumentation down to angstrom level measurements. The MEMS-based transducer continues to use electrostatic

actuation with MEMS fabrication to offer significantly more sensitive load and displacement measurement. The

xProbe transducer is built with a high axial stiffness to increase he mechanical bandwidth which improves the

feedback response time (this enables high strain rate testing).

The xProbe is available in indentation only (standard) mode and scratch (two dimensional; lateral).

12.1 PROBEThe xProbe transducer and probe are a single assembly and care not interchangeable. Different geometry probes are

available fore the xProbe transducer but the entire transducer and probe assembly is ordered and installed as one

piece. Any physical contact with the xProbe probe will result in damage to the MEMS-based transducer and/or

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diamond probe. Do not attempt to touch, modify, or remove the probe from the xProbe transducer.

! Do not touch, modify, or attempt to remove the probe from the xProbe transducer.

12.2 HARDWARE INSTALLATIONThe xProbe transducer attaches to the TriboScanner piezo scanner and connects to the same transducer electrical

connection as the standard capacitive transducer. If the system is equipped with a dual head configuration the xProbe

transducer can be used in slot 1 or 2.

No additional wiring or connections are required for the xProbe operation.

Figure 12.1 xProbe transducer connection

12.2.1 XPROBE TRANSDUCER DETAILSThe xProbe transducer is extremely fragile and the user should avoid any contact with the MEMS-based transducer

and probe. Contacting the MEMS-based transducer and/or probe will cause damage to the system requiring return to

Hysitron for repair.

The xProbe transducer is shipped with a protective acrylic cube (Figure 12.2). The protective acrylic cube covers the

MEMS-based transducer and probe when not in use (when stored in the supplied black plastic case with pink foam)

and when handling the xProbe transducer before and after the installation.

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The protective acrylic cube is attached with two friction-fit pins so it will push on and pull off without any setscrews

or other securing device. The protective acrylic cube should be removed before the xProbe transducer is installed on

the TriboScanner and it should be reinstalled immediately after removing the xProbe transducer from the

TriboScanner.

Figure 12.2 xProbe transducer details

! The protective acrylic cube should be used when the transducer is stored, transported, or otherwise handled. Any contact with the MEMS-based transducer or diamond probe will cause damage requiring the xProbe transducer to be returned to Hysitron for repair.

12.2.2 XPROBE TRANSDUCER SPECIFICATIONSThe MEMS-based xProbe transducer is significantly more sensitive than other transducers offered by Hysitron. With

the increased sensitivity the transducer will have lower force and displacement limits than other Hysitron transducers.

Do not attempt to operate the xProbe transducer beyond the limits given below.

Table 12.A xProbe transducer specifications xProbe 2D (lateral) xProbe

Indentation Displacement Range

500 nm 2 μ

Indentation Displacement Noise

0.02 nm 0.3 nm

Indentation Maximum Force

1 mN 500 μN

Indentation Force Noise

2 nN 30 nN

Lateral Displacement Range

N/A ~60 μm(TriboScanner piezo range)

Lateral Displacement Noise

N/A 0.5 nm

Lateral Maximum Force

N/A 150 μN

Lateral Force Noise N/A 50 nN

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xProbe Transducer

CHAPTER 13 XPROBE TRANSDUCER OPERATION

When using the xProbe transducer it is important that the user select the xProbe transducer from the software start up

splash screen (Figure 12.3). It is important to select the xProbe transducer from the splash screen when using the

xProbe transducer hardware because different limits will be applied to the system to prevent damage to the sensitive

MEMS-based hardware.

Always operate the xProbe transducer hardware with the software set to xProbe (from the splash screen).

Figure 12.3 xProbe selection

After TriboScan has started the Transducer Slot toggle switch on the Action Bar should be set to xProbe (Figure 12.4)

in order to activate the xProbe transducer and apply the necesssary limits to the xProbe transducer.

Figure 12.4 xProbe transducer slot

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xProbe Transducer

13.1 XPROBE TRANSDUCER CALIBRATIONSThe calibrations discussed in this section are specific to the xProbe option. This section is intended as a supplement to

the System Calibrations section presented earlier in this user manual.

! Calibrations in the earlier presented System Calibrations section must be completed and/or verified before performing sample testing.

13.1.1 VERIFY THE TRANSDUCER CONSTANTSTransducer constants (as discussed in the TriboIndenter base user manual) should be verified. This includes the Load

Scale Factor, Displacement Scale Factor, Electrostatic Force Constant, and Plate Spacing. The electrostatic force

constant and plate spacing lower limits will be adjusted from the default transducer when toggled into xProbe mode.

The default Electrostatic Force Constant value for xProbe is about 0.01 and the default Plate Spacing for xProbe is

about 10.

13.1.2 TRANSDUCER INDENTATION AXIS CALIBRATIONThe Transducer Indentation Axis Calibration for xProbe is initiated identically to the standard Transducer

Indentation Axis Calibration. The force that is automatically calculated for the Peak Force of the load function will

be lower to reflect the lower maximum displacement range of the xProbe transducer.

13.1.3 LATERAL AXIS CALIBRATIONThe 2D (lateral) xProbe transducer does not require a lateral axis calibration because the movement in the lateral

direction is performed by the TriboScanner piezo scanner.

13.1.4 OPTIC-PROBE TIP OFFSET CALIBRATIONThe Optic-Probe Tip Offset calibration is performed identically to the process defined in the TriboIndenter base user

manual with a few exceptions:

1. Due to the lower force and displacement range it will be more difficult to optically locate the pattern. Using the Automatic Optic-Probe Tip Offsetcalibration (ATOCW) is suggested whenever possible.

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xProbe Transducer

2. If the xProbe geometry is a cube corner or Berkovich the calibration pattern should be visible.

3. Do not perform the manual Probe-Tip Optic calibration with the imaging only AFM-probe style xProbe transducer. This very sharp probe is not intended for high force and displacement testing (imaging only) and performing the Probe-Tip Optic calibration with this imaging only xProbe will damage it. Use the ATOCW calibration with this xProbe.

4. For systems previous to TriboScan 10 the Probe-Tip Optic offset may need to be adjusted manually to account for small differences between optical focus and lateral imaging. The manual adjustment is located at Calibrationtab Stage Calibration sub tab Setup menu Adjust Tip-Optic Offset.

! Do not perform the manual Probe-Tip Optic calibration with the imaging only AFM-probe style xProbe transducer.

13.1.5 PROBE AREA FUNCTION The probe area function calibration is performed identical to the process discussed in the TriboIndenter base user

manual. There are limitations on force and displacement for the MEMS-based xProbe transducer that cannot be

exceeded. Imaging only AFM-probe style xProbe should be used for imaging only and performing a probe area

function with this xProbe transducer will dull or damage the probe.

! Imaging only AFM-probe style xProbe should be used for imaging only and performing a probe area function with this xProbe transducer will dull or damage the probe.

13.2 XPROBE TRANSDUCER TESTING & ANALYSISThe testing, analysis, and in-situ imaging process for the xProbe transducer is identical to the standard transducer

with the exception of the lower force and displacement limits and the lower noise levels (allowing for lower setpoint

and preload forces depending on overall system noise).

13.2.1 GAIN SETTINGSThe default gains used for the standard transducer (as defined in the TriboIndenter base user manual) are good

starting values for the xProbe transducer. It is suggested the user start with the standard transducer load function gains

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xProbe Transducer

and adjust by small increments up or down to find optimal gain settings for your system. Optimal gain settings will

produce a stable, desired result with minimal overshoot and reasonable response time.

The default in-situ SPM imaging Integral Gain is about 30.

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3D OmniProbe/MultiRange NanoProbe

SECTION | 3D OMNIPROBE/MULTIRANGE NANOPROBE

• 3D OmniProbe/MultiRange NanoProbe (indentation forces up to 10 N and displacements up to 80 µm) option installation, connections, and calibrations for TriboIndenter system

• 3D OmniProbe/MultiRange NanoProbe test creation and analysis

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This section of the user manual is intended for systems that have purchased the 3D OmniProbe/MultiRange

NanoProbe (MRNP) option. Due to numerous similarities, some portions of this section will refer to the base portion


This section of the user manual assumes the user has read and is familiar with the TriboIndenter base section and the

following calibrations have been satisfactorily performed:

• Optic-Probe Offset (H-pattern) calibration• Probe area function (for MultiRange NanoProbe transducer)• Tare value verification

The system must be set up and the calibrations listed above performed before continuing with this section of the user

manual.

All indentation tests with the 3D OmniProbe/MNRP are performed in feedback control. There are two modes of

operation for the feedback control: Load and Displacement control. With load control, the user will control the

probe’s force versus time, while measuring displacement. With displacement control, the user controls the probe’s

depth into the sample versus time, while measuring force. These two modes were discussed in more detail in the

TriboIndenter base section of this user manual

Actuation of the probe when performing an indentation is provided by a pre-stressed piezo material. As the voltage

applied to the piezo is increased, it will lengthen, pushing the probe into the sample. This is different than the

actuation discussed in the TriboIndenter base section of this user manual which uses electrostatic actuation (for three-

plate capacitive load testing and nanoDMA testing). The piezo actuation allows for larger forces and displacements

but the trade-off is the higher noise floor when compared to three-plate capacitive load indentation test results.

A load cell in series with the actuator and probe measures the force applied to the probe. A capacitive displacement

sensor in parallel with the actuator/probe/load cell measures the displacement of the probe. During an indentation

test, voltage is applied to the piezo actuator to push the probe into the sample. The voltage of the piezo is controlled

through a feedback loop based on the displacement sensor or load cell (for displacement control or load control). The

user will input the displacement or force vs. time, and the feedback loop will follow this ramp.

CHAPTER 14 3D OMNIPROBE/MRNP HARDWARE

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The basic components of the 3D OmniProbe/MRNP option is listed below:

• 3D OmniProbe/MultiRange NanoProbe (MRNP) transducer head• Hysitron control unit• Properly licensed TriboScan 9 (or later) software• Nanoindentation probe for 3D OmniProbe/MultiRange NanoProbe (MRNP)• Cabling

! The 3D OmniProbe/MRNP transducer is a very delicate component that is constructed primarily of fragile piezo material and carefully calibrated springs. Avoid any blunt or shear forces to the bottom (threaded portion) of the 3D OmniProbe/MRNP transducer.

! Although the diamond nanoindentation probes appear to be much larger and more resilient to damage they are still very fragile. Great care should be taken not to drop or contact the probe with any foreign objects.

14.1 INSTRUMENT CONNECTIONSThe 3D OmniProbe/MultiRange NanoProbe (MRNP) system is controlled with a Hysitron control unit (performech

or digital control unit). The 3D OmniProbe/MultiRange NanoProbe (MRNP) transducer head replaces the standard

piezo/transducer assembly and is installed in the standard system piezo dovetail. The installation of the transducer

head is discussed further in this user manual.

If the system is equipped with a dual head configuration the 3D OmniProbe/MRNP transducer can be installed in an

alternate slot from the standard piezo/transducer to allow for larger scale testing (with the 3D OmniProbe/MRNP)

and lower force imaging or testing with the standard piezo/transducer.

This section only discusses connections specific to the 3D OmniProbe/MultiRange NanoProbe. Any existing connections between the Hysitron control unit and other electronics or the instrument back panel should remain connected and undisturbed. If there are any questions regarding connecting the MultiRange NanoProbe, contact a Hysitron service engineer before proceeding.

Use the following procedure for connecting the 3D OmniProbe/MultiRange NanoProbe:

1. On the rear of the Hysitron control unit, connect the 25-pin cable between the Transducer 2 connection and the High Load or MRNP connection on the instrument back panel.

2. On the rear of the Hysitron control unit, connect the BNC cable between the High Load or MRNP BNC connection and the High Load or MRNP BNC connection on the instrument back panel.

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3. Within the instrument enclosure, connect the 25-pin cable from the back panel to the top of the MultiRange NanoProbe transducer head.

4. Within the instrument enclosure, connect the High Load or MRNP BNC from the back panel to the micro BNC located on the top of the 3D OmniProbe/MultiRange NanoProbe transducer head.

A connection schematic is shown in Figure 13.1. All existing standard instrument connections should remain

connected.

Figure 13.1 Connection Schematic for

3D OmniProbe/MRNP

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14.2 HARDWARE INSTALLATIONInstalling the MRNP/3D OmniProbe probe is performed similarly to the installation of a probe into a standard

transducer. The probe assembly, including the diamond probe, holder and threaded screw, is installed into a threaded

hole on the 3D OmniProbe/MRNP transducer head. A picture of the probe and probe mounting tool is shown in

Figure 13.3.

The 3D OmniProbe is equipped with X and Y axis sensors to allow for scratch testing. To protect the X/Y axis

sensors, the torsion guard, as shown in Figure 13.2, must be inserted into the 3D OmniProbe before installing or

removing the probe. To install the torsion guard, line up the four pins with the four holes on the bottom of the 3D

OmniProbe transducer and gently slide the guard into the holes. The MRNP is not equipped with X or Y axis sensors

so no torsion guard is required.

! Only install or remove the probe of the 3D OmniProbe transducer head with the torsion guard installed. Without the torsion guard in place, excessive torque will be applied to the X and Y sensors possibly causing damage.

Figure 13.2 The torsion guard

14.2.1 3D OMNIPROBE/MRNP NANOINDENTATION PROBE MOUNTINGUse the following procedure for mounting the probe assembly onto the 3D OmniProbe/MRNP transducer head:

1. Place the 3D OmniProbe/MRNP transducer head on its dovetail so that it is lay-ing horizontally.

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2. Carefully remove the probe from its protective sheath and hold the probe by the threaded portion with the non-dominate hand. The probe has a square mount just below the point of the diamond which fits into the probe mounting tool (Figure 13.3).

! Any contact between the diamond probe and the installation tool can chip or break the diamond probe.

3. With the probe tool in the dominate hand and the probe being held by its threads in the non-dominate hand, carefully insert the square portion of the probe into the probe tool.

4. With the probe inserted in the probe tool, place the threaded portion of the probe on the hole on the 3D OmniProbe/MRNP transducer head. The probe is only held in the tool by gravity, so care should be taken to prevent the probe from falling out of the tool.

! The probe is only held in the tool by gravity and can easily fall out if not held upright at all times. Take extra care so that the probe does not fall out of the tool during the installation.

5. Gently turn the probe anticlockwise until a slight click is felt when the lag of the screw falls into place.

6. Gently turn the probe clockwise until resistance is met. The probe installation tool is equipped with a spring to act as a torque wrench so that the probe cannot be over tightened; when the spring begins to deflect, the probe is fully installed.

7. Attach the 3D OmniProbe/MRNP transducer head to the dovetail mount on the instrument and tighten the dovetail 1/16” locking hex screw (located to the right of the dovetail when viewing the instrument from the front).

8. After the 3D OmniProbe/MRNP transducer has been installed on the Hysitron system the 25-pin transducer cable and the micro BNC cables can be connected to the top of the 3D OmniProbe/MRNP transducer head.

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Figure 13.3 Installing the probe onto a

MNRP transducer head

14.2.2 INSTALLING THE 3D OMNIPROBE/MRNP TRANSDUCER HEADThe 3D OmniProbe/MultiRange NanoProbe transducer head is connected to the instrument in the same position as

the three-plate capacitive transducer/scanner assembly (discussed in the TriboIndenter base section of this user

manual). If the system is equipped, the three-plate capacitive transducer and TriboScanner piezo scanner must first be

removed and stored in a safe location (preferably in the original shipping case) or moved to an alternate slot on dual

head equipped systems.

Gently slide the 3D OmniProbe/MRNP transducer head into the dovetail, ensuring that the dovetail catches on the

stop pin at the bottom of the dovetail mount before releasing. Tighten the 3D OmniProbe/MRNP transducer head in

the dovetail mount using the 1/16” hex set hex screw on the right side of the Z axis stage.

With the 3D OmniProbe/MRNP transducer head tightened in to the dovetail mount, connect the 25-pin Z Transducer

cable and the micro BNC Power cable. If the TriboScan software is running, TriboScan should be paused before

making any connections. If TriboScan is not running, the Hysitron control unit should be powered off prior to making

any connections. The installation of the 3D OmniProbe/MRNP transducer head is shown in Figure 13.4 on a

TriboIndenter.

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Figure 13.4 3D OmniProbe/MRNP

transducer head attached to a TriboIndenter

CHAPTER 15 3D OMNIPROBE/MRNP OPERATION

Prior to using the 3D OmniProbe/MultiRange NanoProbe transducer features, users should be familiar with standard

Hysitron software operation and all calibration/testing procedures for indentation testing (presented in the

TriboIndenter base section of this user manual).

! Before performing any 3D OmniProbe/MultiRange NanoProbe testing all necessary system calibrations should be performed. This may include but is not limited to the Indentation Axis calibration and the Optic-Probe Offset calibration.

Calibrations discussed in the TriboIndenter base section of this user manual that are required for the 3D OmniProbe/

MRNP are:

• ADC calibration• Optic-Probe Offset calibration• Probe calibration

This section of the user manual will also discuss the Tare value verification and Indentation Axis calibration which is

required prior to performing any in-contact testing with the 3D OmniProbe/MRNP transducer.

15.1 3D OMNIPROBE/MRNP CALIBRATIONSThe calibrations discussed in this section are specific to the 3D OmniProbe/MRNP. This section is intended as a

supplement to the System Calibrations section presented earlier in the TriboIndenter base section of this user manual.

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! Calibrations in the earlier presented System Calibrations portion of the TriboIndenter base section of this user manual must be completed and/or verified before performing sample testing.

15.1.1 VERIFY THE TRANSDUCER CONSTANTSThe 3D OmniProbe/MultiRange NanoProbe transducer utilizes a third order fit during the calibration. This results in

a more complex set of transducer constants to be entered into the TriboScan software.

When a new 3D OmniProbe/MRNP transducer head is first used, a transducer constants file should be created. A new

transducer constants file can be created from the Calibration tab System Calibrations sub tab (Figure 14.1). To

create a new file, select File Save and create a new file name. All transducer constants files contain indentation

and scratch transducer constants, however, with the MultiRange NanoProbe the X and Y Force Sensor calibration

constants (in the right column of the System Calibration sub tab) should be ignored.

If a transducer constants file has already been created for the 3D OmniProbe/MRNP transducer head, it can simply be

loaded from the Calibration tab System Calibrations sub tab, select File Open.

After a transducer constants file has been loaded or created, the proper constants can be copied from the transducer

constants sheet provided with the 3D OmniProbe/MRNP transducer head.

Figure 14.1 System Calibration sub tab

There are four main areas of the 3D OmniProbe/MRNP transducer System Calibrations tab:

Values entered from transducer constants

sheet

Values in this area are copied directly from the transducer constants sheet or are properties of the transducer/instrument that will not be adjusted during the calibrations. The X and Y Force Sensor column is unused for the MRNP transducer.

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These values are located in the following headings:• Z Force Sensor Calibration• Z Displacement Sensor Calibration• Calibration Tare Values• Maximum Z Displacement• Maximum Z Load• Machine Compliance• Z Head ID• X & Y Force Sensor Calibration (if equipped)• X & Y Stiffness (if equipped)• Maximum X & Y Load (if equipped)

The MultiRange NanoProbe transducer head cannot perform nanoscratch testing.

Values updated by selecting the Update

button

Values in this area are the measured values of the transducer head at rest. The values are generated and updated by clicking the Update button. The values in this area are defined as the Tare values and will need to be verified prior to starting the calibration process.

These values are located in the following headings:• Current Tare Values

Values generated from the calibration

process

Values in this area are calculated and generated with the completion of the Indentation Axis calibration. These values cannot be edited by the user and will only be updated as the Indentation Axis calibration process completes.

These values are located in the following headings:• Z Spring Force Calibration

Values selected and entered by the user

Values in this area are user-defined values and can be updated or changed as desired.

These values are located in the following headings:• Controller ID• Tip ID• Tip Usable Depth• Test Temperature• Scratch Stage ID

The E-Stop Delay Time parameter given on the System Calibrations sub tab is a user-defined parameter that can be

adjusted to help reduce the occurrence of emergency stop errors generated from the sudden acceleration of the Z axis

motor. The default is 10 ms, however, this parameter can be increased as needed to resolve non-contact (false)

emergency stop errors.

The Machine Compliance parameter given on the System Calibrations sub tab is a user-defined parameter that can be

modified as needed. The default Machine Compliance for a TriboIndenter with 3D OmniProbe/MRNP transducer is

about 0.35 nm/mN

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The calculation of the Machine Compliance value for a MRNP transducer is a bit more complicated than solving for

the Machine Compliance of the standard nanoindentation transducer. Because of this, the Machine Compliance

values should only be modified at the direction of a Hysitron service engineer.

15.1.2 TARE VALUE VERIFICATIONThe tare value of the system can be read at any time the nanoindentation probe is not in contact with a sample surface.

Verifying the tare value is approximately the value given on the supplied transducer constants sheet (typically located

within the black transducer case) indicates that the transducer and probe are installed correctly and the connections

are secure.

To read the tare value of the system, click the Calibration tab System Calibrations sub tab and click the Update

button under the Tare Values heading (Figure 14.1). The tare value will be displayed in the parameter box to the right

of the Update button.

The tare value represents the initial offset of each of the sensors inside the 3D OmniProbe/MNRP transducer head. If

the tare value changes dramatically, this would be indicative that something has changed either electronically or

mechanically in the system, and the transducer head may need to be repaired or recalibrated at Hysitron. The Z Force

tare value should be very close to the value on the constants sheet (within about 5%). The Z Displacement tare will

vary more than the Z Force tare value but should still be similar to the value given on the transducer constants sheet

(within about 20%).

The tare values of the system should be verified each time the transducer controller is powered on or any hardware components have been removed, replaced or modified.

If the tare value reading is not in agreement with the transducer constants sheet, reinstall the nanoindentation probe. Many times an incorrect tare value reading is caused by a poorly mounted probe.

Some versions of TriboScan may have a user-defined parameter to enter the tare value. For these versions of TriboScan it is important the user copy the tare value given on the transducer constants sheet into the TriboScan software as this tare value is being used as a reference point.

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15.1.3 3D OMNIPROBE/MRNP INDENTATION AXIS CALIBRATIONThe 3D OmniProbe/MRNP indentation axis calibration should be performed daily, when the transducer cables have

been disconnected/reconnected, or when other environmental conditions have changed.

Before any testing can begin, the spring constant of the load cell spring must first be calibrated. The spring constant

can change based on temperature, humidity or mass of the probe. Because the spring constant can change from day to

day, this calibration should be performed whenever the 3D OmniProbe/MRNP transducer head is removed, replaced

or modified or daily (each day the instrument will be in use) whichever comes first. The Indentation Axis calibration

will perform an indentation test out of contact with any sample and then automatically calculate and generate the Z

Spring Force Calibration values in the System Calibrations sub tab (Figure 14.3). All values from the transducer

constants sheet must be copied into the System Calibrations sub tab prior to running the Indentation Axis calibration.

Access the Indentation Axis calibration by clicking the Calibration tab System Calibrations sub tab Calibrate

button.

After clicking the Calibrate button, TriboScan will automatically open the Load Function tab with a two-segment

displacement-controlled load function with a maximum displacement of 80% the maximum displacement of the

transducer (as entered in the Calibration tab System Calibrations sub tab). On this window, the user must click the

Cal Air Indent button to begin the Indentation Axis calibration process. A real-time plot of the Indentation Axis

calibration will appear while the test is being performed (Figure 14.2).

! The Indentation Axis calibration procedure should only be performed with the probe out of contact with all samples. Performing this calibration while the probe is in contact with a sample is unsafe and will produce an undesirable result.

Figure 14.2 Indentation Axis calibration real-

time plot

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When the test has finished, there will be a brief pause (approximately 30 seconds) as the piezo within the transducer

head resets to the original position. When the piezo has successfully reset, the MRN Air Calibration result window

(Figure 14.3) will be displayed. Within the MRN Air Calibration window there is force vs. displacement plot and a

force residuals vs. displacement plot. The force vs. displacement plot should go from the origin upward at a diagonal

and cover, at minimum, about 75% of the available transducer displacement. The force residuals vs. displacement

plot is summarized by the RMSE (root mean squared error) value given above the plot. The RMSE value is a measure

of the error in the calibrated plot and should be less than 0.001% of the maximum load of the MRNP transducer head.

Because an acceptable RMSE value will scale with the maximum force of the transducer head, the user can expect

values similar to the following list based on the maximum force of the installed transducer head.

• 1 N maximum force: ≤10 μN RMSE• 2 N maximum force: ≤20 μN RMSE• 5 N maximum force: ≤50 μN RMSE• 10 N maximum force: ≤100 μN RMSE


result plot

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15.1.4 NANODMA-HL CALIBRATIONThe 3D OmniProbe/MRNP system can be upgraded to be nanoDMA-HL (high load) which requires software access

to the nanoDMA parameters as well as a modification within the 3D OmniProbe/MRNP transducer. Please contact

Hysitron if you are unsure if your 3D OmniProbe/MRNP is equipped with nanoDMA-HL.

The 3D OmniProbe/MRNP transducer should be calibrated daily (when nanoDMA-HL testing will be performed).

The nanoDMA-HL calibration should be performed following the indentation axis calibration. The button to initiate

the nanoDMA-HL calibration is located on the Calibration tab System Calibrations (High Load) sub

tab Calibrate button (Figure 14.4).

Figure 14.4 Location of nanoDMA-HL

Calibrate button

The software will open the Load Function tab Indentation sub tab and automatically populate the Dynamic

Calibration HL.ldf file. Click the nanoDMA Air Cal button to allow the system to cycle through the available

frequencies and generate the result.

nanoDMA-HL testing and analysis will have similar functionality for test types and range as discussed in the

nanoDMA section of this user manual. A notable difference with the nanoDMA-HL testing is that the maximum

frequency is limited to 200 Hz.

15.2 SAMPLE MOUNTINGWhen working in the higher force regime, as with the 3D OmniProbe/MRNP transducer head, machine compliance,

including sample compliance, becomes a fundamental component. Modulus measurements taken at high forces are

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especially sensitive to errors in the machine or sample compliance. Samples must be rigidly fixed to the stage to

minimize machine compliance effects.

It is important to use rigid adhesives for mounting samples intended for use with the TI series systems. Compliant

adhesives (or double-sided tape) will increase the compliance of the system and result in an erroneous displacement

measurement. Samples attached with cyanoacrylate-based adhesives (suggested adhesive) can be removed with

acetone.

Magnetic mounts may show increased compliance at higher loads. It is suggested to adhere the 3D OmniProbe/

MRNP samples directly to the sample stage or with an alternate screw-down or clip mount.

! Samples must be mounted rigidly to avoid increased machine compliance and erroneous displacement measurements. DO NOT use compliant adhesives or double-sided tape.

When using the TI series systems it is strongly suggested to test samples that are at a similar height (within about

1 mm height difference). If the height between samples varies by more than about 1 mm the samples should be tested

separately and not placed on the stage while the system is at the focus optical focus position or testing a sample.

! Only samples of similar height (within about 1 mm) should be tested at the same time. Samples with large height differences should be tested separately.

15.3 3D OMNIPROBE/MULTIRANGE NANOPROBE TESTINGThe 3D OmniProbe/MultiRange NanoProbe is operated as discussed in the Indentation Testing portion of the base

section of this user manual (nearly identical to standard indentation testing). This portion of the user manual will

discuss only the parameters that are specific to the operation of the 3D OmniProbe/MRNP transducer head.

! The user should be familiar with the Indentation Testing, Analysis, and Automation discussed in the base section of this user manual before proceeding with this section of the user manual.

Testing with the 3D OmniProbe/MRNP transducer head is limited to load and displacement control; there is no open-loop testing with the 3D OmniProbe/MRNP transducer head.

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15.3.1 XY APPROACH OFFSETThe XY Approach Offset parameter allows the user to perform the sample approach in an offset location and perform

the test in the originally focused position (to prevent disturbing the testing location). The XY Approach Offset is

available in all testing modes, however, due to the larger approach forces used with the 3D OmniProbe/MultiRange

NanoProbe transducer head an approach offset from the test location is more important (to prevent surface damage

from affecting the resulting test).

The XY Approach Offset parameters can be found at the bottom of the Preferences tab (in TriboScan 9) and in the

Load Function tab near the Lift Height parameter (in TriboScan 10). When a test is initiated and the XY Approach

Offset is enabled and a value is entered in either the X or Y offset the initial probe approach will be offset by the

defined vale. During the Lift Height the X and/or Y-axis stages will shift so the test is performed at the desired focus

position.

! The user must use care to enter an adequate Lift Height on the Load Function tab so that during the offset the probe does not contact the sample surface (due to tilt or sample roughness) or damage to the sample, probe, or transducer may result.

15.3.2 SYSTEM TEST TABIn the System Test tab (Figure 14.5) there are four parameters given at the bottom of the window that are used during

the sample quick approach and standard sample approach. The four parameters and a description of each are given

below:

Piezo Bias (V) The Piezo Bias is a voltage calculated during the Indentation Axis calibration piezo shake-down procedure (immediately following any indent) that determines the current rest position of the piezo and applies the bias necessary to move the piezo back to the origin position. This parameter should not be modified by the user unless instructed by a Hysitron service engineer. The default value (typically around 0 V) may be modified following every indentation test where the Z-axis piezo is actuated.

Contact Threshold (μN)

The Contact Threshold is analogous to the Imaging Setpoint while using the standard system hardware (base systems). During a quick approach or sample approach, the system will continue to move the Z-axis downward until a force equivalent to the Contact Threshold is achieved. This parameter can be modified by the user and should be increased if the system false engages due to Z-axis motor noise during the approach. The default value is 250 μN but this value will typically scale with maximum load (higher load results in higher noise) of the MRNP transducer.

After the system senses a force equal to the Contact Threshold the Z-axis motor will stop stepping down and the system will extend/retract the MRNP piezo to maintain the Preload (as defined on the Load Function tab). The Contact Threshold is only

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used for the initial Z-axis motor approach; the Preload is the force used to sense surface contact during the Lift Height reseek.

Approach I Gain The Approach I Gain is the integral gain used for the quick approach and standard approach. If there are any oscillations, or if the system has trouble maintaining contact with a sample surface, this parameter should be modified. The default value is 0.5.

Approach Attenuation (%)

The Approach Attenuation is the parameter that defines how far the piezo within the transducer head is attenuated during the approach process. It is ideal to have the piezo nearly fully attenuated while performing the approach, so this parameter should only be modified at the instruction of a Hysitron service engineer. The default value is 99.3%.

Figure 14.5 System Test sub tab

15.3.3 INDENTATION TESTING3D OmniProbe/MultiRange NanoProbe testing is performed identically to the indentation testing procedures

presented in the Indentation Testing portion of the base section of this user manual. Refer to the earlier sections of this

user manual for more information on testing parameters, procedures, or gain tuning.

15.3.4 IN-SITU SPM IMAGINGThe 3D OmniProbe/MultiRange Nanoprobe transducer is not equipped with an X/Y piezo scanner and therefore is

unable to perform in-situ SPM imaging as discussed in the base section of this user manual.

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If the system is configured for dual head operation in-situ imaging can be performed with the standard transducer and

testing can be performed with the 3D OmniProbe/MRNP transducer (set the Transducer Slot toggle switch on the

Action Bar to High Load before performing a standard transducer in-situ SPM image).

15.3.5 AUTOMATED TESTING METHODS3D OmniProbe/MultiRange NanoProbe automated testing methods with the TI series systems and are performed

identically to the automation procedures presented in the Automated Testing Methods portion of the base section of

this user manual. Refer to the earlier sections of this user manual for more information on testing parameters,

procedures, or gain tuning.

Because the 3D OmniProbe/MultiRange NanoProbe transducer head cannot perform an in-situ SPM Image of the sample surface and Piezo Automation testing (as discussed in the base section).

15.3.6 INDENTATION ANALYSIS3D OmniProbe/MultiRange NanoProbe indentation analysis with the system is performed identically to the

indentation analysis presented in the Analysis portion of the base section of this user manual. Refer to the earlier

sections of this user manual for more information on analysis parameters and procedures.

Because of the larger approach noise and contact forces used it may become more necessary to manually zero the

indentation curves for more accurate displacement sensing.

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SECTION | PROBE CLEANING PROCEDURE & SELECTION GUIDE

Probe Cleaning Procedure & Selection Guide

CHAPTER 16 CLEANING HYSITRON PROBES

Cleaning a Hysitron probe is a delicate process. Cleaning the probe should only be performed if there are symptoms

that the probe may be dirty; do not clean the probe merely for the sake of doing it being as irreversible damage can

easily occur. Contact Hysitron if there are questions regarding dirty probe symptoms.

The safest way to clean a Hysitron probe without causing damage is to perform several (10 or more) very deep

indentation tests in a soft material such as a cork or the aluminum (001) standard sample. Many times this is

successful in dislodging any material that had been picked up by the probe during previous testing. After attempting

this method, check to see if the symptoms persist. If the probe still appears to be dirty proceed to the next procedure.

Manually cleaning the probe, as described below, should be performed with care as damage to the probe may easily

occur. This procedure should only be performed if the method described in the preceding paragraph was unsuccessful

and it has been confirmed that the problem is a dirty probe. Contact Hysitron if there are questions regarding dirty

probe symptoms.

To clean the probe manually, use the following procedure:

1. Obtain a cotton swab and some acetone or methanol. In an effort to minimize the possibility of damage to the probe, begin by pulling some cotton off the end of the swab to make a ‘wispy’ or ‘fluffed’ end so as to apply less force to the probe.

2. Remove the probe from the transducer. Attempting to clean the probe when it is installed in a transducer is risky and is more likely to cause damage to the probe and the transducer.

Figure 15.1 Do not attempt to clean the

probe while it is installed in a transducer

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3. After the probe has been removed from the transducer, carefully hold the probe threaded side with the non-dominant hand. With the dominant hand take the cotton swab, which should be soaked with acetone or methanol, and gently wipe from the threaded end to the tip of the probe. DO NOT wipe from the tip of the probe to the threaded end as damage may easily occur when wiping in that direction because cotton could get snagged on the diamond tip.

Figure 15.2 Gently wiping the probe with a

fluffed cotton swab from the base to the tip

4. Rotate the probe 90˚ and repeat so that all sides of the probe have been cleaned.

The probe should now be clean. Install the probe into the transducer and continue testing. If symptoms of a dirty

probe are still present, attempt the cleaning steps again. If the problem persists, contact Hysitron for assistance.

The area function should be verified and possibly recalculated depending on how similar the orientation of the

transducer and probe are with respect to how they were prior to the removal.

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CHAPTER 17 PROBE SELECTION GUIDE

The dynamic range and load capabilities of Hysitron’s family of nanomechanical testing instruments make it an

extremely versatile tool for testing a wide variety of samples. Depending on the application, different probes should

be chosen to maximize the effectiveness of the tool in obtaining repeatable and reliable quantitative data. For this

reason, Hysitron offers an extensive list of different geometries and sizes of probes to accommodate almost any

application. This guide is designed as a tool to help users choose the most appropriate probe for a particular

application.

The indenter geometries offered by Hysitron are generally split into three separate categories:

• 3-Sided Pyramidal probes• Cono-spherical probes• Specialty probes

Probes in all three categories can be used with most of the options available, however, the selection for a particular

option may be limited. Contact Hysitron to find out which probes are available for a particular option.

The two major applications that separate the use of probes are nanoindentation and nanoscratch. Most probes can be

used for either applications, but it is always best to use separate probes for indentation and scratch tests. Scratch

testing can blunt the probe quickly, which may change the probe area calibration that is used for quantitative

indentation.

17.1 BERKOVICH PROBESThe Berkovich probe (Figure 16.1) is the standard nanoindentation probe. It has a total included angle, the angle from

one edge to the opposite side, of 142.35°. The half-angle, or the angle from the perpendicular to one face (θ), is

65.35°. The aspect ratio of the probe is 1:8. A typical radius of curvature for a standard Berkovich probe would be

approximately 150 nm. Sharper Berkovich probes with a radius of less than 50 nm are available.

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Figure 16.1 3-Sided pyramidal probe

Because the Berkovich probe is the standard probe for nanoindentation, it should be used whenever possible. The

well-accepted models for nanoindentation use this geometry because the Berkovich probe has the same depth to area

ratio as a Vickers. This probe is the best probe for most bulk samples, unless the roughness is more than

approximately 50 nm RMS. It also works well for thin films greater than approximately 200 nm in thickness. For

thinner films, the sharper Berkovich probe with radius less than 50 nm should be used.

Berkovich probes will generally provide good SPM images. Berkovich probes are not so sharp that they will dull very

little on materials with modulus greater than 1 GPa. If softer samples are used, Berkovich probes may not image them

well.

Ideal probe area function for a Berkovich probe:

• C0 = 24.5• C1-C5 = fitted parameters

Typical indentation applications for Berkovich probes:

• Bulk Ceramics and Glasses• Bulk Metals and Steels• Thin, Hard Films and Coatings Greater than 100nm Thick• Hard, Smooth Biomaterials (Polished Bone and Tooth Samples)• Hard Polymers (Modulus Greater than 1GPa)

Typical scratch and wear applications for Berkovich probes:

• Scratch resistance of thin coatings (less than 100 nm)• Adhesion of thin coatings (less than 100 nm)• Scratch applications where imaging is important

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17.2 90 DEGREE PROBES (CUBE CORNER)The 90 degree (cube corner) nanoindentation probes are similar to the Berkovich probes in that they are also 3-sided

pyramidal probes (Figure 16.1). The total included angle of the cube corner probes is 90°. The half-angle, or the angle

from the perpendicular to one face (angle θ), is 35.26°, which gives the cube corner probe an aspect ratio of 1:1.

Because the aspect ratio is higher, it is much simpler to make the radius of curvature smaller. Typical radii of

curvature measurements for these probes are around 150 nm. North Star™ cube corner probes have the same

geometry as standard cube corner probes, but the radius will be less than 40 nm.

The primary advantage that the cube corner probe has over other probes is the sharpness. The radius of curvature can

be less than 40 nm. This allows smaller indentations to be performed, while still creating plastic deformation.

Because of this, smaller indentations can be made, and an accurate hardness can still be measured. The small

indentation impression for a given depth also allows smaller features on a sample or composite material to be

measured.

Because the aspect ratio is higher, the cube corner probe can image rougher samples than a Berkovich probe. If in-situ

imaging is used, the data using a cube corner probe can also be more repeatable than that from a Berkovich probe,

because the sharper probe may be able to better indent between the peaks and valleys of rough samples.

Ideal probe area function for a cube corner probe:

• C0 = 2.598• C1-C5 = fitted parameters

Typical indentation applications for cube corner probes:

• Ultra-thin coatings less than 100 nm thick• Micro/nano-composites• Fracture of samples• Micro/nano structured materials

Typical scratch applications for cube corner probes:

• Ultra-thin coatings less than 20 nm thick• Applications where high-resolution imaging is required

17.3 CONO-SPHERICAL PROBESCono-spherical probes are cone shaped nanoindentation probes with spherical ends. The available cone angles are

60°, 90°, and 120°. With all but the sharpest probes on soft materials, only the spherical end of the probe will be in

contact with the sample, so the cone angle is generally not as important.

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Most of the cono-spherical probes are made from diamond. Diamond is very difficult to grind in a spherical shape, so

the smallest probe radii are limited to about 0.5 µm. This radius can be increased up to about 100 µm. Probes larger

than this are actual spherical probes, not conical at the top, and are made from sapphire or other materials.

Cono-spherical probes are generally separated into two categories: imaging and non-imaging. Probes with radii larger

than 10 µm are too blunt to create useful in-situ SPM images. Probes sharper than 10 µm can generate usable in-situ

SPM images on smooth samples.

17.3.1 IMAGING CONO-SPHERICAL (RADII < 10 µM)The cono-spherical probes with radii of less than 10 µm are typically used in applications where imaging is required.

The imaging resolution of these probes are not as high as with pyramidal probes, but are sufficient for pre-placement

and post imaging analysis. These probes are sharp enough that they can create plastic indentation marks on samples

as hard as fused quartz with the standard 10 mN transducer.

Figure 16.2 Cono-spherical nanoindentation

probe

The sharper cono-spherical probes can be used to indent on polymer samples. They work best when the modulus of

the sample is greater than 0.5 GPa. If the samples are softer than this, then the probes may penetrate too far into the

surface even before a very low force of 1 µN is detected.

Typical indentation applications for imaging cono-spherical probes:

• Harder polymers (modulus greater than 0.5 GPa) • Hard biomaterials

Typical scratch and wear applications for imaging cono-spherical probes:

• Polymers with modulus greater than 0.5 GPa• Hard and soft coatings greater than 50 nm thick • Hard biomaterials• Measuring coefficient of friction

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17.3.2 NON-IMAGING CONO-SPHERICAL PROBES (RADII > 10 µM)The radii of curvature of these probes are too large to generate useful images when scanning. So these probes should

only be used on materials where nanoscale positioning is not important, such as on homogenous, flat materials. These

probes are ideal for very soft materials such as rubbery polymers or soft biomaterials. The indentation area of these

probes is much larger at small depths than any of the other probes, so smaller indentation depths can be achieved with

these probes on soft materials.

These probes will not typically cause plastic deformation on most materials, so they are also ideal for testing small

structures to find stiffness qualities.

Ideal probe area function for a cono-spherical probe:

• C0 = -π or -3.14• C1 = 2 × π × R or 6.28 × R, where R is the radii of the probe in nanometers• C2-C5 = fitted parameters

Typical indentation applications for non-imaging cono-spherical probes:

• Soft polymers (modulus less than 0.5 GPa) • Soft biomaterials (tissue, skin, contact lenses, fluid cells)• Structured samples (nano-springs, posts, cantilevers)• MEMS/NEMS

Typical scratch applications for non-imaging cono-spherical probes:

• Soft polymers (modulus less than 0.5 GPa) • Soft biomaterials (tissue, skin, contact lenses, fluid cell)• Coefficient of friction

17.4 SPECIALTY PROBESSpecialty probes include any probes that are not in the above two categories. These probes are typically reserved for

specialty or custom applications.

17.4.1 VICKERS PROBESThe Vickers probe is a four-sided pyramidal probe. The depth to area ratio and area function is the same as a

Berkovich probe. When four planes are cut into the diamond to create the probe, they will intersect in a line rather

than a point, so the radius of curvature is typically much larger than a Berkovich probe, typically greater than 500 nm.

This limits how much work can be performed with the standard 10 mN transducer, so Vickers probes are more

limited to use with the higher force options. The main purpose of the Vickers probe is to find scale connectivity

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between the nanoindentation and microindentation regimes. Vickers indentation is typically performed with a

microindenter with the size of the indent measured optically. At nanoscale, depth sensing indentation is used, so this

probe is not as useful for low-load quantitative studies.

17.4.2 KNOOP PROBESThe Knoop probe is a four-sided pyramidal probe. The cross sectional of the probe is rhomboidal, so that one axis is

much more elongated than the other. This probe was developed for microindentation. Smaller indents with a Knoop

probe are too small to image optically. The rhomboidal shape of the Knoop probe makes it possible to measure the

length of the longer axis to calculate the area of the indentation impression optically. Because it is four sided, the

probe radius is often much larger than three sided pyramidal probes, limiting this probe to higher load applications.

One area where this probe has been used for nanoindentation is for samples that have a directional dependence. The

Knoop probe can be oriented along the direction of grains or other structure in the sample to investigate these

properties.

17.4.3 FLAT ENDED PROBESTwo different types of flat ended probes are available. The first is a flat punch, which is a cylindrical shaped probe

with a flat end. The second is a 60 degree cone with a flat end. The flat ended probes are typically only used with very

soft samples, as it is very difficult to get the probe perfectly parallel to the sample. With soft samples, it is possible to

load the probe enough to get the full contact area. Flat ended probes can also be used to test structure materials, such

as nano-dots or pedestal samples to find the stiffness.

17.4.4 WEDGE PROBESA few different geometries of wedge probes are available. The smaller wedge probes are used when there is a

directional dependence in a sample, or for testing specific geometries of samples. One example is for performing

bend tests on a suspended wire or beam. Wedge probes are sometimes used to cause delamination by indenting

directly at the interface between a substrate and thin film. The radius of the end of the probe is about 1 µm, which

limits the types of systems that can be tested in this manner.

17.4.5 FLUID CELL PROBESMost probe geometries discussed in this appendix are available in a fluid cell configuration. The fluid cell probes

have an extended shaft, approximately 4 mm in length, which allows the end of the probe to be completely immersed

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in a fluid, while the probe holder and transducer remain in the air. The diameter of the extended shaft is about 700 µm

to minimize and meniscus forces that will be present where the probe penetrates the fluid. Fluid cell probes are used

for any applications that require the sample to be immersed in fluid. This would include many biomaterials

applications, electrochemical experiments, and Chemical Mechanical Planarization, experiments.

17.4.6 TEMPERATURE CONTROL STAGE PROBESMost probe geometries discussed in this appendix are available in a temperature control stage configuration. The

temperature control stage probes are mounted in a slightly longer, ceramic holder assembly with a heat-resistant

epoxy. The use of these materials limit the amount of heat transfer to the transducer and allow the temperature control

stage to be used at higher temperatures.

17.4.7 NANOECR PROBESThe nanoECR probes are constructed to be used with the nanoECR (Electrical Contact Resistance) upgrade. The

nanoECR probes are constructed using a boron doped diamond and a low-resistance conductive path through the

probe holder into the transducer so that the electrical signals from the sample stage can be transmitted.

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LIST OF FIGURES AND TABLES

TI 980 TriboIndenter system automated stage specifications .......................................................11TI 980 TriboIndenter magnetic sample stage .................................................................................12TI 980 TriboIndenter granite frame ................................................................................................13TI 980 TriboIndenter acoustic enclosure ........................................................................................14TI 980 TriboIndenter USB 3.0 optical camera system ....................................................................15TI 980 TriboIndenter IEEE 1394 CCD camera zoom specifications .................................................16Active vibration isolation control unit (left) and vibration isolation units (right) ..........................17Specifications of the active vibration isolation system ..................................................................17Transmissibility plot for Herzan AVI-200 S/LP active vibration isolation system ...........................18TriboScanner ..................................................................................................................................19TriboScanner piezo ceramic tube construction ..............................................................................20Ideal behavior, hysteresis, and creep of piezo electric material ....................................................21Specifications of the TriboScanner .................................................................................................21Installation of the TriboScanner on a TI 980 TriboIndenter ...........................................................22Standard 1D and 2D transducer assemblies ...................................................................................23Cross sectional schematic of standard (1D) transducer assembly .................................................24Transducer displacement measurement diagram .........................................................................25Transducer force measurement diagram .......................................................................................25Specifications of the Transducer Assembly ....................................................................................26Location of 0.035” hex screw .........................................................................................................27Transducer ready for probe installation .........................................................................................27Removing the nanoindentation protective sheath ........................................................................28Probe installation tool with probe .................................................................................................28Probe tool and probe geometry .....................................................................................................28Installation of nanoindentation probe ...........................................................................................29Removing the probe tool from the installed nanoindentation probe ............................................30Example probe calibration sheet ....................................................................................................31Location of 0.035” hex screw .........................................................................................................31Hysitron performech II back panel .................................................................................................32Hysitron control unit specifications ................................................................................................35performech II TI 980 TriboIndenter connection diagram ...............................................................36performech II dual low load option connection .............................................................................37Computer requirements for TI 980 TriboIndenter systems ...........................................................38TriboScan Action Bar ......................................................................................................................42System Progress Panel ...................................................................................................................44Sample Navigation tab ...................................................................................................................48Move pad with color enhancement to illustrate stage speeds ......................................................50Nanoindentation Probe Position ....................................................................................................51Stage positions area .......................................................................................................................52Sample Boundaries parameters .....................................................................................................53Indentation sub tab ........................................................................................................................55Standard Load Function menu .......................................................................................................56User Mode menu ............................................................................................................................56Automatic Save menu ....................................................................................................................57Control Feedback pull-down menu ................................................................................................58Control Feedback parameters ........................................................................................................59Illustration of PID gain operation ...................................................................................................60Constant strain rate load function editor .......................................................................................63Partial unload load function editor ................................................................................................65XPM sub tab ...................................................................................................................................67

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Standard Load Function menu .......................................................................................................69User Mode menu ............................................................................................................................70Automatic Save menu ....................................................................................................................70Scratch sub tab ...............................................................................................................................72ScanningWear sub tab ....................................................................................................................76 Quasi sub tab .................................................................................................................................80File Calibration Constants window (accessed from the Edit button) .............................................81Displacement offset of load control test ........................................................................................85Graphical representation of plotted values ...................................................................................86Multiple curve plot .........................................................................................................................88Hardness and Reduced Modulus versus Contact Depth Plot .........................................................89XPM sub tab ...................................................................................................................................90Nanoscratch File Constants window ..............................................................................................93Axis Settings window ......................................................................................................................95in-situ sub tab .................................................................................................................................97in-situ sub tab Button and Menu Bar .............................................................................................98Consecutive image capture window ..............................................................................................99in-situ image Capture Images window ...........................................................................................99Captured *.hdf file suffixes ..........................................................................................................100Channel Selection window ...........................................................................................................101Background Subtraction window .................................................................................................101Scan Settings area of the in-situ sub tab ......................................................................................105Position Controls area of the in-situ sub tab ................................................................................107in-situ image with reticule ............................................................................................................108Scan Line/Histogram are of the in-situ sub tab ............................................................................108Location of histogram functions ...................................................................................................109Automation tab ............................................................................................................................110Method Operation/Data Storage area .........................................................................................112Edit Method window ....................................................................................................................112Pattern Selection area ..................................................................................................................112Pattern Editor window .................................................................................................................113Target Positions area ....................................................................................................................113Methods, Groups, Positions and Patterns representation ...........................................................114Load Function Configuration area ................................................................................................115Load Function Setup window .......................................................................................................115Delay Control window ..................................................................................................................116Imaging Setup window .................................................................................................................116in-situ Imaging/Method Chaining area .........................................................................................117Position side tab ...........................................................................................................................118Script Mode pull-down menu .......................................................................................................119Array Script piezo automation ......................................................................................................120Constant direction and serpentine translation protocols ............................................................120Click Script piezo automation .......................................................................................................121Select directory for piezo automation data .................................................................................122Select base file name for piezo automation data .........................................................................122Set beginning and ending forces for piezo automation tests .......................................................122System Calibrations sub tab with color-coded parameters .........................................................125Stage Calibration sub tab .............................................................................................................129Set Speeds window ......................................................................................................................130Define sub tab ..............................................................................................................................132Machine Compliance sub tab .......................................................................................................134in-situ sub tab ...............................................................................................................................134Auto Cal sub tab ...........................................................................................................................135Table sub tab default parameters ................................................................................................138

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Piezo sub tab default parameters ................................................................................................139Hysitron customer support center website ..................................................................................140Example transducer constants sheet ...........................................................................................143Location of Update button and verification of tare value ............................................................144DSP Calibration Result window ....................................................................................................145Installed data acquisition cards by instrument configuration ......................................................146Verification of indentation axis transducer constants .................................................................147Indentation Axis calibration load function ...................................................................................148Indentation Axis calibration reminder window ............................................................................148Real-time indentation plot for the Indentation Axis calibration ..................................................149Indentation Axis calibration confirmation window ......................................................................149Indentation Axis calibration ESF vs. displacement plot ................................................................150Indentation Axis calibration result ...............................................................................................151Lateral Axis calibration result .......................................................................................................152Performing an Optical Zoom calibration ......................................................................................156ATOCW patterned wafer sample .................................................................................................158Optical images of ATOCW patterned wafer .................................................................................159Enable the Approach Auto E-Stop Recover feature .....................................................................160Initiating the ATOCW ....................................................................................................................160ATOCW center on image 1 ...........................................................................................................161ATOCW center on image 2 ...........................................................................................................161ATOCW real-time plot ..................................................................................................................162Optic-Probe Tip Offset calibration options ...................................................................................163Z Safety Disabled prompt .............................................................................................................164Enter force for calibration indents prompt ..................................................................................164Lower the Z-axis prompt ..............................................................................................................165H pattern on aluminum standard .................................................................................................165Locate the H pattern prompt .......................................................................................................166Auto Search button ......................................................................................................................166Auto Search prompt .....................................................................................................................166H pattern with eight indent to identify pattern as used ..............................................................167Calibration grating scanned with an uncalibrated (left) and calibrated scanner (right) ..............168Modified Imaging tab with Scanner Calibration area ...................................................................169Measuring the X/Y axis grating .....................................................................................................169Schematic of nanoindentation .....................................................................................................172Load Function Setup window for probe area function procedure ...............................................175Multiple curve plot of calibration indents ....................................................................................175Calculate sub tab ..........................................................................................................................177Standard samples reference table ...............................................................................................177Standard probes reference table .................................................................................................177Probe radius effects with shallow indentation .............................................................................178Hardness and reduced modulus plot for a probe with radius of around 120 nm ........................180Machine Compliance sub tab .......................................................................................................183Machine compliance load range selection ...................................................................................184Auto Calibration sub tab ...............................................................................................................185Automated calibrations flow chart ...............................................................................................186Auto calibration initiation options ...............................................................................................186Auto Calibration sub section ........................................................................................................187Transducer Calibration sub section ..............................................................................................189 Tip Check section .........................................................................................................................190Tip Calibration section ..................................................................................................................191Plot Multiple Curves window .......................................................................................................193 Hysitron standard system testing modes ....................................................................................196Placement of samples with height differences ............................................................................198

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Sample boundary creation procedure ..........................................................................................199Disable X, Y and Z Safety Disabled radio buttons .........................................................................199New Sample button location ........................................................................................................200Rename Sample prompt ...............................................................................................................200Sample Boundaries pull-down menu ...........................................................................................200Pos. Add button to add first point ................................................................................................201Pos. Add button to add additional sample points ........................................................................201Completed sample boundary .......................................................................................................201Enable X, Y and Z Safety Disabled radio buttons ..........................................................................201Location of Quick Approach button .............................................................................................203Move optics over a defined sample space ...................................................................................205Select test Mode ...........................................................................................................................205Click the Perform Indent button to start an indentation test from the optical focus position ....206Single Indent window ...................................................................................................................206Progress window ..........................................................................................................................206Drift Monitor window ...................................................................................................................207Real Time Plot window .................................................................................................................207Save As window ............................................................................................................................208Default gain settings .....................................................................................................................208Feedback control gain suggestions ...............................................................................................210PID Tuning window .......................................................................................................................211XPM test performed too fast ........................................................................................................213Approach button ..........................................................................................................................214Go button .....................................................................................................................................214Withdraw button ..........................................................................................................................215Measuring roughness within TriboView .......................................................................................216Calculating wear volume with TriboView .....................................................................................217Test button ...................................................................................................................................218Mode pull-down menu .................................................................................................................219Piezo Automation sub tab ............................................................................................................220Script Mode pull-down menu .......................................................................................................220Array Script options ......................................................................................................................220Click Script options .......................................................................................................................221Piezo automation testing options ................................................................................................221Selecting directory for saving piezo automation data ..................................................................222Selecting base file name for piezo automation data ....................................................................222Piezo automation load adjustment parameters ...........................................................................222Pattern Selection area ..................................................................................................................224Target Positions area ....................................................................................................................224Load Function button ...................................................................................................................225Load Function Setup window .......................................................................................................225Combi utility text file ....................................................................................................................227Combi circular wafer setup ..........................................................................................................227Combi Panel ..................................................................................................................................228Wafer Details Panel ......................................................................................................................229Calculate wafer angle & sample shape ........................................................................................230Nanoindentation curve displayed in Quasi sub tab ......................................................................233Verifying lift segment and correct origin of curve ........................................................................233Identifying dirty sample, probe, or poorly mounted sample .......................................................234Incorrectly measured or excessive drift rates ..............................................................................234Hold time is not adequate for sample creep ................................................................................235Dislocations or fractures in loading curve ....................................................................................235Nanoindentation fitting parameters ............................................................................................236Update graph after each fit prompt .............................................................................................237

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Select segments to analyze prompt .............................................................................................238Quasi sub tab result after loading XPM test .................................................................................239XPM Analysis Parameters window ...............................................................................................239XPM test result .............................................................................................................................240Scratch Data analysis tab ..............................................................................................................241Tilt correction process ..................................................................................................................242Location of Friction button ...........................................................................................................243Coefficient of Friction vs. Time plot .............................................................................................243Segment Plotted pull-down menu ...............................................................................................243Coefficient of Friction vs. Time plot of scratch segment only ......................................................244Select Image Directory window ....................................................................................................245Image Browser ..............................................................................................................................246Information available by hovering the mouse over an image thumbnail ....................................246Image window ..............................................................................................................................247Section tab ....................................................................................................................................247Histogram tab ...............................................................................................................................248Background Subtraction tab .........................................................................................................248Background subtraction routines available from TriboView ........................................................249Info tab .........................................................................................................................................2503D Plot window ............................................................................................................................252High Resolution Image check-box location ..................................................................................2523D Properties Control tab .............................................................................................................2533D Properties 3D tab ....................................................................................................................2543D Properties Axis tab ..................................................................................................................2553D Properties Lighting tab ............................................................................................................2553D Properties Plots tab .................................................................................................................256Parallel plate DMA testing ............................................................................................................259Uni-axial DMA testing ...................................................................................................................260Kelvin model for polymeric systems .............................................................................................260nanoDMA connection diagram ....................................................................................................262Location of amplifier settings .......................................................................................................263Values for lock-in amplifier settings .............................................................................................264System Calibrations sub tab .........................................................................................................265Lock-in Amplifier calibration results window ...............................................................................268Dynamic calibration button ..........................................................................................................269Dynamic calibration load function ...............................................................................................269Satisfactory Dynamic calibration result ........................................................................................270Standard Load Function menu .....................................................................................................272User Mode menu ..........................................................................................................................272nanoDMA side tab ........................................................................................................................273Representation of Variable Dynamic Load and Constant Quasi/Dynamic Ratio scaling ..............273Graphical representation of Constant Dynamic Load scaling ......................................................274Dynamic Load Scaling options ......................................................................................................274Time Constants window ...............................................................................................................275 Lock-In Sensitivity settings ..........................................................................................................277Dynamic Sweep Generator window .............................................................................................278Force vs. time plot for variable frequency test ............................................................................281Dynamic Sweep Generator window .............................................................................................281Variable Frequency test result .....................................................................................................282Constant Strain Rate CMX test .....................................................................................................284CMX test result .............................................................................................................................285Using a nanoDMA III data file for a probe area function ..............................................................286Reference Creep test ....................................................................................................................287Reference Creep test result ..........................................................................................................287

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nanoDMA sub tab .........................................................................................................................289Data Selection tab ........................................................................................................................292Data Point Values tab ...................................................................................................................293Multiple Files tab ..........................................................................................................................294Dynamic signals ............................................................................................................................295nanoDMA III data analysis (nanoDMA sub tab) ............................................................................2983D modulus map of ceramic fiber within a matrix rendered in TriboAnalysis .............................300Lock-in control icon ......................................................................................................................300Modulus Mapping Setup window ................................................................................................301Modulus mapping low pass filter response ..................................................................................303Modulus mapping imaging tab options ........................................................................................304Amplitude scan line during modulus map ....................................................................................305Standard lock-in control window values ......................................................................................305Deep and shallow indentation test showing different probe radius determination ...................307Using TriboScan to measure the displacement at a given force ..................................................308xProbe transducer connection .....................................................................................................311xProbe transducer details .............................................................................................................312 xProbe transducer specifications ................................................................................................312xProbe selection ...........................................................................................................................313xProbe transducer slot .................................................................................................................313Connection Schematic for 3D OmniProbe/MRNP ........................................................................320The torsion guard .........................................................................................................................321Installing the probe onto a MNRP transducer head .....................................................................3233D OmniProbe/MRNP transducer head attached to a TriboIndenter .........................................324System Calibration sub tab ...........................................................................................................325Indentation Axis calibration real-time plot ..................................................................................328Indentation Axis calibration result plot ........................................................................................329Location of nanoDMA-HL Calibrate button ..................................................................................330System Test sub tab ......................................................................................................................333Do not attempt to clean the probe while it is installed in a transducer ......................................338Gently wiping the probe with a fluffed cotton swab from the base to the tip ............................3393-Sided pyramidal probe ..............................................................................................................341Cono-spherical nanoindentation probe .......................................................................................343

352 of 353 Revision 10.0.1216

353 of 353 Revision 10.0.1216


TI 980 TriboIndenter User Manual

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