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High temperature nanoindentation up to 810°C:
Experimental Optimization
N. X. Randall, M. Conte, B. Bellaton, Jarod Zhao
Anton Paar TriTec SA, Rue de la Gare 4, Peseux CH2034, Switzerland
[email protected]
G. Mohanty, J. Schwiedrzik, J. M. Wheeler, J. Michler
EMPA, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for Mechanics of
Materials and Nanostructures, Feuerwerkerstrasse 39, Thun CH3602, Switzerland
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1 • Background to High Temperature Indentation Testing
2 • Current Challenges
3 • How does UNHT3 HTV address such challenges?
4 • Basic system overview
5 • Validation of specifications over entire temp. range
6 • Application examples
7 • Conclusions
Summary
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Background to high temperature testing
Industrial applications are:
▸ Cutting tools hard coatings for high speed machining;
▸ Semiconductors;
▸ Thermal barrier coatings;
▸ Nuclear materials
Academic applications are:
▸ Investigation on dislocation induced by high temperature and deformation;
▸ Creep and fatigue changes with temperature;
▸ Hardness variation with temperature;
▸ Etc.
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Current challenges to high temperature indentation
Sample and tip oxidation
J. M. Wheeler and J. Michler, Review of
Scientific Instruments 84, 101301 (2013)
Tip Hardness decay
Diamond tip
after contact with
steel sample at
500 °C
J. M. Wheeler and J. Michler, Review of
Scientific Instruments 84, 101301 (2013)
Sample and tip interaction
Courtesy of UTC, France
Tip contamination
High Vacuum or Inert gas
environment
Tip material opportune choice depending on the
sample material
Tip cleaning process
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UNHT3 HTV High Vacuum System Features
• Ultimate Vacuum: 10-7 mbar
• Process Vacuum: 10-6 mbar
• Vacuum chamber Volume: 100 liters
• Pumping speed: 800 l/s
• Primary pump is rotary vane
• Secondary pump is turbo molecular
with magnetic levitation bearings
• Partial pressure mixture gas control:
10-900 mbar
• Flow gas mixture control rate: 0-2000
sccm
• User available additional ports
• Integrated compressed air-pistons
Vacuum
Buffer
P1
P2
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UNHT3 HTV High Vacuum System Features
Active air pads
Damped frame
Integrated
electronics
High Vacuum enclosure
Ultimate vacuum 2x10-7 mbar
Water cooling
circuit
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Some pictures
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UNHT3 HTV Adjustable sample holder
Cement vs clamping
Patent pending PCT/EP2017/051035
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Stage
sample
A1
I
A2
R Reference contact
A1 & A2: piezoelectric actuators
Motorized Z table
Feedback loop for accurate low force
sensing
Feedback loop on force sensor FN
Dz
Load-depth curve
UNHT3 HTV Head Design
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UNHT3 HTV Head Features
Infra Red Heaters (x2)
Water Cooled Jacket Reflective Mirror
Long Shaft Indenter
& Reference
Pending Patent EP14191443.2: UNHT3 HT Tip heating design
Pending Patent EP14191442.4: UNHT3 HT Design of heated probe
Vacuum Compatible Piezos
Zerodur frame ensures negligible thermal
expansion (0 – 100°C)
Cu-Be Springs, range 0 – 100 mN
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Indentation/reference tips
Tip
heating
system
Sample heating
module Sample
A comprehensive approach is needed: the problem is not only the heating up but also controlling the
temperature and keeping it stable for a long time. The whole system must be considered.
UNHT3 HTV Heating System Features: IR Bath
Pending Patent EP16151845.1: UNHT3 HT Sample holder arrangement
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UNHT3 HTV Temperature Management
Reference
Thermocouple
Sample
Thermocouple *
Sample Holder
Thermocouple
[Security]
Indenter
Thermocouple
UNHT3 HT Head
Thermocouple
[Security for head < 40°C]
Sample Heater
Power
* Two thermocouples are available:
(1) Under sample holder
(2) On sample surface
User can choose which of the 2
thermocouples to use for regulation
Indenter, Reference and Sample temperatures can be regulated independently in 3 ways:
(1) Power regulation (e.g., constant wattage control, user definable)
(2) Target temperature (via PID control, user definable)
(3) Slope or heating ratio (°/min, user definable)
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UNHT3 HTV Temperature Management
Z0
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High Purity Molybdenum (Raw Data)
Thermal drift measurements
(raw data) on pure
Molybdenum at 810°C
showing < 2 nm/min. average
drift rate over a 300 s pause at
10% of maximum applied load.
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High Purity Molybdenum (Raw Data)
23°C 810°C
23°C
810°C
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Titanium Nitride (TiN) on WC substrate
TiN thickness: 3 µm
Maximum load: 30 mN, holding time 10 sec
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Titanium Nitride (TiN) on WC substrate (Raw Data)
TiN thickness: 3 µm
Maximum load: 30 mN, holding time 10 sec
RT 200C 400C 600C
Hardness (GPa): 27.3 21.4 18.3 7.6
Elastic Modulus (GPa): 397 321 289 183
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Alumina (Al2O3) on WC substrate
Al2O3 thickness: 10 µm
Maximum depth: 400 nm, holding time 10 sec
Loading/Unloading speed: 150 nm/min
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THANK YOU