1 2ND INTERNATIONAL CONFERENCE AND EXPO ON CERAMICS AND COMPOSITE MATERIALS SHERATON BERLIN GRAND HOTEL ESPLANADE, 10785 BERLIN, GERMANY NEW X-RAY DEVELOPMENTS TO CHARACTERIZE CERAMIC MATERIALS A. DOMMANN*, O. KUZIOR, A. FLISCH, S. HARTMANN, R. KAUFMANN AND A. NEELS , EMPA, SWISS FEDERAL LABORATORIES FOR MATERIALS SCIENCE AND TECHNOLOGY, CENTER FOR X-RAY ANALYTICS, SWITZERLAND Materials Materials Processing Analytics Simulations Multi-layer and system fabrication Materials behavior by in-situ studies Model simulations of joining processes Interfacial design of nano- structured materials Accelerate progress by sharing know how 2
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2ND INTERNATIONAL CONFERENCE AND EXPO ON CERAMICS AND COMPOSITE MAT ERIALS
SHERATON BERLIN GRAND HOTEL ESPLANADE, 10785 BERLIN, GERMANY
NEW X-RAY DEVELOPMENTS TO CHARACTERIZE CERAMIC MATERIALS
A. DOMMANN*, O. KUZIOR, A. FLISCH, S. HARTMANN, R. KAUFMANN AND A. NEELS ,EMPA, SWISS FEDERAL LABORATORIES FOR MATERIALS SCIENCE AND TECHNOLOG Y, CENTER FOR X-RAY ANALYTICS, SWITZERLAND
MaterialsMaterials
Processing
AnalyticsSimulations
Multi-layer and system
fabrication
Materials behavior
by in-situ studies
Model simulations of
joining processes
Interfacial design of nano-
structured materials
Accelerate progress by sharing know how
2
2
TEM/STEM HRSEMHe-SEM
FIB
ToF-SIMS
AFM
7.5 x 7.5 mm2
3D NanoChemiscope
Surface Analytics
HRXRD
X-ray Analytics: Methods & Tools
X-RAYSAbsorption
XRDHRXRD
SAXS
XPCI
Imaging: 2D, 3D
X-ray tool & methods optimisationfor materials & system studies
Oxidation behaviour of TiCN / AlCrO at 900°C (air, 30 min)
H2 = 32 nm
Thermal stability
6
Support in process development:
Hard coatings
Dedicated Design of High Temperature Corrosion Resistant PVD Oxide Coatings for Automotive Applications
Simulations Characterization:
XRD, ex- and in-situ
RBS
Mechanics
Testing
Understanding
Reactive cathodic arc evaporation (PVD)
11
High Temperature Corrosion Resistant Al-Cr-O Coatings Deposited by Arc Operation
12
7
Crystal Structure Consistency with Vegard’s law
Cr / Al ratio
4.70
4.75
4.80
4.85
4.90
4.95
5.00
0.0 0.5 1.0 1.5 2.0
13.00
13.10
13.20
13.30
13.40
13.50
13.60
13.70
13.80
4.70
4.75
4.80
4.85
4.90
4.95
5.00
0.0 0.5 1.0 1.5 2.0
13.00
13.10
13.20
13.30
13.40
13.50
13.60
13.70
13.80Measured values
(Al0.85Cr0.15)2O3(Al0.85Cr0.15)2O3
(Al0.7Cr0.3)2O3(Al0.7Cr0.3)2O3
(Al0.5Cr0.5)2O3(Al0.5Cr0.5)2O3
(Al0.25Cr0.75)2O3(Al0.25Cr0.75)2O3
latt
ice
para
mete
r a
[Å]
latt
ice
para
mete
r c
[Å]
13
Cathode surface vs layer composition
Cathodes
• Phase transformation process at the cathode surface?• How this influences the deposited layer?
Layers
A. Neels, X. Maeder, A. Dommann, J. Ramm 14
8
Al-Cr system:
XRD High temperature experiment
XRD Chamber at 1300°C
• Phase transformation at high temperature
• Progressive oxidation study• Stability of the coating
A. Neels, X. Maeder, A. Dommann, J. Ramm 15
Wear resistant hard coatings
Oerlikon developed a complete new deposition method:
Reactive Cathodic Arc Deposition
Need: fundamental understanding of this new deposition process
Approach: Combination of characterization, simulation and testing
Cathodic arcprocess Deposition
O2
Intermetallics + OxidesPure Al and pure Hf
O2 O2
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Post-hot isostatic pressing
Thin film multilayers: PZT
Piezoelectric materials for switches
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PZT layers by sol-gel deposition.
10
J. Am. Ceram. Soc., 97, 2069–2075 (2014)
3D schematic view
The five-layer lead zirconate titanate device after patterning the three topmost electrodes:
2D schematic of the cross section
PZT multilayer systems
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Platinum
Lead Zirconium Titanium Oxide
Pt(
111)
Pt(
002)
PZ
T(0
11)
PZ
T(1
11)
PZ
T(0
01)
PZ
T(1
12)
Pt(
220)
PZ
T(0
02)
PZ
T(0
12)
Phase analysis
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11
PZT layers trough sputtering: Pole figures show the PZT fiber texture, the preferred orientation direction is (001). Much higher texturing compared to the sol-gel deposition process.
Texture analysis: PZT pole figures
001 011 111
002 012 112
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Only small loss in texture. Quantification trough texture index.
support tool for layer deposition process optimization
System understanding and layer design
HRXRD For oxide materials and devices
Addressing in-plane diffraction for accessing directly in-planestructural parameters: strain, mosaicity
X-Ray Tomography For 3D information of oxide materials and devices
High sensitivity of the dark-field mode to small voids.
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Curiosity, Flexibility, Communication
Röntgenhaus
Antonia Neels, Rolf Kaufmann, Tanja Kramer, Thomas Lüthi, Alex Flisch, Felix Reifler, Olga Kuzior, Gelu Rotary, Mathieu Plamondon, Mario Beltran, Kai Zweiacker, Michele Griffa, Yu Liu, Carina Stritt, Fei Yang, Jürgen Hofmann,
Alex Dommann, Stefan Hartmann, Zoltan Balogh, Selina Kolokytha, Ramon Schmid, Kim von Allmen.