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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
Low to high Energies
In-situ studies:- Temperature- Humidity- Mechanical stresses
Detectordevelopments
4
3
X-ray Analytics: Imaging & XRD
Imaging Seeing the invisible
Atomic and Molecular StructureWhere are the atoms
SiO2
Macromolecules
5
Structural properties addressed by X-ray techniques
Domain ordering
Phases
Mosaicity
Stress / Strain
Crystallite Size
Density
XRD / HRXRD
(Interface)
roughness
Layer
thickness
Texture
Defects
Nano-particle Size
Distribution
SAXS / GISAXD
Reflectivity
3D molecular structures for
new materials
Orientation
6
4
Hard Coatings: (Al,Cr)2O3 & (Al,Hf)2O3
7
THERMAL BARRIER COATINGS (TBC)
5
(Al,Cr)2O3 TiCN uncoated
Thermal Stability
9
10
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
9
Post-hot isostatic pressing
Thin film multilayers: PZT
Piezoelectric materials for switches
18
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
19
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
20
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
21
Only small loss in texture. Quantification trough texture index.
Texture developpement in multilayers:
J. Am. Ceram. Soc., 97, 2069–2075 (2014)
22
12
HRXRD
Epitaxial Systems
23
22.07.2016 24Center for X-ray Analytics: [email protected]
Strain
Defects
Layer thickness
Lateral structure
Chemical composition
Lattice parameters
Analytical tasks to address for epitaxy films
24
13
In-plane diffraction
Thin film X-ray Diffraction: Geometries
Out-off-plane diffraction
25
Thin epitaxial films: Out-off plane BTO(002)
26
BaTiO3: reflection (002) on SiOut-off-plane diffraction
d-spacing FWHM FWHM (RC)
BTO-Si 1.9975 0.45 1.401
A. Neels, M. Reinke, P. Hoffmann, A. Dommann
14
22.07.2016 27Center for X-ray Analytics: [email protected]
BaTiO3: asymmetric reflection (103) on Si
BTO
BaTiO3: reflection (103) on Siasymmetrical reflection
A. Neels, M. Reinke, P. Hoffmann, A. Dommann 27
22.07.2016 28Center for X-ray Analytics: [email protected]
In plane diffraction:
28
15
22.07.2016 29Center for X-ray Analytics: [email protected]
BaTiO3: in-plane BTO(200) on Si and MgO
High mosaicity forBTO on MgO
BTO
BTO
MgO
Si substrate MgO substrate
A. Neels, M. Reinke, P. Hoffmann, A. Dommann 29
X-Ray Tomography
30
16
X-RAY CT SETUPS: FAN BEAM & CONE BEAM
31
source
collimator
object
detector line
manipulator
source object
detector arraymanipulator
X-ray uCT (160/220 keV)
Linac X-ray CT (4/6 MeV)
Industrial X-ray CT (450 keV)
Cone beam CT (450 keV)
High energy X-ray imaging
Insulator, region of interest (160 x 140 x 100 mm)
expoxide resign filled with aluminum oxide
pore, d = 0.7 mm
aluminum core
scan parameters:
X-ray source: 450 kV, 3 mA
Pixel size: 0.15 x 0.15 mm
17
• Measurement of X-ray phase-shift and scattering instead of absorption
• Dark field imaging: sensitive to sub-micrometre structures (e.g. pores)
• Virtual Institute for New X-ray Methods in Material Science
X-RAY PHASE CONTRAST AND DARK-FIELD IMAGING
TWO XPCI SYSTEMS
G0G1G2
Add-on to µCT45 keV design energy
New, dedicated setup35 keV design energy
18
BRUKER
XPCI Tomography of a tooth
enamel
caries
dentin
µ-crack
Absorption cross sections Dark-field cross sections
In c
olla
bo
rati
on
wit
hC
SEM
Discussion
XRD and in-situ XRD
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.
36
19
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.
37
KEYNOTE SPEAKERS (to be completed)
Jan Pieter Abraham, Basel University, Switzerland
Bob Cernik, University of Manchester, UK
Birger Dittrich, Georg-August-University Göttingen, Germany
Robert von Dreele, Argonne National Laboratory, USA
Francesca Fabbiani, Göttingen, Germany
Makoto Fujita, University of Tokyo, Japan
Sandra W. Jacob, Novartis Pharma AG, Basel, Switzerland
Sven Lidin, Lund University, Sweden
Gabor Oszlanyi, Academy of Sciences, Budapest, Hungary
Simon Parsons, University of Edinburgh, UK
Werner Paulus, Montpellier, France
Martin U. Schmidt, University of Frankfurt, Germany
Peter Schurtenberger, Lund University, Sweden
Ada Yonath Jean-Marie Lehn