New Developments in 3D Grain Mapping: Using Diffraction Contrast Tomography (DCT) on a Laboratory X-ray Microscope DIR 2015 Ghent, 2015-06-24 Michael Feser Carl Zeiss X-ray Microscopy, Inc.
New Developments in 3D Grain Mapping: Using Diffraction Contrast Tomography (DCT) on a Laboratory X-ray Microscope
DIR 2015 Ghent, 2015-06-24
Michael FeserCarl Zeiss X-ray Microscopy, Inc.
XRM Applications for Materials Research and Engineering
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Diverse interests and applications for structural characterization…
Batteries/Fuel Cells Ceramics CompositesPolymers
GlassCoatingsMetals Concrete
DIR 2015 Ghent 2015-06-24
Material Science Microscopy Toolset
3D Voxel Dimension [m]10-3 10-4 10-5 10-6 10-7 10-8
sam
ple
size
[m]
1
10-1
10-2
10-3
10-4
10-5
10-6
ZEISSXradia Ultra
ZEISSXradia Versa
Sub-micron 3D X-ray MicroscopeHigh-resolution X-ray Detectors
Nanoscale3D X-ray MicroscopeX-ray Optics for Magnification FIB-SEM
10-9
10-7HIM
ZEISS Crossbeam
ZEISSORION Nanofab
micron nanometer
micron
mm
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ZEISSMetrotomX-ray CT
NDT
0
2
4
6
8
10
12
14
0 10 20 30 40 50
Res
olut
ion
(µm
)
Geometric Mag Based MicroCTs
Resolution rapidly degrades with increasing sample size
X-ray Microscope versus Micro-CT
Working Distance (mm)Source to center of sample rotation
High Res
Low
Res
Substantial difference in resolution as sample size increases
XRM
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X-rays
SampleDetector
Conventional Tomography: Absorption (and some phase) Contrast
+ With particles of varying density6
Basics and Principles for DCTHow to Measure? – X-ray Tomography
DIR 2015 Ghent 2015-06-24
X-rays
Detector
Conventional Tomography: Absorption (and some phase) Contrast
Sample+ Polycrystalline sample, same density
Problem: No grain contrast! Resolved by operating in DCT mode
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Basics and Principles for DCTHow to Measure? – X-ray Tomography
DIR 2015 Ghent 2015-06-24
ZEISS Xradia 520 Versa
Vision: Make X-ray 3D crystallographic imaging a routine tool on a laboratory x-ray microscope
Powered by
Beyond Structural Imaging:Spatially Resolved Crystallographic Information
DIR 2015 Ghent 2015-06-24
• Many engineering materials (metals, ceramics) are polycrystalline and their properties are heavily affected by their grain structure
• Generally there is no contrast in normal CT imaging to visualize grains
3D Crystallographic X-ray ImagingDeveloped at Synchrotron Sources
Provides complimentary information to e.g. absorption & phase contrast
Non-destructive -> allows for studies of microstructure evolution
A. Johnson, E.M. Lauridsen, P.W. Voorhees et al. In preparation
M. Herbig, A. King, P. Reischig, H. Proudhon, E.M. Lauridsen, J. Marrow, J-Y Buffiere, W. Ludwig, Acta Materialia 59 (2011) 590–601
Key points:
C.M. Hefferan, J. Lind, S. Li, U. Lienert, A.D. Rollett, R.M. Suter, Acta Materialia 60 (2012) 4311–4318
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Coupling to 3D simulations
• 3D grain maps are perfectly suited for coupling to 3D computer simulations of microstructure evolution
I.M. McKenna, S.O. Poulsen, E.M. Lauridsen, W. Ludwig, P.W. Voorhees, Acta Materialia, 78 (2014), 125-134
Experiment Simulation
W. Ludwig, A. King, P. Reischig et al, Materials Science and Engineering A 524 (2009) 69–76
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Existing facilities for 3D Crystallographic Imaging at Synchrotrons
APS: HEDM/3DXRD/DAXM
ESRF: 3DXRD/DCT
PETRA: 3DXRD/DCT
SPRING-8: 3DXRD
CHESS: HEDM/3DXRD
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Great tools – but…
Grain Mapping
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Patent Pending
Lab DCT Details Add-on module to standard
ZEISS Xradia 520 Versa
Not impacting standard use
White divergent X-ray beam
Laue focusing geometry
Experimental Implementation:
Laboratory Diffraction Contrast Tomography (Lab DCT)Introduction of the Technology
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Patent Pending
Version 0.5 implementationLaue focusing geometry
L LSource Sample Detector
Source Focusing position Magnifying position
Laboratory Diffraction Contrast Tomography (Lab DCT)Laue Focussing Geometry
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Complimentary validation experiments: Synchrotron DCT + EBSD
Application Case Timet S titanium alloy
labDCTvs
synchDCT
labDCTvs
EBSD
1) Top region mapped by synchDCT
2) Top layer removed by
polishing
3) New top layer mapped by EBSD
4) New top region mapped by labDCT
5) SynchDCT & EBSD used for
validation
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Laboratory Diffraction Contrast Tomography (Lab DCT)Example Results on Timet SSample and Reconstruction
Material Beta-21S titanium
Grain size 100-400 micron
Space group 229 (Im-3m)
#grains 176
Sample photograph
Diffraction pattern on Detector
Reconstructed crystallography
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Laboratory Diffraction Contrast Tomography (Lab DCT)Example Results on Timet SValidation against Established Techniques
Lab DCT Synchrotron DCT
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Laboratory Diffraction Contrast Tomography (Lab DCT)Example Results on Timet SValidation against Established TechniquesComparison of angular misorientation of adjacent grains
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Agreement with established techniques
Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)
DIR 2015 Ghent 2015-06-24
• Ex-situ sintering of samples at 1050 ˚C
• Observing re-orientation and consolidation of grains
Manuscript in preparation
Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)
DIR 2015 Ghent 2015-06-24
Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)
DIR 2015 Ghent 2015-06-24
Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)
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Recent DCT reconstruction results of rock salt embedded in epoxy
Identification of grain centers:
Identification of grain orientations:
Orientation of cubes matching facets of { 1 0 0 } from cleaving of rock salt.
Note: not all grain centerslie in the shown tomography slices Successful identification of grain positions and orientations
Laboratory Diffraction Contrast Tomography (Lab DCT)Application Example – Low-Z Material (Rock Salt)(Proxy material for high-performance explosives)
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3D EBSD Synchrotron DCT GrainMapper3D™ lab DCT
Probe Electrons Synchrotron X-rays Laboratory X-rays
Non-destructive x
Voxel dimension 0.2 µm 1-5 µm ~5 µm
Angular resolution 0.1 - 0.5° 0.05° ~0.1°
Scanning time 4 – 60+ hours 0.5h – 2h ~2h-10h
Grain sizes < 1 µm 20-500 µm 40-500 µm
4D Studies x
Sub-graindeformation x x
Sample Volume (50 µm)^3 (0.3-2.0 mm)^3 (0.3-2.0 mm)^3
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Laboratory Diffraction Contrast Tomography (Lab DCT)3D Crystallographic Imaging Techniques Comparison
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Summary/Outlook
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• DCT modality demonstrated and now available on laboratory XRM• Validated against synchrotron/EBSD performance comparable to
synchrotron-based approaches• Enables 4D studies, under in situ environments to follow
microstructure evolution• Complementary to EBSD which can be performed after
evolution (coroner’s office)• Provides environment to perform ‘routine’ DCT acquisition and
reconstruction by non-experts• Potential to expand, future capabilities (higher resolution, full 3D
morphology, strain, multi-phase etc.)• Pilot installations
• U. Manchester, U.K.• Denmark Technical University, Denmark
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Acknowledgments
Research Collaboration Partners:
• University of Manchester: Phil Withers, Sam McDonald, Robert Bradley
• DTU-Wind: Søren Faester and Yubin Zhang
• Los Alamos National Laboratory: Brian Patterson
Commercial Development Partners:
• Xnovo Technology ApS: Erik Lauridsen, Peter Reischig, Henning Poulsen
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