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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.

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Page 1: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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.

Page 2: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

XRM Applications for Materials Research and Engineering

2

Diverse interests and applications for structural characterization…

Batteries/Fuel Cells Ceramics CompositesPolymers

GlassCoatingsMetals Concrete

DIR 2015 Ghent 2015-06-24

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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

3DIR 2015 Ghent 2015-06-24

ZEISSMetrotomX-ray CT

NDT

Page 4: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

4DIR 2015 Ghent 2015-06-24

Page 5: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

Page 6: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

7

Basics and Principles for DCTHow to Measure? – X-ray Tomography

DIR 2015 Ghent 2015-06-24

Page 7: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

Page 8: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

DIR 2015 Ghent 2015-06-24

Page 9: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

DIR 2015 Ghent 2015-06-24

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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

DIR 2015 Ghent 2015-06-24

Page 11: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

Great tools – but…

Grain Mapping

DIR 2015 Ghent 2015-06-24

Page 12: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

DIR 2015 Ghent 2015-06-24

Page 13: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

DIR 2015 Ghent 2015-06-24

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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

DIR 2015 Ghent 2015-06-24

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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

DIR 2015 Ghent 2015-06-24

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Laboratory Diffraction Contrast Tomography (Lab DCT)Example Results on Timet SValidation against Established Techniques

Lab DCT Synchrotron DCT

DIR 2015 Ghent 2015-06-24

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Laboratory Diffraction Contrast Tomography (Lab DCT)Example Results on Timet SValidation against Established TechniquesComparison of angular misorientation of adjacent grains

DIR 2015 Ghent 2015-06-24

Agreement with established techniques

Page 18: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

Page 19: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)

DIR 2015 Ghent 2015-06-24

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Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)

DIR 2015 Ghent 2015-06-24

Page 21: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

Laboratory Diffraction Contrast Tomography (Lab DCT)Application Examples – University of ManchesterSintering of Cu (4D, ex-situ)

DIR 2015 Ghent 2015-06-24

Page 22: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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)

DIR 2015 Ghent 2015-06-24

Page 23: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

24

Laboratory Diffraction Contrast Tomography (Lab DCT)3D Crystallographic Imaging Techniques Comparison

DIR 2015 Ghent 2015-06-24

Page 24: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

Summary/Outlook

25

• 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

DIR 2015 Ghent 2015-06-24

Page 25: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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

DIR 2015 Ghent 2015-06-24

Page 26: New Developments in 3D Grain Mapping: Using Diffraction … · 2015. 7. 13. · Grain sizes < 1 µm 20-500 µm 40-500 µm 4D Studies x Sub-grain deformation xx Sample Volume (50 µm)^3

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