3D tracking of microstructure responses: nf-, ff-hedm and High Energy Tomography

Transcription

1 3D tracking of microstructure responses: nf-, ff-hedm and High Energy Tomography Bob Suter D. Menasche, S. Madalli, R. Chen A.D. Rollett P. Kenesei, J. S. Park, S. Shastri, J. Almer P. Shade Carnegie Mellon University, Advanced Photon Source, AFRL Support at CMU: NSF, DOE/BES/NNSA, AFRL Carnegie Mellon Summer School 2015

2 Outline 1. Near-field HEDM measurement a. Ex: Complex topologies in Ti64 b. Ex: REX in high purity Al 2. APS 1-ID facilities (future developments later) a. Near-field, far-field, tomography b. Ex: Ti-7Al creep 3. High Energy X-rays and diffraction a. Near- vs far-field detector images 4. Data flow (current developments) 5. The APS Upgrade project and implications

3 Non-destructive 3D mapping of microstructures Direct Observation of Responses Via Near-field High Energy X-ray Diffraction Microscopy (nf-hedm) Advanced Photon Source Measurements 1-ID high brilliance, kev x-rays Millimeter samples probed with micron spatial, < 0.1 deg orientation resolution Tera-byte data sets > 3 x 10 6 Bragg peaks 10 3 core parallel processing: 2D images to 3D orientation maps HEDM measurement schematic Image diffracted beams 360 images/layer ~100 successive crosssections Poulsen, Springer 2004 Suter et al, Rev. Sci. Instruments, 2006 Li and Suter, J. Appl Cryst, D copper microstructure Colors represent crystal lattice orientations Computational reconstruction Optimizes orientations in > 10 7 voxels (volume elements) 0.4 mm 3

4 Forward Modeling Reconstruction: Minimal initial assumptions Mesh illuminated plane Mesh size << grain size Search orientation space Optimal orientation provides maximal overlap of simulated diffraction with observed diffracted beams Suter et al, RSI

5 Forward Modeling Reconstruction: Minimal initial assumptions Copper: 0.4 mm 3 Li & Suter, J. Appl. Cryst Suter et al, RSI 2006 ~10 5 voxels/layer > 10 7 orientations resolved per voxel ~100 layers Parallel computation: CMU, NSF/XSEDE Shortcuts: Hierarchical search Growth of found orientations Input from far-field measurements A brute force but general purpose microstructure measurement 5

6 Confidence metric C = fraction of simulated peaks overlapping experimental peaks Relative measure, not an absolute metric Reduction at boundaries: extrapolating voxel scattering to edges of reduced experimental diffraction spots Reduction in deformed materials: loss of high Q scattering 0.6 Confidence J. Lind work Annealed Zr 0.25

7 Near-field Data Collection Over Dw = 180 deg, collect N images integrated over dw intervals Traditionally, dw = 1 deg Interline CCD detector interfacing allows continuous rotation and readout: dw more or less arbitrary Rotation speed Material and material state dependent: deformation reduces signal strength (particularly at high Q) Higher Z materials scatter more strongly 1 to 5 seconds per degree (reduced by SCU) Layer data sets 180 to 1800 images for each of two to three L-distances 4MB per image: 1.4 to 14 GB per layer 6 to 30 minutes per layer Volume data sets: ~ 100 layers 36,000 to 360,000 images, 140 GB to 1.4 TB per sample state 4 micron spacing: 0.4 mm length, ~0.4mm 3 volume spanned

8 Ti-6Al-4V: Complex alpha-phase morphologies E. Wielewski, et al, submitted to JAC 8

9 ALPHA COLONY MORPHOLOGY EXAMPLES 9

10 BURGERS ORIENTATION RELATIONSHIP 6 variants b Phase High T 12 variants a Phase Room T 10

11 PRIOR-BETA GRAIN RECONSTUCTION a Phase Room T b Phase High T 11

12 COLONY RELATIVE MISORIENTATION DISTRIBUTIONS 12

13 Misorientation (deg) COLONY RELATIVE MISORIENTATION

14 Example: Light annealing of high purity aluminum Spatially resolved recovery and recrystallization Single layer in three states Annealing Hefferan et al, Acta Mat 2012

15 Hefferan et al, Acta Mat 2012 annealing Recrystallization in pure Al Voxel-based reconstruction shows new grain and nature of prior neighborhood Lattice orientations Confidence metric KAM map: 0.5 deg scale

16 Simple ex-situ set-up: Near-field, far-field, tomography Sample Sample translations Aerotech air bearing rotation Stage translations

17 Combining nf- and ff-hedm: AFRL-PUP APS 1-IDE hutch J. Schuren, P. Shade, T.J. Turner (AFRL) J. Park, P. Kenesei, J. Almer, A. Mashayekhi, K. Goetze, E. Benda (APS) S.F. Li, J. Lind, J. Bernier (LLNL), D. Menasche, R.M. Suter (CMU), B. Blank (PulseRay) 17

18 Combining nf- and ff-hedm: AFRL-PUP APS 1-IDE hutch J. Schuren, P. Shade, T.J. Turner (AFRL) J. Park, P. Kenesei, J. Almer, A. Mashayekhi, K. Goetze, E. Benda (APS) S.F. Li, J. Lind, J. Bernier (LLNL), D. Menasche, R.M. Suter (CMU), B. Blank (PulseRay) 18

19 Focusing Optics: Si sawtooth lenses: ~ 1 meter focal length 1 mm beam at sample position Au fluorescence: knife-edge scan Top and bottom lenses

20 AFRL in-situ loading apparatus Full rotation under load Rotation and Axial Motion System (RAMS) Far Field Detector 20

21 AFRL in-situ loading apparatus Full rotation under load Rotation and Axial Motion System (RAMS) Sample grips Air bearings Far Field Detector 21

22 AFRL in-situ loading apparatus Full rotation under load Rotation and Axial Motion System (RAMS) Far Field Detector Incident beam Beam block 22

23 AFRL in-situ loading apparatus Full rotation under load Rotation and Axial Motion System (RAMS) Far-field Detector Near-field Camera Incident beam Scintillator 23

24 Ti-7Al Creep Evolution: combined nf- and ff-hedm using same line focused beam Schuren et al, COSSMS

25 Ti-7Al Creep Evolution Schuren et al, COSSMS

26 High Energy Photons: Access to Bulk Structure

27 Commissioning of Superconducting Undulator June 2015

28 Rotating Crystal Measurement with Area Detector Movie courtesy of J. Bernier k f = k i + G hkl when k. i G hkl = - G hkl 2 / 2

29 At high energies, q s are small and this condition is not restrictive

30 Number of Bragg peaks over 180 degrees

31 Number of Bragg peaks over 180 degrees Example: Aluminum

32 Number of Bragg peaks over 180 degrees Example: Aluminum

33 Near-field: Extended scattering from extended grains

34 Near-field: Extended scattering from extended grains

35 Near-field: Extended scattering from extended grains Image analysis: Separate signal from background Keep weak signals next to strong ones Reconstruction matches binary patterns

36 Far-field: Peaks on Debye-Scherrer Rings Almost complete rings from fine grained structure GE medical imaging detector, 80 mm pixels AM 316L stainless, as deposited

37 Far-field: Peaks on Debye-Scherrer Rings Isolated Bragg peaks from coarsened structure GE medical imaging detector, 80 mm pixels AM 316L stainless, annealed

38 Work flow

39 First IceNine reconstruction on ALCF s BlueGene/Q (Mira) Run on July 3, 2015 D. Menasche (CMU) and K. Maheshwari (ANL) Toward real time data availability during runs Pipeline preparation for August AFRL-PUP run 40mm x 50mm x 30 mm annealed gold (Shade) Lattice Orientation Map Confidence Map

40 nf-, ff- & Tomography Combined

41 Y (µm) Y (µm) The APS Upgrade: The world s leading high-brightness hard x-ray storage ring The APS Upgrade is a nextgeneration x-ray synchrotron: Optimized for hard x-rays Incorporating advanced beamlines, optics and detectors Round source ideal for imaging APS Upgrade will exceed the capabilities of today s synchrotrons by 2 to 3 orders of magnitude in Brightness Coherent flux Nano-focused flux World s brightest storage ring light source above 4 kev APS Today X (µm) Technical features Technical Features APS Upgrade X (µm) 6 GeV, 200 ma, swap-out injection Circumference 1100 m Multi-bend achromat (7 bend) lattice High-brightness, ultra-low emittance (e x, e y ) 50-60, 5-50 pm Diffraction limited vertical emittance to 15 kev, horizontal emittance to 2 kev 35 insertion device straight sections Flexible operation: High-brightness and timing modes, round and flat beams >30 world-class ID beamlines upon commissioning 43

42 Critical beam characteristics for coherent diffraction at high energies (~ 60 kev) Higher coherence fraction than current beam at 10 kev Comparable coherent flux to current beam at 10 kev

43 Topological defect dynamics in operando battery nanoparticles, Ulvestad et al, Science 348, 1344 (2015) Single spinel nanoparticle Observe Angstrom scale elastic distortion field around a dislocation at 30nm resolution Watch dislocation motion during charging / discharging With high energy Bragg CDI, can watch such fields in metallic polycrystals respond to thermal, mechanical, other external fields

44 Conclusions nf- + ff- + tomo has become standard in HEDM measurements Variety of thermo/mechanical conditions in development High value data sets, expensive to obtain Unique observations Ideal for comparison to models Direct relevance here Meshing, registration, data mining The future Proposal for dedicated, high throughput beamline Mail-in? 3D maps output, not diffraction data Upgrade Accelerated collection, higher spatial resolution, zoom in to nano-scale