Oddershede, Jette

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Downloaded from orbit.dtu.dk on: Oct 23, 2019X-ray imaging and 3DXRD - Fundamentals and ApplicationsOddershede, JettePublication date:2010Document VersionPublisher's PDF, also known as Version of recordLink back to DTU OrbitCitation (APA):Oddershede, J. (2010). X-ray imaging and 3DXRD - Fundamentals and Applications. Paper presented at 2010LANSCE Neutron School: Structural Materials, Los Alamos (US), 5-13 Aug, .X-ray imaging and 3DXRD- FundamentalsRisø DTU, Denmark: D. Juul Jensen, E.M. Lauridsen, A. Lyckegaard,            J. Oddershede, U.L. Olsen, W. Pantleon, H.F. Poulsen, S. Poulsen, S. Schmidt, H.O. Sørensen, G. WintherESRF, France: A. Goetz, W. Ludwig, P. Reischig, G. Vaughan, J. WrightAPS, USA: U. Lienert, K. EvansSPRING-8, Japan: K. Uesugi, A. TaheuchiGKSS, Germany:  F. Beckmann, A. KingBrookhaven, USA: L. MarguliesNaval Research, USA: R. Fonda, G. SpanosNorthwestern, USA: I. McKenna, M. P. Gururajan, P. VorheesDTU, Denmark: P.C. Hansen, L. Ottaviani, K. YvindToyohashi Uni, Japan: M. KobyashiCity Uni of N.Y., USA: G.T. HermanTU Berlin, Germany: W. ReimersKTH, Sweden: X. Badel, J. LinrosRisø DTU, Technical University of DenmarkDenmark07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 2Risø DTU, Technical University of DenmarkRisø National Laboratory for Sustainable Energy07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 3CopenhagenRisøRisø DTU, Technical University of DenmarkMotivation4D studies of energy materials07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 4Compositesfor wind Fuel cells Batteries Superconductors Fusion Cell stackCenter for Fundamental Research:Metal Structures in 4 DimensionsRisø DTU, Technical University of DenmarkMicrostructure visualisationSectioning + optical microscopy TEM tomographySample 1cm, Res: 2 µm Sample 500 nm. Res 5 nmFIB+EBSD 3D Atom ProbeSample 20 µm, Res: 30 nm Sample 30 nm. Res 1 Å07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 510 µmRisø DTU, Technical University of DenmarkX-rays- a complementary tool• Non-competitive• Spatial resolution• Diffraction does not give direct imaging• Benefits• Non-destructive• Fast = dynamics• Strain• 50-80 keV = high penetration = bulk grains07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 6Risø DTU, Technical University of DenmarkX-raysSynchrotron radiation• High flux• Low angular divergence• Tunable wavelength07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 7FELRisø DTU, Technical University of DenmarkX-RAY TOMOGRAPHY07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 8Risø DTU, Technical University of DenmarkX-ray tomographyPrinciples and reconstruction07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 9• Conventional tomography uses absorption contrast• Pores, cracks, inclusions….Collect ~1500 absorption images over 180º rotationFiltered back projection algorithm reconstructs the sample– No contrast between two grains of the same phaseMPD-5, Cornell University, Itchaca, NY, July 18-20 2007Risø DTU, Technical University of DenmarkX-ray tomographyWhat gives the contrast?07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 10Absorption PhaseSmallest detectable hole at 25 keV in a 4 mm thick sample:Absorption: 20 µmPhase: 0.05 µmDiffractionGrain shapes and orientationscan be obtained.Principle and results:Application lectureRisø DTU, Technical University of DenmarkAbsorption contrastPlastic flow in 3D07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 11Cu with 200,000 W particles:Displacement fieldResult: domains---------------------K. Haldrup, S. F. Nielsen, F. Beckmann, J. A. WertJ. Microscopy,  222 (2006),  28–35Risø DTU, Technical University of DenmarkPhase contrastGrain boundaries in 3D07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 12100	µmSample-detector distanceb-Ti alloy with a-Ti formed on grainboundaries upon annealing at 725°C Risø DTU, Technical University of DenmarkPhase and diffraction contrastGrain boundaries and orientations in 3D• Comparisons with phase field simulations are ongoing07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 13Cylinder diameter 300 µm. Grain size 30 µm. Voxel size 0.7 µm. DCTPhase contrast tomographyβα+β---------------------I. McKenna, M.P. Gururajan, P. Voorhees, E.M. Lauridsen, S.O. Poulsen, W. LudwigR.W. FondaRisø DTU, Technical University of DenmarkPhase versus diffraction contrastDiffraction contrast tomographyPhase contrast tomographyREVIEW OF SCIENTIFIC INSTRUMENTS (2009), 80, 033905, W. Ludwig, P. Reischig, A. King, M- Herbig, E. M. Lauridsen, G. Johnson, T.J. Marrow and J.Y. Buffiere100 µm07-aug-201014 Jette Oddershede   jeto@risoe.dtu.dk Risø DTU, Technical University of Denmark3-DIMENSIONAL X-RAY DIFFRACTION(3DXRD) MICROSCOPY07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 15Risø DTU, Technical University of DenmarkNear-field~10 mmFar-field20-50 cm3DXRD setup07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 16Movie by J. BernierRisø DTU, Technical University of Denmark 07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 17Risø DTU, Technical University of DenmarkNear-field~10 mmFar-field20-50 cm3DXRD setup07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 18In situ sample environmentsTime resolutionStrain resolutionSpatial resolutionRisø DTU, Technical University of DenmarkData analysisSoftware07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 19• FABLE: Fully Automatic BeamLines and Experiments• Open source software for analysis of 3DXRD data• http://sourceforge.net/apps/trac/fable/wiki• ~10 developers/contributors:• Risø DTU• ESRF• APS• Lawrence Livermore • TU DelftRisø DTU, Technical University of DenmarkData analysisIdentifying grains07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 20Indexing: Identifying copies of the set of theoretical reflections in the polycrystalline dataset. RotationsRisø DTU, Technical University of DenmarkData analysisGrainSpotter07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 21Spots:Filter bad spots awayIndexing: Find vertices in Rodrigues(orientation) spaceIntegrated intensities:Determine grain volumesS. Schmidt, in workTrick:Straight lines inRodrigues spaceResult of simulations:Find 700 out of 700 grainswithin 30 secRisø DTU, Technical University of DenmarkData analysisRefining grain properties• Position• Orientation• Strain• Volume• Morphology or shape• Phase or crystal structure07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 22And most importantly:How these evolveduring the in situexperiment!Risø DTU, Technical University of DenmarkLimitations07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 23• Mapping a representative volume• Larger deformationsUndeformed  6% deformed100 grains  10,000 grainsRisø DTU, Technical University of DenmarkExperiment design 07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 24Time resolutionSpatialresolutionManygrainsEvolution ratesGrainshapesStatisticsYou cannot have it all LRisø DTU, Technical University of DenmarkExperiment design • Grain averaged data• Time resolution• Farfield• Voxellated data• Spatial resolution• Nearfield07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 25Risø DTU, Technical University of DenmarkHigh time resolutionNucleation and grain growth07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 26Grain volume (µm3 )01020304050Annealing time (s)0 400 800 1200 1600 2000 2400Grain radius (µm)0246Fig. 3 Growth curves:0 20 40 60 8001020304050Nucleation time [min]Frequency [%]All orientations0 20 40 60 8001020304050Nucleation time [min]Frequency [%]Cube orientation0 20 40 60 8001020304050Nucleation time [min]Frequency [%]Rolling orientations0 20 40 60 8001020304050Nucleation time [min]Frequency [%]Other orientations0 2 4 6x 10-30510152025Growth rate [µm/s]Frequency [%]All orientations0 2 4 6x 10-30510152025Growth rate [µm/s]Frequency [%]Cube orientation0 2 4 6x 10-30510152025Growth rate [µm/s]Frequency [%]Rolling orientations0 2 4 6x 10-30510152025Growth rate [µm/s]Frequency [%]Other orientations244 grainsStatisticsNew Avrami-type model0                   1                   2log (time)log(-ln(1-VV))E.M. Lauridsen, H.F. Poulsen, S.F. Nielsen, D. Juul Jensen (2003) Acta Mat. 51, 4423 AnnealingNucleation = new spotsGrowth = intensity increaseFarfield detectorSmall scan range Risø DTU, Technical University of DenmarkMany grainsPlastic deformation07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 272D centre of massPositions and orientation0%, 3% and 9% deformationFarfield detectorLarge scan range Layer-by-layer0% -> 3% 0% -> 9% J. Oddershede, J.P. Wright, L. Margulies, X. Huang, H.F. Poulsen, S. Schmidt and G. WintherIF steel BCC100 110111Cu FCC0% -> 6%G. Winther, L. Margulies, S. Schmidt and H. F. Poulsen (2004) Acta Mater. 52, 2863Risø DTU, Technical University of DenmarkHigh spatial and time resolutionRecrystallization of 42% deformed pure Al07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 28--------------------------S. Schmidt, S. F. Nielsen, C. Gundlach, L. Margulies, X. Huang, D. Juul Jensen (2004) Science 305, 229.Nearfield, one reflectionTotal annealing time at ~300°C: 30 h 50 layers of 6 µmShape resolution: 5 µmTime resolution: 10 minHeterogeneous growth with protrusionsRisø DTU, Technical University of DenmarkHigh spatial resolution, many grainsNi, undeformed07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 29-----C.M. Hefferan, S.F. Li, J. Lind, U. Lienert, A.D. Rollett, P. Wynblatt, R.M. Suter, Computers, Materials and Continua, 14, 209-219 (2009).Nearfield, large scan range 9 layers, 1101 grainsResolution: 5 µm and 0.1°Grain boundary statisticsRisø DTU, Technical University of DenmarkBridging grain averaged and voxellated data Laguerre tesselation• Method to get approximate 3D grain map from centre of mass positions and relative grain volumes07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 30Risø DTU, Technical University of DenmarkBridging grain averaged and voxellated data Laguerre tesselation• Method to get approximate 3D grain map from centre of mass positions and relative grain volumes• Test on positions, volumes and grain shapes from from microtomographyon meta-stable beta-titanium alloy 07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 31--------------------------Lyckegaard, Lauridsen, Ludwig, Fonda and Poulsen (2010) Adv. Eng. Mater. in press Risø DTU, Technical University of DenmarkWhere can these experiments be performed?Dedicated 3DXRD setups• ID11, ESRF, Grenoble, France • 1-ID, APS, Chicago, USA• HEMS, Petra-III, Hamburg, Germany• From 201107-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 32Risø DTU, Technical University of DenmarkSummary• Penetration power to non-destructively probe bulk structures• Probing volume large enough to obtain grain statistics• Sufficient time resolution to follow typical processes in situ• Depending on setup a number of the following can be probed: grainposition, morphology, phase, orientation, elastic strain07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 33Risø DTU, Technical University of DenmarkTake home messages• Application examples• The potentials of 3DXRD and X-ray tomography• Inspiration• Don’t be afraid to try new techniques!• Experiment design• Define exactly what information you want to gain from the experiment• Realise that you will probably have to prioritise between spatialresolution, time resolution and the number of grains• Discuss with beam line scientist prior to applying for beamtime07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 34Risø DTU, Technical University of DenmarkOutlook for next talk• Strain can only be obtained by diffraction• Mapping subgrain structures• Diffraction contrast tomography• Pushing the limits of voxellated mapping• Better spatial resolution, going nano• Higher deformations07-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 35Risø DTU, Technical University of DenmarkReferencesOverviews 3DXRD:• Chapter 19 in ”Neutrons and Synchrotron Radiation in engineeringMaterials Science” Eds. W. Reimers et al., (Wiley, 2008)• H.F. Poulsen. In ”Advanced Tomographic Methods in Materials Research and Engineering”,  Ed.: J. Banhart (Clarendon, Oxford, 2007)• D. Juul Jensen et al. Materials Today (2006) 9, 18-25.• H.F. Poulsen et al. MRS Bulletin, March 2004, pp 166-169• H.F. Poulsen: ”Three-dimensional X-ray diffraction microscopy”. (Springer, Berlin, 2004)Software:• http://sourceforge.net/apps/trac/fable/wikiComparison 4D experiments and 4D modelling:• MRS Bulletin June 200807-aug-2010Jette Oddershede   jeto@risoe.dtu.dk 36

X-ray imaging and 3DXRD - Fundamentals and Applications

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X-ray imaging and 3DXRD - Fundamentals and Applications

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