Perspectives on Materials Science in 3D and 4D D. Juul Jensen Section for Materials Science and Advanced Characterization
DTU Wind Energy, Technical University of Denmark
DTU Wind Energy, Technical University of Denmark
3D (x, y, z) and 4D (x, y, z, t) are the ways forward for many types of experiments DTU Wind Energy, Technical University of Denmark
3D techniques are not new • Serial sectioning • Sample dissolution • X-ray methods • Neutron diffraction DTU Wind Energy, Technical University of Denmark
The materials science community has started to realize the need for 3D and 4D results Advancing existing 3D/4D methods and developing new unique techniques Goals include: • Much easier/less manpower-requiring operations • Better spatial resolution • Non-destructive methods • Fast measurements DTU Wind Energy, Technical University of Denmark
Techniques behind the most frequently published 3D/4D results on the micrometer scale Advanced serial sectioning • Semi/fully automatic mechanical sectioning • FIB • Laser sectioning X-ray methods • Tomography • 3DXRD (monochromatic x-ray beam) in many variants • Polychromatic x-ray microdiffraction • Local texture techniques TEM methods • Tomography • 3DOmiTEM DTU Wind Energy, Technical University of Denmark
3DXRD Three Dimensional X-Ray Diffraction from Idea to Implementation DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation Dream 1994 To develop a technique allowing fast non-destructive orientation measurements in µm-sized local volumes within the bulk of mm 3 – cm 3 samples Motivation The need for in-situ studies of local deformation and recrystallization phenomena occurring in the bulk DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation Requirements • High penetration power • High intensity Only possible solution was X-rays from powerfull synchrotron sources DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation Henning F Poulsen DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation Center for Fundamental Research: Metal Structures in 4D, 2001 – 2011, 9 mio Euro DTU Wind Energy, Technical University of Denmark
DTU Wind Energy, Technical University of Denmark 3DXRD Characterization and modeling
3DXRD set-up Area detector Position and shape Orientation and strain DTU Wind Energy, Technical University of Denmark
I II III C A 5 B 4 1 3 LC ML MB WB 2 WBS DTU Wind Energy, Technical University of Denmark
3DXRD – from idea to implementation First version of 3DXRD at ESRF commissioned during the summer of 1999 Today: ESRF: 3D x-ray nanoscope 3D x-ray microscopes now also at APS in USA, SPring 8 in Japan and Hasylab/Desy in Germany. Plus 3DXRD in Shanghai in the near future. DTU Wind Energy, Technical University of Denmark
3DXRD (at ESRF) specifications Experimental conditions – Energy Range 50 – 100 keV Flux 10 11 – 10 12 p/s – Measurements of: – Position and volume – Crystallographic orientation – Elastic and plastic strain – 3D shape – Dynamics Spatial resolution – Mapping precision 500nm x 500nm x 1000nm – Min. size 30nm (no mapping) DTU Wind Energy, Technical University of Denmark 3DXRD Characterization and modeling
Three 3DXRD modes of operation with different time resolutions ? Temporal: msec – sec 30 sec 1 hour DTU Wind Energy, Technical University of Denmark
100 μ m 1277 grains 539 grains E.M. Lauridsen and S.O. Poulsen DTU Wind Energy, Technical University of Denmark
3DXRD measurements Metallurgy: 1. Grain orientation rotations during plastic strain 2. Plastic deformation/ Plastic strain 3. Recrystallization 4. Grain growth 5. Elastic strains in individual grains 6. Phase transformations 7. Relations to mechanical properties • Structural biology • Phamaceuticals • Photochemistry • Geology DTU Wind Energy, Technical University of Denmark
Examples of key experiments done by 3DXRD or the related DCT technique DTU Wind Energy, Technical University of Denmark
Stress corrosion cracking A. King, G. Johnson, D. Engelberg, W. Ludwig, and J. Marrow, Science (2008) 321 , 382 - 385 DTU Wind Energy, Technical University of Denmark
Grain nucleation and growth during phase transformation Construction Steel (0.21%C, 0.51% Mn, 0.20%Si) Cooling: 900 ° C - 600 ° C Low temperature: Ferrite + Cementite High temperature: Austenite Work discussed by Aaronson in Scripta Materialia, and later by Spanos. See also Sharma Acta Mater (2012) 229 S.E. Offerman et al. Science 298 (2002), DTU Wind Energy, Technical University of Denmark 1003-1005
Grain-resolved elastic strains in Cu Cu 50µm initial grain size ~ random texture In situ tensile deformation stress rig driven in position control to a plastic strain of 1.5% (measurements under load) In total 871 bulk grains J. Oddershede et al. Materials Characterization 2011; 62, DTU Wind Energy, Technical University of Denmark 651
Results Accuracy: Center of mass 10 µm Volume 20% rel. error Orientation 0.05º Axial strain 10 -4 Strong effect of orientation on elastic strain along tensile direction DTU Wind Energy, Technical University of Denmark
Plastic deformation - Dislocation structures 2 m m • traditional line profiles analysis • reciprocal space mapping with high angular resolution 3DXRD Al DTU Wind Energy, Technical University of Denmark Work lead by Wolfgang Pantleon
High angular resolution 3DXRD Conventional 3DXRD High angular resolution 3DXRD Zoom DTU Wind Energy, Technical University of Denmark
In-situ XRD investigations with high angular resolution peak shapes • of individual grains • embedded in bulk • during deformation • high angular resolution 0.004 ° =10 ″=7 10 -5 rad B. Jakobsen, H.F. Poulsen, U. Lienert, J. Almer, S.D. Shastri, H.O. Sørensen, C. Gundlach, W. Pantleon, Science 312 (2006) 889 DTU Wind Energy, Technical University of Denmark
High angular resolution 3DXRD = + ------------- B. Jakobsen, H.F . Poulsen, U. Lienert, J. Almer, S.D. Shastri, H.O. Sørensen, C. Gundlach, W. Pantleon Science 312 (2006) 889-892 DTU Wind Energy, Technical University of Denmark
Jakobsen, et al. Scripta Mater. 56 (2007) 769-772 DTU Wind Energy, Technical University of Denmark
Dynamics y = 0 ° a = 1 Rocking (orientation) Detector horizontally (orientation) DTU Wind Energy, Technical University of Denmark
Emergence of subgrains • uninterupted test • strain rate 7 1 6 10 s • subgrains emerge at very low strain • structures form during deformation 2 m m DTU Wind Energy, Technical University of Denmark
Recrystallization Need for 3D and 4D measurements DTU Wind Energy, Technical University of Denmark
Fundamental questions • Where do nuclei form? – And with what orientation? • How do boundaries move? – And interact with dislocations? • Do all nuclei/grains grow with the same speed irrespective of their crystallographic orientation/misorientation? • What are the mobilities of a boundary surrounding a recrystallizing grain and how can it be measured experimentally • • • DTU Wind Energy, Technical University of Denmark 36
Nucleation orientation relationships The orientation of the nuclei important for texture and microstructure (average grain size after recrystallization) DTU Wind Energy, Technical University of Denmark
Nucleation orientation relationships DTU Wind Energy, Technical University of Denmark
Recommend
More recommend
