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X-ray Diffraction Techniques for Materials Characterization

X-ray Diffraction Techniques for Materials Characterization. Jim Britten McMaster Analytical X-ray (MAX) Diffraction Facility Chemistry / BIMR. OUTLINE. Diffraction Single Crystal Diffraction XRD – Powder Diffraction XRD 2 – 2D Powder Diffraction XRD 3 – 3D Polycrystal Diffraction

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X-ray Diffraction Techniques for Materials Characterization

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  1. X-ray Diffraction Techniques for Materials Characterization Jim Britten McMaster Analytical X-ray (MAX) Diffraction Facility Chemistry / BIMR 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  2. OUTLINE • Diffraction • Single Crystal Diffraction • XRD – Powder Diffraction • XRD2 – 2D Powder Diffraction • XRD3 – 3D Polycrystal Diffraction • Diffuse and Incommensurate Scattering • CLS – Brockhouse X-ray Diffraction and Scattering Sector and more 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  3. Diffraction • Sub-nanoscale measurements (Ǻ) • Interatomic distances ~ 0.8 to 3.5 Ǻ • Use ‘Hard’ X-rays as ruler, ~ 0.2 to 3.0 Ǻ • X-rays interact with electrons • Scattering power increases linearly with atomic number • Assume elastic absorption and emission • Each atom becomes X-ray source at λ 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  4. Diffraction • Atomic electron cloud causes exponential drop-off of scattering power away from incident X-ray beam direction (compare to neutrons!) From Pecharsky and Zavalij 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  5. Diffraction • The diffraction pattern is the resultant of scattering from a group of atoms • Fhkl = Σ faexp(hx+ky+lz) • If the group of atoms (unit cell) is repeated periodically in 3D, single crystal diffraction restricts h,k,l to integers, and results in Bragg diffraction spots. 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  6. Single Crystal Diffraction • Bragg’s law for single crystal diffraction • nλ = 2d sinθ • http://www.eserc.stonybrook.edu/ProjectJava/Bragg/index.html • Map diffraction pattern into Reciprocal Space 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  7. Single Crystal Diffraction From Pecharsky and Zavalij 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  8. Single Crystal Diffraction From Pecharsky and Zavalij 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  9. Single Crystal Diffraction • Symmetry of packing determines crystal class • Anorthic, monoclinic, orthorhombic, trigonal, tetragonal, hexagonal, cubic • Symmetry elements define one of 230 space groups • Point symmetry of unit cell determines symmetry of diffraction pattern • Translational symmetry elements result in systematically absent Bragg spots. 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  10. Single Crystal Diffraction • Crystal size 1 to 500 μm – need minimum volume • 200 - 500 μm X-ray point source (Mo) • Transmission expt. • CCD area detector • 3 or 4 circle goniometer 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  11. Single Crystal Diffraction • Data collection • Rotate crystal in beam ~0.36° during CCD acquisition • Collect contiguous frames to scan reciprocal space • Rotate sample on alternate axes to complete coverage of asymmetric diffraction volume • Redundancy helps (aniso. abs. corr., S/N) 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  12. Single Crystal Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  13. Single Crystal Diffraction 3D reciprocal space 2θ increases radially Resolution increases radially Reciprocal cell indexed on lattice Spot intensities depend on atom types and positions Fourier transform of F’s (√I) with phases gives ρ(r) Refine model by least squares minimization of ω||Fo2|-|Fc2|| 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  14. Single Crystal Diffraction • H2Na2Ni3O10P2 , or Na2Ni3(OH)2(PO4)2 • Space group C2/m, Z = 2 • a = 14.2292(7), b = 5.6786(3), c = 4.9249(2)Ǻ, α = 90, β = 104.328(3), γ = 90° • Atom positions • x y z U(eq) • ______________________________________ • Ni(1) 0 .5000 .5000 .006(1) • Ni(2) 0 .2330(1) 0 .006(1) • P(1) .1251(1) 0 .5968(2) .005(1) • O(1) .0722(1) .5000 .2116(2) .007(1) • O(2) .0880(1) .2232 .7173(2) .008(1) • O(3) .0934(1) 0 .2721(2) .006(1) • O(4) .2357(1) 0 .6928(2) .012(1) • Na(1) .2658(1) 0 .2119(2) .022(1) • H(1) .1288 .5000 .2453 .008(14) • Peter Tremaine, Liliana Trevani – Guelph University 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  15. Single crystals 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  16. XRD – Powder Diffraction • Major method of materials characterization • Identification, ‘fingerprinting’ • Quantitative phase analysis • Rietveld structure refinement • Ab initio structure solution • Use a bucket of microcrystals: 1 – 20 μm • Need uniform orientation distribution • Transmission and reflection geometries, line source • “Fundamentals of Powder Diffraction and Structural Characterization of Materials” • Vitalij K. Pecharski and Peter Y. Zavalij 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  17. XRD – Powder Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  18. XRD – Powder Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  19. XRD – Powder Diffraction Calculated ideal powder pattern from single crystal structure. 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  20. XRD – Powder Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  21. XRD2 – 2D Powder Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  22. XRD2 – 2D Powder Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  23. XRD2 – 2D Powder Diffraction • Micro layers of Au & Pt sheet • Purdy, Garret • Au on top layer • Notice the texture from rolling of sheets 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  24. XRD2 – 2D Powder Diffraction • Nano-layers - solid solution of Au & Pt Pt: (80.188, 9659) (SS: 79.5, 7325) (Au: 77.643, 6850) 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  25. XRD2 – 2D Powder Diffraction • Compare the Ferrite (110), (200) and (211) peaks and Austenite (111), (200) and (220) peaks (2θ = 18 to 38) • X-ray diffraction performed using Mo Kαradiation • Detector moved back to 17 cm to improve the resolution • Detector position: 2θ = -28 • Sample position: ω = 166, χ = 55, φ = 0 to 50 • Time = 300s • wt. % C is calculated from the measured lattice parameter of the retained austenite 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  26. XRD2 – 2D Powder Diffraction • Texture analysis – crystallite orientations • 5° frames for coarse textures • 1° frames for sharp features • Generate stereographic projection for chosen 2θ 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  27. XRD2 – 2D Powder Diffraction • (1 1 1) orientations for CdTe on SrTiO3 (100) 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  28. A B C D 5 um 0 D A B C 5 um 5 um 0 0 0 5 um XRD2 – 2D Powder Diffraction • The Role of Substrate Surface Termination in the Deposition of (111) CdTe on (0001) Sapphire • S. Neretina, P. Mascher, R. A. Hughes, J. F. Britten, J. S. Preston, N. V. Sochinskii • 2D-XRD data and the corresponding AFM images showing the evolution of the domain structure and surface morphology as the substrate termination evolves from oxygen to aluminum (left to right). 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  29. XRD2 – 2D Powder Diffraction • Polymer diffraction – WAXS • Fraction of polymer crystalline • Fraction of polymer fibrous • Fraction of polymer amorphous • Texture as a result of preparation • Polymer diffraction – SAXS • Nanoscale interactions • Polymer profiles 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  30. XRD2 – 2D Powder Diffraction Polyethylene(PE) Fiber axis∥[001] 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  31. XRD2 – 2D Powder Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  32. XRD2 – 2D Powder Diffraction • SAXS on a single crystal instrument • Parallel focused Cu RA, SMART6000 CCD 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  33. XRD2 – 2D Powder Diffraction • Residual stress analyses • Choose high angle line • 7 to 10 frames at various orientations, ~1hr • Co or Cr radiation best, Cu okay, Mo useless • Find peak position (2θ) for several hundred points • Bi- or Tri-axial stress elements calculated from deviations from circle (or sphere) 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  34. σ2 = - 486 MPa σ1 = - 394 MPa XRD2 – 2D Powder Diffraction Principle stresses 310 Compressive biaxial stress for 5% elongated TRIP steel 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  35. XRD3 – 3D Polycrystal Diffraction • When we scan around φ or ωfor orientation information for a polycrystalline solid using a 2D detector, we are storing 3D reciprocal space information • Why not have a look at it??? • MAX3D can display the full diffraction volume • http://www.chemistry.mcmaster.ca/facilities/xray/MAX3D.htm 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  36. XRD3 – 3D Polycrystal Diffraction • Texture scan of Au/Pt system • Concentric shells at Bragg allowed 1/d • Hot spots show crystallite orientation distribution for each reflection 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  37. XRD3 – 3D Polycrystal Diffraction • Texture of CdTe film on SrTiO3 • All nanocrystals have 111 direction normal to substrate • Several preferred rotational orientations, with ‘Gaussian’ distribution 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  38. XRD3 – 3D Polycrystal Diffraction • Observe all ‘pole figures’ at once • Scan reciprocal space volume with 2θ probe 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  39. XRD3 – 3D Polycrystal Diffraction • Compare 111 pole figure at ~23° 2θ 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  40. Diffuse and Incommensurate Scattering • Incommensurate Lattices • Gaulin, Dabkowska, Dr. J.P. 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  41. Diffuse and Incommensurate Scattering • LuFe2O4 - Young-June Kim 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  42. Diffuse and Incommensurate Scattering 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  43. Diffuse and Incommensurate Scattering 9° Slice of Reciprocal Space for LuFe2O4 at various temperatures -160C 24C 80C 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  44. Diffuse and Incommensurate Scattering 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  45. Diffuse and Incommensurate Scattering 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  46. Canadian Light SourceHard X-ray Diffraction Capabilities • Hard X-ray MicroAnalysis (HXMA) • Canadian Macromolecular Crystallography Facility (CMCF 1 and CMCF 2) • Very Sensitive Elemental and Structural Probe Employing Radiation from a Synchrotron (VESPERS) • Synchrotron Laboratory for Micro And Nano Devices (SyLMAND) • Brockhouse X-ray Diffraction and Scattering Sector 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  47. Canadian Light SourceHard X-ray Diffraction Capabilities • Hard X-ray MicroAnalysis (HXMA) • Description: The Hard X-ray Micro-Analysis (HXMA) beamline at CLS 06ID-1 is a multipurpose hard X-ray beamline, based on a 63 pole superconducting wiggler. The HXMA has been designed to provide the community with XAFS, K-B mirror microprobe, and x-ray diffraction capabilities. • Techniques: • X-ray Absorption Fine Structure (XAFS) • Microprobe • Diffraction 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  48. Canadian Light SourceHard X-ray Diffraction Capabilities • Canadian Macromolecular Crystallography Facility (CMCF 1 and CMCF 2) • Description: The scientific goal of the 08ID-1 beamline is to operate a protein crystallography beamline suitable for studying small crystals and crystals with large unit cells. 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  49. Canadian Light SourceHard X-ray Diffraction Capabilities • Very Sensitive Elemental and Structural Probe Employing Radiation from a Synchrotron (VESPERS) • Description: VESPER is a hard x-ray microprobe capable of providing a high level of complementary structural and analytical information. The techniques of x-ray diffraction and x-ray fluorescence spectroscopy are employed to analyze a microscopic volume in the sample. Multi-bandpass and pink beam capability are built in to meet variable requirements. • Techniques: • X-ray Laue Diffraction • X-ray Fluorescence Spectroscopy • X-ray Absorption Near Edge Structure • Differential Aperture X-ray Microscopy • Multi-bandpass and pink beam capability 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

  50. Canadian Light SourceHard X-ray Diffraction Capabilities • Synchrotron Laboratory for Micro And Nano Devices (SyLMAND) • Description: SyLMAND will be dedicated to research in and fabrication of polymer microstructures. The combination with subsequent process steps, such as metallization of the polymer templates, allows a huge variety of micro-electro-mechanical systems (MEMS) applications in fields such as radio frequency MEMS, micromechanics, optics/photonics and biomedical. The SyLMAND facility will consist of a dedicated beamline as well as a process support cleanroom laboratories required to run the individual process steps. • Techniques: • Deep X-ray lithography • LIGA process lithography steps 19-Jun-07 BIMR workshop on characterization of materials with Electrons, Photons and Neutrons

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