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  • 1. Materials Characterization Lab www.mri.psu.edu/mcl OIM/EBSD Maria Klimkiewicz mxk4@psu.edu 865-3624 July 20, 2005
  • 2. Materials Characterization Lab www.mri.psu.edu/mcl Summer Characterization Open Houses Technique Time Date Location Thermal analysis (TGA, DTA, DSC) 9:45 AM June 8 250 MRL Bldg. Transmission Electron Microscopy (TEM/STEM) 9:45 AM June 15 114 MRI Bldg Scanning electron microscopy (SEM) 9:45 AM June 22 541 Deike Bldg. Analytical SEM 11:00 AM June 22 541 Deike Bldg. X-ray Diffraction (XRD) 9:45 AM June 29 250 MRL Bldg. Dielectric Characterization (25 min lecture only) 9:45 AM July 6 250 MRL bldg. High temperature sintering lab (20 min lecture only) 10:15 AM July 6 250 MRL Bldg. Focused Ion Beam (FIB) 9:45 AM July 13 114 MRI Bldg TEM sample preparation 11:00 AM July 13 114 MRI Bldg Orientation imaging microscopy (OIM/EBSD) 9:45 AM July 20 250MRL Bldg. Chemical analysis (ICP, ICP-MS) 9:45 AM July 27 541 Deike Bldg. Atomic Force Microscopy (AFM) 9:45 AM August 3 114 MRI Bldg Small angle x-ray scattering (SAXS) 9:45 AM August 10 541 Deike Bldg. Particle Characterization 9:45 AM August 17 250 MRL X-ray photoelectron spectroscopy (XPS/ESCA) 9:45 AM August 24 114 MRI Bldg Auger Electron Spectroscopy (AES) 11:00 AM August 24 114 MRI Bldg
  • 3. Materials Characterization Lab www.mri.psu.edu/mcl Materials Characterization Lab Locations Bldg Telephone MRL 863-7844 MRI 865-0337 MRI Bldg: Hosler 865-1981 XPS/ESCA, SIMS, E&ES 863-4225 TEM, HR-TEM, FE- Auger, AFM, XRD MRL Bldg: Hosler Bldg: SEM, XRD, OIM, DTA, SEM, ESEM, FE- DSC, TGA, FTIR, Penn Stater SEM, EPMA, ICP, Hotel Raman, AFM, Powder, E&ES Bldg: ICP-MS,BET, SAXS dielectric, prep, shop, SEM IC, UV-Vis Route 322 Steidle Bldg: Atherton Street Nanoindenter (322 Business) I-99 Park Ave. 0 0 0 0 0 0 0 Ave. 0 0 0 0 0 Park 0 Beaver 0 0 Stadium 0 0 0 Centre 0 0 Porter Road Community Univ Shortlidg Hospital 0 0 Burrowes Road ersi ty D e Pollock Road Road rive North Hastin Deike Bldg: gs Ro ad College Ave.
  • 4. Materials Characterization Lab www.mri.psu.edu/mcl Outline ― Introduction to OIM/EBSD ― OIM examples ― how to get started ―OIM resources ― a brief lab tour
  • 5. Materials Characterization Lab www.mri.psu.edu/mcl Introduction to OIM/EBSD
  • 6. Materials Characterization Lab www.mri.psu.edu/mcl OIM/EBSD and Hitachi S-3500N SEM
  • 7. Materials Characterization Lab www.mri.psu.edu/mcl Schematic of OIM/EBSD
  • 8. Materials Characterization Lab www.mri.psu.edu/mcl Bragg’s Law Assumptions: Monochromatic beam Parallel beam http://hyperphysics.phy-astr.gsu.edu/hbase/quantum/bragg.html
  • 9. Materials Characterization Lab www.mri.psu.edu/mcl Electron Backscatter Diffraction in the SEM (EBSD/OIM) 70°
  • 10. Materials Characterization Lab www.mri.psu.edu/mcl Electron Backscatter diffraction pattern The crystal lattice symmetry is reflected in the pattern. The width and intensity of the bands are directly related to the spacing of atoms in the crystal planes. The angles between the bands are directly related to the angles between planes in the crystal lattice
  • 11. Materials Characterization Lab www.mri.psu.edu/mcl Introduction to OIM “indexing” the pattern: Locating the bands . Determine the angles between the bands Comparing the angles to theoretical values Determining the phase
  • 12. Materials Characterization Lab www.mri.psu.edu/mcl Indexed EBSP Indexed EBSP An image processing algorithm (Hough 114 Transform) is used to 013 125 112 detect bands in the 125 323 211 diffraction pattern. The 111 pattern can be indexed by 233 323 comparing the angles 011 between the detected 121 bands to the theoretical 152 look-up-table. Indexing the 251 141 pattern allows the 031 152 crystallographic orientation to be determined TSL/EDAX
  • 13. Materials Characterization Lab www.mri.psu.edu/mcl As the beam is moved from grain to grain the electron backscatter diffraction pattern will change due to the change in the orientation of the crystal lattice in the diffracting volume. TSL/EDAX
  • 14. Materials Characterization Lab www.mri.psu.edu/mcl OIM consists of two parts: • Data Collection- “On Line” • and Analysis-” Off Line”
  • 15. Materials Characterization Lab www.mri.psu.edu/mcl Part one OIM :Data Collection Interactive mode
  • 16. Materials Characterization Lab www.mri.psu.edu/mcl Part one OIM :Data Collection .................... .................... OIM scan: .................... Automatic mode .................... .................... .................... .................... .................... .................... .................... .................... ....................
  • 17. Materials Characterization Lab www.mri.psu.edu/mcl Part two OIM- Analysis Application The stored data (location, orientation, image quality, confidence index, and phase) can be processed to create Orientation Imaging Micrographs
  • 18. Materials Characterization Lab www.mri.psu.edu/mcl Orientation Map Orientation map is generated by shading each point in the OIM scan according to some parameter reflecting the crystallographic rotation. The colors correspond to the crystal orientations as shown in the projection. Crystals with their 111 axis normal to the surface of the sample will be blue, and so on.
  • 19. Materials Characterization Lab www.mri.psu.edu/mcl Image Quality Map • Image Quality (IQ) map is created by analyzing the intensity of the Hough transform peaks for each point in a scan. The white areas indicate good crystallinity and high quality patterns. Dark areas represent areas of poor diffraction, which can be due to a number of factors such as defects, strain, overlapping/poor patterns at grain boundaries, oxidation, poor sample prep, etc.
  • 20. Materials Characterization Lab www.mri.psu.edu/mcl Grain Boundary Map • A Grain boundary Map can be generated by comparing the orientation between each pair of neighboring points in an OIM scan. A line is drawn separating a pair of points if the difference in orientation between the points exceeds a given tolerance angle. TSL/EDAX
  • 21. Materials Characterization Lab www.mri.psu.edu/mcl Maps, from left to right(1)Image Quality,(2) Boundaries defined as>10degree variation between points, (3) Boundaries defined as >1degree variation between points, (4) Boundaries defined as > 0.5degree variation between points TSL/EDAX
  • 22. Materials Characterization Lab www.mri.psu.edu/mcl OIM examples
  • 23. Materials Characterization Lab www.mri.psu.edu/mcl Multiphase identification Amy Stauffer Dept. of Material Science & Engineering
  • 24. Materials Characterization Lab www.mri.psu.edu/mcl Powder containing crystals of : Hematite, Magnetite or Wuestite ? Fe2O3(hematite) Tsubasa Otake
  • 25. Materials Characterization Lab www.mri.psu.edu/mcl Hematite, Magnetite or Wuestite ? FeO (wuestite) Tsubasa Otake
  • 26. Materials Characterization Lab www.mri.psu.edu/mcl Hematite, Magnetite or Wuestite ? No magnetite Tsubasa Otake
  • 27. Materials Characterization Lab www.mri.psu.edu/mcl Multiphase identification Titanium (Alpha) and Titanium (Beta) Amy Stauffer
  • 28. Materials Characterization Lab www.mri.psu.edu/mcl Phase color map and phase fraction Titanium (Alpha) and Titanium (Beta) Amy Stauffer
  • 29. Materials Characterization Lab www.mri.psu.edu/mcl Grain size and misorientation angle plots and charts Titanium (Alpha) and Titanium (Beta) Amy Stauffer
  • 30. Materials Characterization Lab www.mri.psu.edu/mcl Grain size:Titanium (Alpha) and Titanium (Beta)
  • 31. Materials Characterization Lab www.mri.psu.edu/mcl ND TD RD Average Grain Size (by Area) = 1.75 µm Random oriented PMN-32.5 PT, K. Brosnan Dept. of Materials Science & Engineering
  • 32. Materials Characterization Lab www.mri.psu.edu/mcl (Na1/2Bi1/2)TiO3- BaTiO3 (NBT-BT), is a lead free candidate ceramic for a piezoelectric material. The dielectric constant and piezoelectric constant increase as the degree of texture in the ceramic increases. H. Yilmaz
  • 33. Materials Characterization Lab www.mri.psu.edu/mcl Example of texture
  • 34. Materials Characterization Lab www.mri.psu.edu/mcl Strontium Titanium Oxide single crystal H. Yilmaz
  • 35. Materials Characterization Lab www.mri.psu.edu/mcl OIM for Single Crystal Identification OIM used for identification of alpha-alumina crystal morphology produced under glycothermal conditions. R. Kumar MRI
  • 36. Materials Characterization Lab www.mri.psu.edu/mcl Homoepitaxial growth on 6-H SiC single crystal, A. Badzian MRI
  • 37. Materials Characterization Lab www.mri.psu.edu/mcl Sample preparation • Mechanical polishing • Electropolishing • Chemical etching • Ion etching • Conductive Coating
  • 38. Materials Characterization Lab www.mri.psu.edu/mcl Get Started Contact: Maria Klimkiewicz 1. SEM training 2. Sample preparation 3. OIM training
  • 39. Materials Characterization Lab www.mri.psu.edu/mcl OIM resources • OIM users manual • Electron Backscatter Diffraction in Materials Science- book edited by A. J. Schwartz M. Kumar and B. L. Adams • http://www.edax.com/