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MSE465 : Structural and Chemical Characterization of Materials

Study of the basic structural and chemical characterization techniques that are commonly used in materials science and engineering. X-ray, electron and neutron diffraction, a wide range of spectroscopies, microscopies, and scanning probe methods will be covered. Lectures will be integrated with a laboratory where the techniques will be demonstrated and/or used by the student to study a material. Techniques will be presented in terms of the underlying physics and chemistry.

Prerequisites: MSE 250/220 or equivalent, MSE 242 and MSE 350 suggested

Course Topics:

  1. X-ray production and properties
  2. Crystallography and Diffraction
  3. Lab 1: Safety and operation of x-ray equipment and x-ray adsorption (Miniflex)
  4. Diffraction
  5. Reciprocal Space
  6. Lab 2: Diffraction from bone and refractory metals (Miniflex)
  7. Ewald sphere construction
  8. Structure factor
  9. Diffraction Intensity
  10. Electron Diffraction
  11. Lab 3: Transmission Electron Diffraction (JEOL 4000 FX)
  12. Surface Diffraction and Film growth
  13. Lab 4: Orientation and quality of crystals (RHEED)
  14. Diffraction from real crystals
  15. Electron Microscopy and image contrast
  16. Lab 5: TED/TEM of polycrystalline film
  17. Fourrier Transform methods and diffraction
  18. Scanning electron microscopy
  19. Lab 6: Orientation imaging and Biological imaging in the environmental SEM (Phillips Scope and OIM system and environmental SEM)
  20. Neutron Diffraction
  21. General Concepts of Spectroscopy
  22. Non-radiative spectroscopy: Auger Electron Spectroscopy (AES)
  23. Lab 7: AES (Phi Scanning Auger)
  24. X-ray Photoelectron Spectroscopy (XPS)
  25. Lab 8: XPS (Perkin Elmer XPS system)
  26. Rutherford Backscattering Spectroscopy (RBS)
  27. Lab 9: RBS (Michigan Ion Beam Laboratory)
  28. Secondary Ion Mass Spectroscopy
  29. Radiative spectroscopy: X-ray energy and wavelength dispersive spectroscopies (XEDS/WDS)
  30. Electron Energy Loss Spectroscopy (EELS)
  31. Lab 10: XEDS/EELS (JEOL 2010)
  32. Absorption spectroscopy: Fourrier Transformed Infrared spectroscopy (IR)
  33. Lab 11: FTIR from Natural Silk Fibers (Nicolet FTIR)
  34. Scanning probe microscopies (STM and AFM)
  35. Lab 12: AFM: Crystallites of Dental Enamel (Nanoscope III)

Course Objectives:

  1. To provide students with a foundation in the structural and chemical characterization of materials to prepare them for jobs in industry or research in this field.
  2. To teach students intermediate concepts of diffraction and scattering mechanisms both physically and with a high degree of mathematical sophistication.
  3. To apply concepts from physics, chemistry and mathematics to the underlying mechanisms responsible for the spectroscopic methods presented in the course.
  4. To teach students basic concepts of forensic design to solve real problems in materials characterization.
  5. To teach students, the advantages, limitations and inherent resolution of characterization methods.
  6. To expose the students to the actual characterization technologies used in modern materials analysis via a laboratory component of the course.

Course Outcomes:

The students who successfully pass this course with an A grade will be able to (at a minimum):

  1. Use absorption data to determine the absorption characteristics of materials, and explain the origins of different absorption. processes.
  2. Explain how x-rays, electrons, neutrons, and ions can be produced and what the spectra from these sources would look like.
  3. Calculate the wavelength of electrons and neutrons with proper relativistic corrections.
  4. Derive the Bragg and Laue equations and the Ewald sphere construction.
  5. Describe reciprocal space and its value to their parents.
  6. Demonstrate the calculation of structure factor and explain why this is the Fourrier transform of the unit cell.
  7. Identify and describe the physical origin of the corrections that are needed to calculate the intensity of a diffraction pattern.
  8. Explain the advantages and limitations of electron, x-ray and neutron diffraction.
  9. Use the Ewald sphere construction to describe any of the diffraction experiments that we cover in class.
  10. Explain why reciprocal lattice spots will undergo shape transforms as a result of the shape and size of the sample.
  11. Index zone axis electron diffraction patterns.
  12. Explain the origin and use of Kikuchi bands.
  13. Explain the origin of diffraction contrast, strain contrast, and thickness fringes in a TEM image.
  14. Explain why a '2-beam' condition is used for imaging in the dark field and why a weak beam image is often acquired.
  15. Draw and explain the diffraction patterns that would be observed from amorphous materials.
  16. Explain how real crystals would modify the diffraction from ideal crystals including, strain, temperature, mosaic spread, beam divergence and heterogeneous structure.
  17. Describe how the following instruments work: TEM, SEM, x-ray diffractometer, synchrotron source, solid state, ccd, and proportional detectors, etc.
  18. Describe the mechanisms for energy absorption or evolution in each of the following spectroscopies: AES, XPS, XEDS, EELS, IR, RBS.
  19. Explain what spectroscopy is and what it can do.
  20. Describe the resolution limits of each of the spectroscopies studied and explain what limits it.
  21. Design a strategy for solving materials characterization problems.
  22. Choose the correct combinations of characterization tools to solve particular problems.

Assessment Tools:

  1. Two, in-class, closed-book exams.
  2. Weekly problem sets and/or Laboratory reports.
  3. Project involving the construction of a web page on a selected characterization problem and solution.