Hostname: page-component-76fb5796d-dfsvx Total loading time: 0 Render date: 2024-04-26T07:27:25.677Z Has data issue: false hasContentIssue false
  • English
  • Français

Microdiffraction phase identification in the scanning electron microscope (SEM)

Published online by Cambridge University Press:  06 March 2012

R. P. Goehner  and
J. R. Michael
R. P. Goehner
Affiliation:
Materials Characterization, Sandia National Laboratories, Albuquerque, New Mexico 87185-1405
J. R. Michael
Affiliation:
Materials Characterization, Sandia National Laboratories, Albuquerque, New Mexico 87185-1405
Get access Rights & Permissions [Opens in a new window]

Abstract

The identification of crystallographic phases in the scanning electron microscope (SEM) has been limited by the lack of a simple way to obtain electron diffraction data of an unknown while observing the microstructure of the specimen. With the development of charge coupled device (CCD)-based detectors, backscattered electron Kikuchi patterns, alternately referred to as electron backscattered diffraction (EBSD) patterns, can be easily collected. Previously, EBSD has been limited to crystallographic orientation studies due to the poor pattern quality collected with video rate detector systems. With CCD detectors, a typical EBSD can now be acquired from a micron or submicron sized crystal using an exposure time of 1–10 s with an accelerating voltage of 10–40 kV and a beam current as low as 0.1 nA. Crystallographic phase analysis using EBSD is unique in that the properly equipped SEM permits high magnification images, EBSDs, and elemental information to be collected from bulk specimens. EBSD in the SEM has numerous advantages over other electron beam-based crystallographic techniques. The large angular view (∼70°) provided by EBSD and the ease of specimen preparation are distinct advantages of the technique. No sample preparation beyond what is commonly used for SEM specimens is required for EBSD.

Type
Special Section on Microanalysis
Information
Powder Diffraction , Volume 19 , Issue 2 , June 2004 , pp. 100 - 103
Copyright
Copyright © Cambridge University Press 2004

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Alam, M. N., Blackman, M., and Pashley, D. W. (1954). “High-angle Kikuchi Patterns,” Proc. R. Soc. ZZZZZZ 221, 224.Google Scholar
Baba-Kishi, K. J. (1991a). “A study of the breakdown of Friedel’s law in electron backscatter Kikuchi diffraction patterns: Application to the zincblende-type structures,” J. Appl. Crystallogr. JACGAR 24, 38. acr, JACGAR CrossRefGoogle Scholar
Baba-Kishi, K. J. (1991b). “Use of Kikuchi line intersections in crystal symmetry determination: application to chalcopyrite structure,” Ultramicroscopy ULTRD6 36, 355. ult, ULTRD6 CrossRefGoogle Scholar
Baba-Kishi, K. J.and Dingley, D. J. (1989). “Application of backscatter Kikuchi diffraction in the scanning electron microscope to the study of NiS2,” J. Appl. Crystallogr. JACGAR 22, 89. acr, JACGAR CrossRefGoogle Scholar
Dingley, D. J. (1981). “A Comparison of Diffraction Techniques for the SEM,” SEMI/II, 383.Google Scholar
Dingley, D. J. and Baba-Kishi, K. Z. (1986). “Use of backscattered electron diffraction patterns for determination of crystal symmetry elements,” in Scanning Electron Microscopy, edited by O. Johari (SEM, Chicago), Vol. II, p. 383.Google Scholar
Dingley, D. J., MacKenzie, R., and Baba-Kishi, K. Z. (1989). “Application of backscatter Kikuchi diffraction for phase identification and crystal orientation measurement in materials,” in Scanning Electron Microscopy, edited by O. Johari (SEM Chicago), Vol. II, p. 305.Google Scholar
Goehner, R. P.and Michael, J. R. (1995). “Applied Crystallography In The SEM Using A CCD Detector,” Adv. X-ray Anal. AXRAAA 38, 539. axr, AXRAAA Google Scholar
Goehner, R. P.and Michael, J. R. (1996). “Phase Identification in a Scanning Electron Microscope Using Backscattered Electron Kikuchi Patterns,” J. Res. Natl. Inst. Stand. Technol. JRITEF 101, 301. jri, JRITEF CrossRefGoogle Scholar
Goehner, R. P., Michael, J. R., Hills, C. R., and Carr, M. J. (1992). “Analysis of SEM Electron Backscattered Kikuchi Patterns Using a CCD Detector and a Macintosh Computer,” Proc. 50th Annual Meeting of EMSA, pp. 1310–1311.Google Scholar
Michael, J. R. and Goehner, R. P. (1993a). “Crystallographic Phase Identification in the Scanning Electron Microscope: Backscattered Electron Kikuchi Patterns Imaged with a CCD-Based Detector,” MSA Bulletin ISSN:1062-9785, Microscopy Society of America, Vol. 23(2), pp. 168–175.Google Scholar
Michael, J. R. and Goehner, R. P. (1993b). “Crystallographic Phase Identification In The Scanning Electron Microscope: Backscattered Electron Kikuchi Patterns,” in Proceedings 51st Annual Meeting of the Microscopy Society of America, pp. 772–773.CrossRefGoogle Scholar
Michael, J. R. and Goehner, R. P. (1994). “Advances In Backscattered-Electron Kikuchi Patterns For Crystallographic Phase Identification,” in Proc. 52nd Annual Meeting of the Microscopy Society of America, pp. 596–597.Google Scholar
Michael, J. R. and Goehner, R. P. (1996). “Development Of Backscattered Electron Kikuchi Patterns For Phase Identification In The SEM,” in Developments in Materials Characterization Technologies, ASM International, pp. 63–70.Google Scholar
Powder Diffraction File (PDF), International Centre for Diffraction Data, 12 Campus Boulevard, Newtown Square, PA.Google Scholar
Small, J. A.and Michael, J. R. (2001). “Phase identification of individual crystalline particles by electron backscatter diffraction,” J. Microsc. JMICAR 201, 59. jmi, JMICAR CrossRefGoogle ScholarPubMed
Small, J. A., Michael, J. R., and Bright, D. S. (2002). “Improving the quality of electron backscatter diffraction (EBSD) patterns from nanoparticles,” J. Microsc. JMICAR 206, 170. jmi, JMICAR CrossRefGoogle ScholarPubMed
Wright, S. J.and Adams, B. L. (1992). “Automatic Analysis of Electron Backscattered Diffraction Patterns,” Metall. Trans. A MTTABN 23A, 759. mta, MTTABN CrossRefGoogle Scholar