Hostname: page-component-cd9895bd7-q99xh Total loading time: 0 Render date: 2024-12-28T19:41:55.008Z Has data issue: false hasContentIssue false
  • English
  • Français

Quantitative Electron Probe Microanalysis of Nonconducting Specimens: Science or Art?

Published online by Cambridge University Press:  01 December 2004

Guillaume F. Bastin  and
Hans J.M. Heijligers
Guillaume F. Bastin
Affiliation:
Laboratory of Solid State and Materials Chemistry, University of Technology, P.O. Box 513, NL-5600 MB Eindhoven, The Netherlands
Hans J.M. Heijligers
Affiliation:
Laboratory of Solid State and Materials Chemistry, University of Technology, P.O. Box 513, NL-5600 MB Eindhoven, The Netherlands
Get access

Abstract

The influence of a lack of sufficient electrical conductivity on the results of quantitative electron probe microanalysis has been investigated on a number of oxides. The effect of surface charging and the way it alters the emitted X-ray signals has been studied. It is shown that the presence of conducting coatings, such as carbon or copper, will affect the interelement X-ray intensity ratios, whatever the thickness of the coating may be. Although the effects for heavier elements may be acceptable, they cannot be ignored for a light element such as oxygen, where strong variations with coating thickness were observed. Quantitative analyses of oxygen, on uncoated well-conducting oxide specimens, using uncoated well-conducting hematite (Fe2O3) as a standard yielded excellent results in the range between 4 and 40 kV with the φ(ρz) software used. As soon as coated nonconducting specimens were examined, using the same hematite standard, coated under exactly the same conditions, widely scattering and noncoherent results were obtained. These discrepancies can only be attributed to a lack of conductivity.

Keywords

quantitative electron probe microanalysisnonconducting specimensoxidescoatingscopper filmsspecimen charginggarnets
Type
Research Article
Information
Microscopy and Microanalysis , Volume 10 , Issue 6 , December 2004 , pp. 733 - 738
Copyright
© 2004 Microscopy Society of America

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

REFERENCES

Bastin, G.F., Dijkstra, J.M., & Heijligers, H.J.M. (1998). PROZA96: An improved matrix correction program for electron probe microanalysis, based on a double Gaussian φ(ρz) approach. X-ray Spectrom 27, 3–10.Google Scholar
Bastin, G.F., Dijkstra, J.M., Heijligers, H.J.M., & Klepper, D. (1993). In-depth profiling with the electron probe microanalyzer. Microbeam Anal 2, 29–43.Google Scholar
Bastin, G.F. & Heijligers, H.J.M. (1991). Non-conductive specimens in the electron probe microanalyzer—A hitherto poorly discussed problem. In Electron Probe Quantitation, Workshop at the National Bureau of Standards, Gaithersburg, Maryland 1988, Heinrich, K.F.J., & Newbury, D.E (Eds.), pp. 163–175. New York: Plenum Press.
Cazaux, J. (1986). Some considerations on the electric field induced in insulators by electron bombardment. J Appl Phys 59, 1418–1430.Google Scholar
Duane, W. & Hunt, F.L. (1915). On X-ray wavelengths. Phys Rev 6, 166.Google Scholar
Henke, B.L. & Ebisu, E. (1974). Low energy X-ray and electron absorption within solids. Advance in X-ray Anal 17, 150–213.Google Scholar
Henke, B.L., Gullikson, E.M., & Davies, J.C. (1993). X-ray interactions: Photoabsorption, scattering, transmission, and reflection at E = 50–30,000 eV, Z = 1–92. Atomic Data Nucl Data Tables 54, 181–342.Google Scholar
Henke, B.L., Lee, P., Tanaka, J., Shimabukuro, R.L., & Fujikawa, B.K. (1982). Low-energy X-ray interaction coefficients: Photo-absorption, scattering, and reflection. Atomic Data Nucl Data Tables 27, 1–144.Google Scholar
Love, G., Cox, M.G.C., & Scott, V.D. (1974). Electron probe microanalysis using oxygen X-rays: I. Mass absorption coefficients. J Phys D Appl Phys 7, 2131–2141.Google Scholar
Weisweiler, W. (1974). Elektronenstrahl-Mikroanalytik elektrisch nichtleitender Proben leichter Elemente am Beispel von Oxiden. Arch Eisenhüttenwes 45, 287–295.Google Scholar
Weisweiler, W. (1978). Quantitative Analyse von Oxiden mit der Elektonenstrahl-Mikrosonde. Arch Eisenhüttenwes 49, 555–562.Google Scholar