Hostname: page-component-586b7cd67f-2plfb Total loading time: 0 Render date: 2024-11-23T14:49:00.870Z Has data issue: false hasContentIssue false

Methods of Quantitative Electron Probe Analysis*

Published online by Cambridge University Press:  06 March 2019

David B. Wittry*
Affiliation:
University of Southern California Los Angeles, California
Get access

Abstract

Methods of quantitative electron probe analysis using empirical working curves have achieved only partial success because of variations in instrument design, analysis conditions, and homogeneity of standards. These problems have been solved for X-ray fluorescence analysis, but many of the more successful empirical methods cannot be used in electron probe analysis; instead, a more theoretical approach is indicated. In electron probe analysis quantitative results can be achieved with only pure elements as standards provided (1) the analysis conditions are carefully selected, (2) the observed intensities can be corrected to obtain the primary intensity actually produced in the specimen, and (3) the relationship of the primary intensity and concentration can be calculated. While present methods of making some of the corrections required improvement and a “universal” theory for relating the primary X-ray intensities to the concentrations still does not exist, the success achieved with this approach indicates that it should be used to the fullest extent before resorting to calibration curves. Moreover, as information is accumulated, the number of cases requiring the use of calibration curves should diminish, so that eventually it may be possible to perform quantitative analysis in any system with only pure elements as standards,

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1963

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.)

Footnotes

*

This work was supported in part by the Air Force Office of Scientific Research under grant No. AF—AFOSR—76—63. Reprinted with permission of the American Society for Testing and Materials, Philadelphia, Pennsylvania, from Symposium on X-ray and Electron Probe Analysis, Special Technical Publication 349. This paper was presented at the 66th Annual Meeting of ASTM.

References

1. Theisen, R. and. Lemaitre, J., “High-Precision Microprobe Analysis by Thin Metallic Film Calibration,” Proc. of the Xth Colloquium Spectroscopicum Internationale, Spartan Books, Washington, 1963, p, 391.Google Scholar
2. Wittry, D. B., Ph.D. Thesis, California Institute of Technology, Pasadena, California, 1957.Google Scholar
3. Wittry, D. B., “Resolution of Electron Probe Microanalyzers,” J. Appi, Phys. 29: 1543, 1958.Google Scholar
4. Wittry, D. B., USCEC Rept. 84-204, University of Southern California, Los Angeles, 1962.Google Scholar
5. Faessler, A., “X-Ray Emission and the Chemical Bond,” Proc. of the Xth Colloquium Spectroscopicum Internationale, Spartan Books, Washington, 1963.Google Scholar
6. Castaing, R. and Descarnps, J., “On the Physical Basis of Localised Analysis by X-Ray Spectrography,” J. phys. radium 16: 304, 1955.Google Scholar
7. Green, M., “The Target Absorption Correction in X-ray Microanalysis,” Third International Symposium on X-ray Optics and X-Ray Microanalysis, Stanford, California, 1962.Google Scholar
8. Castaing, R., Ph.D. Thesis, University of Paris, 1951, Office Nationale d'Etudes et Recherches Aeronautique, Publ. No. 55, Paris, 1951, translated by P. Duwez and D. B. Wittry, Interim Tech. Rept, No. 3, under contract DA-0JM-95-ORD-463, 1955.Google Scholar
9. Philibert, J., “A Method to Calculate the Absorption Correction in Electron Probe Micro - analysis,” Third International Symposium on X-Ray Optics and X-Ray Microanalysis, Stanford, California, 1962.Google Scholar
10. Archard, G. D. and Mulvey, T., “The Effect of Atomic Number in Quantitative X-Ray Microanalysis,” Third International Symposium on X-Ray Optics and X-Ray Microanalysis, Stanford, California, 1962.Google Scholar
11. Castaing, R., “Electron Probe Microanalysis,” Advances in Electronics and Electron Physics, Vol. 13, Academic Press, New York, 1960, p. 317.Google Scholar
12. Duncumb, P. and Shields, P. K., “Calculation of Fluorescence Excited by Characteristic Radiation in the X-Ray Microanalyzer,” Third International Symposium on X-Ray Optics and X-Ray Microanalysis, Stanford, California, 1962.Google Scholar
13. Birks, L. S., “Calculation of X-Ray Intensities from Electron Probe Specimens,“J. Appl. Phys. 32: 387, 1961; see also Spectrochim. Acta 17: 148, 1961.Google Scholar
14. Henoc, J., Thesis, University of Paris, 1962; publication C.N.E.T. No. 655, P.C.M., Paris.Google Scholar
15. Green, M. and Cosslett, V. E., “The Efficiency of Production of Characteristic X-Radiation in Thick Targets of a Pure Element,” Proc. Phys, Soc. (London) 78: 1206, 1961.Google Scholar
16. Castaing, R. in Advances in X-Ray Analysis, Vol. 4, University of Denver, Plenum Press, New York, 1961, p. 351.Google Scholar
17. Wittry, D. B., “Metallurgical Applications of the Electron Probe Microanalyzer,” Advances in X-Ray Analysis, Vol. 3, University of Denver, Plenum Press, New York, 1960, p. 197.Google Scholar
18. Dills, R. and Zeitz, L., “A Suggested Correction for Secondary Fluorescence in Electron Probe Analysis in a Region of Steep Concentration Gradient,” Third International Symposium on X-Ray Optics and X-Ray Microanalysis, Stanford, California, 1962.Google Scholar
19. Poole, D. M. and Thomas, P. M., “Quantitative Electron-Probe Microanalysis,“J. Inst, Metals 90: 228, 1962; see also “Corrections for Atomic Number Effects in Microprobe Analysis,” Third International Symposium on X-Ray Optics and X-Ray Microanalysis, Stanford, California, 1962.Google Scholar
20. Nelms, A. T., “Energy Loss and Range of Electrons and Positrons,” U.S. Nat. Bur. Standards Circ. No. 577, 1956.Google Scholar
21. Bethe, H. A., “Theory of the Passage of Rapid Corpuscular Rays Through Matter,” Ann. Physics, 5: 325, 1930.Google Scholar
22. Mott, N. F. and Massey, H. S. W., Theory of Atomic Collisions, Clarendon Press, Oxford, 1949.Google Scholar
23. Everhart, T. E., “Simple Theory Concerning the Reflection of Electrons from Solids,” J. Appl. Phys. 31: 1483, 1960.Google Scholar
24. Archard, G. D. “Back Scattering of Electrons,“J. Appl. Phys. 32: 1505, 1961.Google Scholar
25. Kirianenko, A., Maurice, F., Calais, D., and Adda, Y., “L'Analyse des Elements Lourds (Z>80) au Moyen de la ‘Microsonde de Castaing’,” Third International Symposium on X-Ray Optics and X-Ray Microanalysis, Stanford, California, 1962.80)+au+Moyen+de+la+‘Microsonde+de+Castaing’,”+Third+International+Symposium+on+X-Ray+Optics+and+X-Ray+Microanalysis,+Stanford,+California,+1962.>Google Scholar
26. Ziebold, T. O. and Ogilvie, R. E., “Quantitative Analysis with the Electron Beam Microanalyzer,” Eastern Analytical Symposium, New York City, 1962.Google Scholar
27. Clayton, D. B., Brit. J. Appl. Phys. 14: 117, 1963.Google Scholar