Hostname: page-component-8448b6f56d-sxzjt Total loading time: 0 Render date: 2024-04-23T16:01:40.644Z Has data issue: false hasContentIssue false

Homogeneity Characterization of NBS Spectrometric Standards IV: Preparation and Microprobe Characterization of W-20% Mo Alloy Fabricated by Powder Metallurgical Methods

Published online by Cambridge University Press:  06 March 2019

H. Yakowitz
Affiliation:
National Bureau of Standards, Washington, D. C. 20234
R. E. Michaelis
Affiliation:
National Bureau of Standards, Washington, D. C. 20234
D. L. Vieth
Affiliation:
National Bureau of Standards, Washington, D. C. 20234
Get access

Abstract

A significant problem of the National Bureau of Standards Standard Reference Materials program is the provision of standards suitable in homogeneity for use with microanalytical techniques such as the spark source mass spectrograph and the electron probe microanalyser. An interim approach to the problem has been the extended homogeneity characterization of selected existing standards. This paper describes the preparation and evaluation of the first NBS standard tested specifically from the beginning for application to electron probe microanalysers. The standard designated SRM 480 is a tungsten-20 weight percent molybdenum alloy prepared by a powder metallurgy process. Based on the results of about 1500 determinations for both tungsten and molybdenum by electron probe microanalysis, the material was found to be of high homogeneity at about the micrometer leve 1 of spatial re so lution. The coefficient of variation for molybdenum was 2.5% and that for tungsten 1.5%. Correction of relative intensity ratios to obtain concentrations is discussed in terms of input parameter uncertainties such as mass absorption coefficients, and electron backscatter factors. The result of studies for atomic number correction and effects on operating voltage on the microprobe absorption correction, will be given. It is concluded that SRM 480 should be a valuable addition to any microprobe laboratory doing quantitative analyses.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1968

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

1. Yakowitz, H., Vieth, D. L. and Michaeiis, R. E., “Homogeneity Characterization of NBS Spectrometrie Standards III: White Cast Iron and Stainless Steel Powder Compact”, MBS Misc. Publ. 260-12, 13pp (1966).Google Scholar
2. Castaing, R., “Application of Electron Probes to Local Chemical and Crystallographic Analysis”, Thesis, University of Paris, 1951.Google Scholar
3. Duncumb, P. and Shields, P. K., “Calculation of Fluorescence Excited by Characteristic Radiation, in the X-Ray Microanalyzer”, in X-Ray Optics and X-Ray Microanalysis, (H. H. Pattee, V. E. Cosslett and A. Engström, eds) Academic Press, New York (1963) p. 329.Google Scholar
4. Duncumb, P. and Reed, S. J. B., “Progress in the Calculation of Stopping Power and Backscatter Effects”, in Quantitative Electron Probe Microanalysis, (K. F. J. Heinrich, ed) National Bureau of Standards Special Publication 289 (1968) p. 133.Google Scholar
5. Yakowitz, H. and Heinrich, K. F. J., “Quantitative Electron Probe Microanalysis: Absorption Correction Uncertainty”, Mikrochimica Acta 1968(1), 182.Google Scholar
6. Heinrich, K. F. J., “Common Sources of Error in Electron Probe Microanalysis”, Advances in X-Ray Analysis 11, Plenum Press, New York 1968 - in press.Google Scholar
7. Hansen, M., Constitution of Binary Alloys (second ed), McGraw-Hill Book Co., New York 1958, p. 980.Google Scholar
8. Kehl, G. L., Principles of Metallographic Laboratory Practice (third ed) McGraw-Hill Book Co., New York, 1949.Google Scholar
9. Heinrich, K. F. J., “Scanning Electron Probe Microanalysis”, ASIM-STP 430, 315 (1968).Google Scholar
10. Heinrich, K. F. J., Vieth, D. L. and Yakowitz, H., “Correction for Non-Linearity of Proportional Counter Systems in Electron Probe X-ray Microanalysis”, Advances in X-ray Analysis, 9, Plenum Press, New York, 1966, p. 208.Google Scholar
11. Heinrich, K. F. J. and Rasberry, S. D., “MULTI6”. This is a computer program in the BASIC language which corrects electron microprobe data. Available from K. F. J. Heinrich, National Bureau of Standards, Washington, D. C. 20234.Google Scholar
12. Philibert, J., “A Method for Calculating the Absorption Correction in Electron-Probe Microanalysis”, in X-Ray Optics and X-Ray Microanalysis (H. H. Pattee, V. E. Cosslett and A. Engstrom, eds) Academic Press, New York (1963) p. 379.Google Scholar
13. Duncumb, P. and Shields, P. K., “Effect of Critical Excitation Potential on the Absorption Correction”, in The Electron Microprobe, (T. D. McKinely, K. F. J. Heinrich and D. B. Wittry, eds) John Wiley and Sons, New York, 1966, p. 284.Google Scholar
14. Thomas, P. M., “A Method for Correcting for Atomic Number Effects in Electron Probe Microanalysis”, U. K. Atomic Energy Authority Report AERE-R 4593, 16pp (1964).Google Scholar
15. Heinrich, K. F. J. and Yakowitz, H., “Quantitative Electron Probe Microanalysis; Atomic Number Correction Uncertainty” - to be published.Google Scholar
16. Criss, J. W. and Birks, L. S., “Intensity Formulae for Computer Solution of Multicomponent Electron Probe Specimens”, in The Electron Microprobe (T. D. McKinley, K. F. J. Heinrich and D. B. Wittry, eds) John Wiley and Sons, New York, 1966, p. 217.Google Scholar
17. Dewey, R. D., “A Study of X-Ray Mass Absorption Coefficients with Tables of Coefficients”, Reynolds Metals Co. Report 36-XMD-210, 34pp (1967).Google Scholar
18. Frazer, J. D., “A Computer Fit to Mass Absorption Coefficient Data”, Institute for the Study of Matter, University of California, La Jolla Rep't. S.I.O. 67-29, 19pp (1967).Google Scholar
19. Heinrich, K. F. J., ‘!X-Ray Absorption Uncertainty”, in The Electron Microprobe (T. D. McKinley, K. F. J. Heinrich and D. B. Wittry, eds) John Wiley and Sons, New York, 1966, p. 296.Google Scholar
20. Springer, G., “The Loss of X-Ray Intensity due to Backscattering of Electrons in Microanalyzer Targets”, Mikrochimica Acta 1966(3) 587.Google Scholar
21. Caldwell, D. O.,“Range-Energy Relation and Masses of the New Particles ” Phys. Rev. 100, 291 (1955).Google Scholar