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Quantitative X-Ray Microanalysis for the Study of Nanometer-Scale Phases in the Aem

Published online by Cambridge University Press:  21 February 2011

Ian M. Anderson ,
Jim Bentley  and
C. Barry Carter
Ian M. Anderson
Affiliation:
Oak Ridge National Laboratory, Metals and Ceramics Division, P. 0. Box 2008, M. S. 6376, Oak Ridge, TN 37831-6376 University of Minnesota, Department of Chemical Engineering and Materials Science, 421 Washington Ave. S. E., Minneapolis, MN 55455-0132
Jim Bentley
Affiliation:
Oak Ridge National Laboratory, Metals and Ceramics Division, P. 0. Box 2008, M. S. 6376, Oak Ridge, TN 37831-6376
C. Barry Carter
Affiliation:
University of Minnesota, Department of Chemical Engineering and Materials Science, 421 Washington Ave. S. E., Minneapolis, MN 55455-0132
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Abstract

Secondary excitation can be a large source of inaccuracy in quantitative X-ray microanalysis of inhomogeneous specimens in the AEM. The size of the secondary excitation component in the measured X-ray spectrum is sensitive to the geometry of the thin foil specimen. Secondary excitation has been examined in a self-supporting disc specimen of composition NiO-20 wt.% TiO2 which has been partially masked by a gold slot washer. The ratio of the intensities of the characteristic Kα peaks of Ti and Ni in X-ray spectra from a periclase-structured phase, of nominal composition NiO, has been measured to be NTi / NNi ≈ 0.005. There is no apparent Ti L2,3 signal in the corresponding electron energy-loss spectrum. The secondary excitation contribution to the characteristic Ti K≈a-peak from all sources can therefore be no larger than 0.5%. It should be possible to reduce this modest level of secondary excitation still further with a better masking arrangement.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 332: Symposium U – Determining Nanoscale Physical Properties of Materials by Microscopy and Spectroscopy , 1994 , 315
Copyright
Copyright © Materials Research Society 1994

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References

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