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Low-Voltage Electron-Probe Microanalysis of Uranium

Published online by Cambridge University Press:  18 March 2021

Mike B. Matthews ,
Stuart L. Kearns  and
Ben Buse
Mike B. Matthews*
Affiliation:
AWE, Aldermaston, ReadingRG7 4PR, UK School of Earth Sciences, University of Bristol, Wills Memorial Building, Queens Road, CliftonBS8 1RJ, UK
Stuart L. Kearns
Affiliation:
School of Earth Sciences, University of Bristol, Wills Memorial Building, Queens Road, CliftonBS8 1RJ, UK
Ben Buse
Affiliation:
School of Earth Sciences, University of Bristol, Wills Memorial Building, Queens Road, CliftonBS8 1RJ, UK
*
*Author for correspondence: Mike B. Matthews, E-mail: matthm@hotmail.com
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Abstract

Electron-probe microanalysis of uranium and uranium alloys poses several problems, such as rapid oxidation, large poorly constrained correction factors, and a large number of characteristic x-ray lines. We show that U-metal can grow 10 nm of oxide within ~20 s of air exposure, increasing to 15–20 nm within a few minutes, which can produce a 30% quantification error at 5 kV. A 15 nm carbon coating on the UO2 reference material also produces an ~30% quantification error of the uncoated but surface oxidized U sample at 5 kV. Correcting for both the coating and oxide improved the analysis accuracy to better than ±1% down to 7 kV and ~2% at 5 kV, but the error increases strongly below this. The measurement of C in U identified a previously unreported U N6–O4 line interference on the C Kα peak, which can produce over 1% error in the analysis total. Oxide stoichiometry was demonstrated to have only a small impact on quantification. The measurement of the O Kα and U Mα mass absorption coefficients in U as 9,528 and 798 cm2/g, respectively, shows good agreement with recently published values and also produces small differences in a quantification error.

Keywords

carbonEPMAmass absorption coefficienturanium
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 27 , Issue 3 , June 2021 , pp. 466 - 483
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Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

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