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Quantitative Measurement of Iron-Silicides by EPMA Using the Fe Lα and Lβ X-ray Lines: A New Twist to an Old Approach

Published online by Cambridge University Press:  12 April 2019

Aurélien Moy Open the ORCID record for Aurélien Moy [Opens in a new window] ,
John Fournelle  and
Anette von der Handt
Aurélien Moy*
Affiliation:
Department of Geoscience, University of Wisconsin, Madison, WI 53706, USA
John Fournelle
Affiliation:
Department of Geoscience, University of Wisconsin, Madison, WI 53706, USA
Anette von der Handt
Affiliation:
Department of Earth Sciences, University of Minnesota, Minneapolis, MN 55455, USA
*
*Author for correspondence: Aurélien Moy, E-mail: [email protected]
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Abstract

The recent availability of Schottky-type field emission electron microprobes provides incentive to consider analyzing micrometer-sized features. Yet, to quantify sub-micrometer-sized features, the electron interaction volume must be reduced by decreasing accelerating voltage. However, the K lines of the transition elements (e.g., Fe) then cannot be excited, and the L lines must be used. The Fe Lα1,2 line is the most intense of the L series but bonding effects change its atomic parameters because it involves a valence band electron transition. For successful traditional electron probe microanalysis, the mass absorption coefficient (MAC) must be accurately known, but the MAC of Fe Lα1,2 radiation by Fe atoms varies from one Fe-compound to another and is not well known. We show that the conventional method of measuring the MAC by an electron probe cannot be used in close proximity to absorption edges, making its accurate determination impossible. Fortunately, we demonstrate, using a set of Fe–silicide compounds, that it is possible to derive an accurate calibration curve, for a given accelerating voltage and takeoff angle, which can be used to quantify Fe in Fe–silicide compounds. The calibration curve can be applied to any spectrometer without calibration and gives accurate quantification results.

Keywords

EPMAiron silicidelow kVMACsoft X-ray
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 25 , Issue 3 , June 2019 , pp. 664 - 674
Copyright
Copyright © Microscopy Society of America 2019 

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