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A Standards-Based Method for Compositional Analysis by Energy Dispersive X-Ray Spectrometry Using Multivariate Statistical Analysis: Application to Multicomponent Alloys

Published online by Cambridge University Press:  08 January 2013

Monika Rathi*
Affiliation:
South Dakota School of Mines & Technology, Rapid City, SD, USA
S.P. Ahrenkiel
Affiliation:
South Dakota School of Mines & Technology, Rapid City, SD, USA
J.J. Carapella
Affiliation:
National Renewable Energy Laboratory, Golden, CO, USA
M.W. Wanlass
Affiliation:
National Renewable Energy Laboratory, Golden, CO, USA
*
*Corresponding author. E-mail: [email protected]
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Abstract

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy–based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

Type
Software, Techniques and Equipment Development
Copyright
Copyright © Microscopy Society of America 2013

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