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Quantitative Electron-Excited X-Ray Microanalysis of Borides, Carbides, Nitrides, Oxides, and Fluorides with Scanning Electron Microscopy/Silicon Drift Detector Energy-Dispersive Spectrometry (SEM/SDD-EDS) and NIST DTSA-II

Published online by Cambridge University Press:  14 September 2015

Dale E. Newbury  and
Nicholas W. M. Ritchie
Dale E. Newbury*
Affiliation:
National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
Nicholas W. M. Ritchie
Affiliation:
National Institute of Standards and Technology, Gaithersburg, MD 20899, USA
*
*Corresponding author. dale.newbury@nist.gov
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Abstract

A scanning electron microscope with a silicon drift detector energy-dispersive X-ray spectrometer (SEM/SDD-EDS) was used to analyze materials containing the low atomic number elements B, C, N, O, and F achieving a high degree of accuracy. Nearly all results fell well within an uncertainty envelope of ±5% relative (where relative uncertainty (%)=[(measured−ideal)/ideal]×100%). Quantification was performed with the standards-based “k-ratio” method with matrix corrections calculated based on the Pouchou and Pichoir expression for the ionization depth distribution function, as implemented in the NIST DTSA-II EDS software platform. The analytical strategy that was followed involved collection of high count (>2.5 million counts from 100 eV to the incident beam energy) spectra measured with a conservative input count rate that restricted the deadtime to ~10% to minimize coincidence effects. Standards employed included pure elements and simple compounds. A 10 keV beam was employed to excite the K- and L-shell X-rays of intermediate and high atomic number elements with excitation energies above 3 keV, e.g., the Fe K-family, while a 5 keV beam was used for analyses of elements with excitation energies below 3 keV, e.g., the Mo L-family.

Keywords

energy-dispersive X-ray spectrometryscanning electron microscopyquantitative X-ray microanalysislow atomic number elements
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 21 , Issue 5 , October 2015 , pp. 1327 - 1340
Copyright
© Microscopy Society of America 2015 

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