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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. [email protected]
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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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References

Bastin, G. & Heijligers, H. (1991). Quantitative electron probe microanalysis of ultralight elements (boron-oxygen). In Electron Probe Quantitation, Heinrich K. & Newbury D. (Eds.), pp. 163–175. New York, NY: Plenum.Google Scholar
Castaing, R. (1951). Application of electron probes to metallographic analysis. PhD Dissertation, University of Paris.Google Scholar
Chantler, C.T.J. (2005). Detailed Tabulation of Atomic Form Factors, Photoelectric Absorption and Scattering Cross Section, and Mass Attenuation Coefficients in the Vicinity of Absorption Edges in the Soft X-Ray (Z=30 -36, Z=60 -89, E=0.1 keV -10 keV), Addressing Convergence Issues of Earlier Work. Phys Chem Ref Data 2000 29(4), 597–1048. Available online as: (b) Chantler, C. T.; Olsen, K.; Dragoset, R. A.; Chang, J.; Kishore, A. R.; Kotochigova, S. A.; Zucker, D. S. X-Ray Form Factor, Attenuation and Scattering Tables, version 2.1 [Online]; National Institute of Standards and Technology, Gaithersburg, MD, 2005. http://physics.nist.gov/ffast.Google Scholar
Fiori, C.E., Myklebust, R.L., Heinrich, K.F.J. & Yakowitz, H. (1976). Prediction of continuum intensity in energy-dispersive X-ray microanalysis. Anal Chem 48, 172–176.Google Scholar
Fitzgerald, R., Keil, K. & Heinrich, K.F.J. (1968). Solid-state energy-dispersion spectrometer for electron-microprobe X-ray analysis. Science 528, 159–160.Google Scholar
Goldstein, J., Newbury, D., Joy, D., Lyman, C., Echlin, P., Lifshin, E., Sawyer, L. & Michael, J. (2003). Scanning Electron Microscopy and X-Ray Microanalysis, 3rd ed. New York, NY: Springer.CrossRefGoogle Scholar
ISO Gum (2008). Guide to the Expression of Uncertainty in Measurement; Guide 98-3:2008: Geneva , Switzerland, Joint Group for Guides in Metrology, Working Group 1. ISO Central Secretariat, Vernier, Geneva, Switzerland: International Organization for Standards.Google Scholar
Myklebust, R., Fiori, C. & Heinrich, K. (1979). Frame C: A Compact Procedure for Quantitative Energy-Dispersive Electron Probe X-Ray Analysis, Technical Note 1106. Washington, DC, USA: National Bureau of Standards.Google Scholar
Newbury, D.E. & Ritchie, N.W.M. (2015). Review: Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy dispersive X-ray spectrometry (SEM/SDD-EDS). J Mater Sci 50, 493–518.Google Scholar
Pouchou, J.-L. & Pichoir, F. (1995). Quantitative analysis of homogeneous or stratified microvolumes applying the model “PAP”. In Electron Probe Quantitation, Heinrich. K.F.J., Newbury. D.E. (Eds.), pp. 31–75. New York, NY: Plenum.Google Scholar
Reed, S.J.B. & Ware, N.G. (1973). Quantitative electron microprobe analysis using a lithium drifted silicon detector. X-Ray Spectrom 2, 69–74.Google Scholar
Ritchie, N.W.M. (2015). NIST DTSA-II software, including tutorials. Available at www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html (retrieved April 17, 2015).Google Scholar
Ritchie, N.W.M. & Newbury, D.E. (2012). Uncertainty estimates for electron probe X-ray microanalysis measurements. Anal Chem 84, 9956–9962.Google Scholar
Schamber, F.C. (1973). A new technique for deconvolution of complex X-ray energy spectra. Proceedings of the 8th National Conference on Electron Probe Analysis, Electron Probe Analysis Society of America, New Orleans, paper 85.Google Scholar
Struder, L., Fiorini, C., Gatti, E., Hartmann, R., Holl, P., Krause, N., Lechner, P., Longoni, A., Lutz, G., Kemmer, J., Meidinger, N., Popp, M., Soltau, H. & van Zanthier, C. (1998). High resolution non dispersive X-ray spectroscopy with state of the art silicon detectors. Mikrochim Acta 15(Suppl), 11–19.Google Scholar