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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

  • Monika Rathi (a1), S.P. Ahrenkiel (a1), J.J. Carapella (a2) and M.W. Wanlass (a2)


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.


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Ahrenkiel, S.P., Wanlass, M.W., Carapella, J.J., Gedvilas, L.M., Keyes, B.M., Ahrenkiel, R.K. & Moutinho, H.R. (2007). Optimization of buffer layers for lattice-mismatched epitaxy of Ga x In1−x As/InAs y P1−y double-heterostructures on InP. Sol Energy Mater Sol Cells 91, 908918.
Bakhori, S.K.M., Raof, N.H.A, Hassan, H.A. & Hassan, Z. (2011). Photoluminescence and XRD crystalline studies of In x Al y Ga1−x -Yn quaternary alloys. IOP Conf Ser: Mater Sci Eng 17, 012006-1–4.
Bender, B.A., Williams, D.B. & Notis, M.R. (1983). Absorption effects in STEM microanalysis of ceremic oxides. J Am Chem Soc 63, 149151.
Burke, M.G., Watanabe, M. & Williams, D.B. (2006). Quantitative characterization of nanoprecipitates in irradiated low-alloy steels: Advances in the application of FEG-STEM quantitative microanalysis to real materials. J Mater Sci 41, 45124522.
Cliff, G. & Lorimer, G.W. (1975). The quantitative analysis of thin specimens. J Microsc 103, 179185.
Dimroth, F. (2006). High efficiency solar cells from III-V compound semiconductors. Phys Stat Sol C 3, 373379.
Goldstein, J., Newbury, D.E., Joy, D.C., Lyman, C.E., Echlin, P., Lifshin, E., Sawyer, L. & Michael, J.R. (2003). Scanning Electron Microscopy and X-Ray Microanalysis, 3rd ed. New York: Springer.
Hubbell, J.H. & Seltzer, S.M. (1996). Tables of X-ray mass attenuation coefficients and mass energy-absorption coefficients from 1 keV to 20 MeV for elements Z = 1 to 92 and 48 additional substances of dosimetric interest. NISTIR 5632. Gaithersburg, MD: National Institute of Standards and Technology.
Keil, K., Fitzgerald, R. & Heinrich, K.F.J. (2009). Celebrating 40 years of energy dispersive X-ray spectrometry in electron probe microanalysis: A historic and nostalgic look back into the beginnings. Microsc Microanal 15, 476483.
King, R.R., Law, D.C., Edmondson, K.M., Fetzer, C.M., Kinsey, G.S., Yoon, H., Sherif, R.A. & Karam, N.H. (2007). 40% efficient metamorphic GaInP/GaInAs/Ge multijunction solar cells. Appl Phys Lett 90, 183516-2.
Malinowski, E.R. (1991). Factor Analysis in Chemistry. New York: Wiley-Interscience Publication.
McCarthy, J., Friel, J. & Camus, P. (2009). Impact of 40 years of technology advances on EDS system performance. Microsc Microanal 15, 484490.
Press, W.H., Flannery, B.P., Teukolsky, S.A. & Vetterling, W.T. (1993). Numerical Recipes in C, 2nd ed. Cambridge, UK: Cambridge University Press.
Ritchie, N.W.M. (2011). Standards-based quantification in DTSA-II—Part I. Microsc Today 19(5), 3036.
Rossouw, C.J. & Maslen, V.M. (1987). Localization and ALCHEMI for zone axis orientations. Ultramicroscopy 21, 277290.
Schamber, F.H. (2009). 35 years of EDS software. Microsc Microanal 15, 491504.
Vurgaftman, I. & Meyer, J.R. (2001). Band parameters for III-V compound semiconductor and their alloys. J Appl Phys 89, 58155875.
Wanlass, M.W., Ahrenkiel, S.P., Ahrenkiel, R.K., Albin, D.S., Carapella, J.J., Duda, A., Geisz, J.F., Kurtz, S. & Moriarty, T. (2005). Lattice-mismatched approaches for high-performance, III-V photovoltaic energy converters. In Photovoltaic Specialists Conference 2005, Conference Record of the Thirty-First IEEE, Florida, pp. 530535.
Watanabe, M. & Williams, D.B. (2006). The quantitative analysis of thin specimens: A review of progress from the Cliff-Lorimer to the new ζ-factor methods. J Microsc 221, 89109.
Williams, D. & Carter, C.B. (2009). Transmission Electron Microscopy, 2nd ed. New York: Springer.


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