Hostname: page-component-78c5997874-8bhkd Total loading time: 0 Render date: 2024-11-16T07:29:14.094Z Has data issue: false hasContentIssue false
  • English
  • Français

Quantitative Determination of Low Contents of Manganese in Steels by EPMA

Published online by Cambridge University Press:  14 March 2019

Daoling Wang  and
Aiqin Sun
Daoling Wang*
Affiliation:
Structure Analysis Division, Testing Center, Institute of Metal Research, Chinese Academy of Science, Shenyang 110016, China
Aiqin Sun
Affiliation:
Structure Analysis Division, Testing Center, Institute of Metal Research, Chinese Academy of Science, Shenyang 110016, China
*
*Author for correspondence: Daoling Wang, E-mail: [email protected]
Get access

Abstract

The fluorescence effect induced by Kβ photons is usually so small that it can be neglected. However, in the Fe–Mn system, omitting Kβ fluorescence correction will lead to the overestimation of the Mn content especially when Mn is the minor alloy element. In this study, the error in the Mn concentration induced by Kβ fluorescence was investigated by both Monte Carlo simulation, using the pyPENELOPE program, and systematic electron probe measurements on the Fe–0.53% Mn alloy standard by the aid of CalcZAF software. It is shown that the error caused by Kβ fluorescence exceeds 4% for the Fe–0.53% Mn alloy. The problem can be overcome by utilizing CalcZAF in which β-line fluorescence has been included, or by employing a similar standard Fe–0.85% Mn for Mn in the absence of β-line fluorescence correction. In addition, a modified calibration curve method, using k-values instead of X-ray intensity as a variable, is presented and used to measure the Mn concentration. The accuracy of this method is as good as or better than that of the conventional matrix correction method. Compared with conventional calibration curve methods, it is time-saving because the k-value is not sensitive to instrument fluctuations and the established curve remains valid for a long period.

Keywords

electron probe microanalysisfluorescence effectk-valueMnmodified calibration curve methodweighted least squares
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 25 , Issue 3 , June 2019 , pp. 625 - 629
Copyright
Copyright © Microscopy Society of America 2019 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Armstrong, JT (1988). Quantitative analysis of silicates and oxide minerals: Comparison of Monte-Carlo, ZAF and Phi-Rho-Z procedures. In Proceedings of the Microbeam Analysis Society, Newbury, DE (Ed.), pp. 239–246. San Francisco: Microbeam Analysis Society.Google Scholar
Armstrong, JT, Donovan, JJ & Carpenter, PC (2013). CALCZAF, TRYZAF and CITZAF: The use of multi-correction-algorithm programs for estimating uncertainties and improving quantitative X-ray analysis of difficult specimens. Microsc Microanal 19(Suppl 2), 812–813.10.1017/S1431927613006053Google Scholar
Bearden, JA (1967). X-Ray Wavelengths and X-Ray Atomic Energy Levels. Washington, DC: NBS Publication: NSRDS-NBS 14, U.S. Government Printing Office.Google Scholar
Donovan, JJ, Singer, JW & Armstrong, JT (2016). A new EPMA method for fast trace element analysis in simple matrices. Am Mineral 101, 1839–1853.Google Scholar
Fonstein, N (2015). Advanced High Strength Sheet Steels: Physical Metallurgy, Design, Processing, and Properties. Cham, Switzerland: Springer International Publishing AG.Google Scholar
Fournier, C, Merlet, C, Dugne, O & Fialin, M (1999). Standardless semi-quantitative analysis with WDS-EPMA. J Anal At Spectrom 14, 381–386.Google Scholar
GB/T 4930 (1993). General Specification of Electron Probe Microanalysis Standard Specimen. Beijing, China: State Bureau of Technology Supervision.Google Scholar
Gilmour, JB (1970). The role of manganese in the formation of proeutectoid ferrite. PhD Thesis. McMaster University, Hamilton, Ontario.Google Scholar
Heinrich, KFJ (1987). Mass absorption coefficients for electron probe microanalysis. In Proceedings of the 11th International Congress of X-ray Optics and Microanalysis, Brown, JD & Packwood, RH (Eds.), pp. 67–119. London, Ontario: University of Western Ontario Press.Google Scholar
Hyk, W & Stojek, Z (2013). Quantifying uncertainty of determination by standard additions and serial dilutions methods taking into account standard uncertainties in both axes. Anal Chem 85, 5933–5939.Google Scholar
ISO 16592 (2012). Microbeam Analysis—Electron Probe Microanalysis—Guidelines for Determining the Carbon Content of Steels Using A Calibration Curve Method. Geneva, Switzerland: International Organization for Standardization.Google Scholar
Jercinovic, MJ & Williams, ML (2005). Analytical perils (and progress) in electron microprobe trace element analysis applied to geochronology: Background acquisition, interferences, and beam irradiation effects. Am Mineral 90, 526–546.Google Scholar
Liu, ZQ, Miyamoto, G, Yang, ZG & Furuhara, T (2013). Direct measurement of carbon enrichment during austenite to ferrite transformation in hypoeutectoid Fe–2Mn–C alloys. Acta Mater 61, 3120–3129.Google Scholar
Llovet, X & Salvat, F (2017). PENEPMA: A Monte Carlo program for the simulation of X-ray emission in electron probe microanalysis. Microsc Microanal 23, 634–646.10.1017/S1431927617000526Google Scholar
Moreno, I, Almagro, JF & Llovet, X (2002). Determination of nitrogen in duplex stainless steels by EPMA. Mikrochim Acta 139, 105–110.10.1007/s006040200047Google Scholar
Reed, SJB (1975). Electron Microprobe Analysis. Cambridge, UK: Cambridge University Press.Google Scholar
Robaut, F, Crisci, A, Durand-Charre, M & Jouanne, D (2006). Practical aspects of carbon content determination in carburized steels by EPMA. Microsc Microanal 12, 331–334.Google Scholar
Salvat, F (2015). PENELOPE-2014: A code system for Monte Carlo simulation of electron and photon transport. OECD/NEA Data Bank, Issy-les-Moulineaux.Google Scholar
Smith, DGW, Reed, SJB & Ware, NG (1974). Kβ/Kα intensity ratios for elements of atomic number 20 to 30. X-Ray Spectrom 3, 149–150.Google Scholar
Taylor, JR (1997). An Introduction to Error Analysis. Sausalito, California: University Science Books.Google Scholar
Toji, Y, Miyamoto, G & Raabe, D (2015). Carbon partitioning during quenching and partitioning heat treatment accompanied by carbide precipitation. Acta Mater 86, 137–147.Google Scholar
Supplementary material: File

Wang and Sun supplementary material

Wang and Sun supplementary material 1

Download Wang and Sun supplementary material(File)
File 50.3 KB