Hostname: page-component-586b7cd67f-dlnhk Total loading time: 0 Render date: 2024-11-22T19:23:07.669Z Has data issue: false hasContentIssue false
  • English
  • Français

X-Ray Excited Optical Luminescence and Portable Electron Probe Microanalyzer–Cathodoluminescence (EPMA–CL) Analyzers for On-Line and On-Site Analysis of Nonmetallic Inclusions in Steel

Published online by Cambridge University Press:  27 November 2017

Susumu Imashuku ,
Koichiro Ono  and
Kazuaki Wagatsuma
Susumu Imashuku*
Affiliation:
Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan
Koichiro Ono
Affiliation:
Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan
Kazuaki Wagatsuma
Affiliation:
Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan
*
*Corresponding author. [email protected]
Get access

Abstract

The potential of the application of an X-ray excited optical luminescence (XEOL) analyzer and portable analyzers, composed of a cathodoluminescence (CL) spectrometer and electron probe microanalyzer (EPMA), to the on-line and on-site analysis of nonmetallic inclusions in steel is investigated as the first step leading to their practical use. MgAl2O4 spinel and Al2O3 particles were identified by capturing the luminescence as a result of irradiating X-rays in air on a model sample containing MgAl2O4 spinel and Al2O3 particles in the size range from 20 to 50 μm. We were able to identify the MgAl2O4 spinel and Al2O3 particles in the same sample using the portable CL spectrometer. In both cases, not all of the particles in the sample were identified because the luminescence intensities of the smaller Al2O3 in particular were too low to detect. These problems could be solved by using an X-ray tube with a higher power and increasing the beam current of the portable CL spectrometer. The portable EPMA distinguished between the MgAl2O4 spinel and Al2O3 particles whose luminescent colors were detected using the portable CL spectrometer. Therefore, XEOL analysis has potential for the on-line analysis of nonmetallic inclusions in steel if we have information on the luminescence colors of the nonmetallic inclusions. In addition, a portable EPMA–CL analyzer would be able to perform on-site analysis of nonmetallic inclusions in steel.

Keywords

X-ray excited optical luminescencecathodoluminescenceelectron probe microanalyzernonmetallic inclusionon-line and on-site analysis
Type
Instrumentation and Software
Information
Microscopy and Microanalysis , Volume 23 , Issue 6 , December 2017 , pp. 1143 - 1149
Copyright
© Microscopy Society of America 2017 

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

Atkinson, H.V. & Shi, G. (2003). Characterization of inclusions in clean steels: A review including the statistics of extremes methods. Prog Mater Sci 48, 457–520.CrossRefGoogle Scholar
Basu, S., Choudhary, S.K. & Girase, N.U. (2004). Nozzle clogging behaviour of Ti-bearing Al-killed ultra low carbon steel. ISIJ Int 44, 1653–1660.CrossRefGoogle Scholar
Belk, J.A. (1963). Inclusion counting methods: The flying spot microscope. J Iron Steel Inst Special Report 77, 25.Google Scholar
Braun, T.B., Elliott, J.F. & Flemings, C.M. (1979). The clustering of alumina inclusions. Metall Mater Trans B-Proc Metall Mater Proc Sci 10, 171–184.CrossRefGoogle Scholar
Brownridge, J.D. (1992). Pyroelectric X-ray generator. Nature 358, 287.CrossRefGoogle Scholar
Chiba, K., Ono, A., Saeki, M., Ohno, T., Yamauchi, M. & Kanamoto, M. (1991). On-line analysis of molten steel in converter. Anal Sci 7, 655–658.CrossRefGoogle Scholar
Cramb, A.W. (1999). High purity, low residual, and clean steels. In Impurities in Engineering Materials, Briant, J.C.L. (Ed.), pp. 49–90. New York: Marcel Dekker Inc.Google Scholar
Dalby, K.N., Anderson, A.J., Mariano, A.N., Gordon, R.A., Mayanovic, R.A. & Wirth, R. (2010). An investigation of cathodoluminescence in albite from the A-type Georgeville granite, Nova Scotia. Lithos 114, 86–94.CrossRefGoogle Scholar
Goransson, M., Reinholdsson, F. & Willman, K. (1999). Evaluation of liquid steel samples for the determination of microinclusion characteristics by spark–induced optical emission spectroscopy. Iron Steelmak 26, 53–58.Google Scholar
Harada, A., Miyano, G., Maruoka, N., Shibata, H. & Kitamura, S. (2014). Dissolution behavior of Mg from MgO into molten steel deoxidized by Al. ISIJ Int 54, 2230–2238.CrossRefGoogle Scholar
Hemmerlin, M., Meilland, R., Falk, H., Wintjens, P. & Paulard, L. (2001). Application of vacuum ultraviolet laser-induced breakdown spectrometry for steel analysis – Comparison with spark-optical emission spectrometry figures of merit. Spectroc Acta Pt B-Atom Spectr 56, 661–669.CrossRefGoogle Scholar
Imashuku, S., Fuyuno, N., Hanasaki, K. & Kawai, J. (2013a). Portable rare-earth element analyzer using pyroelectric crystal. Rev Sci Instrum 84, 126105.CrossRefGoogle ScholarPubMed
Imashuku, S., Imanish, A. & Kawai, J. (2011). Development of miniaturized electron probe X-ray microanalyzer. Anal Chem 83, 8363.CrossRefGoogle ScholarPubMed
Imashuku, S., Imanish, A. & Kawai, J. (2013b). Focused electron beam in pyroelectric electron probe microanalyzer. Rev Sci Instrum 84, 073111.CrossRefGoogle ScholarPubMed
Imashuku, S., Kawai, J. & Wagatsuma, K. (2016). Methods to distinguish rare-earth magnets using portable cathodoluminescence spectrometer. Sur Interface Anal 48, 1153–1156.CrossRefGoogle Scholar
Imashuku, S., Ohtani, I. & Kawai, J. (2014). Portable analyzer using pyroelectric crystal. J Iron Steel Inst Jpn 100, 905–910.CrossRefGoogle Scholar
Imashuku, S., Ono, K., Shishido, R., Suzuki, S. & Wagatsuma, K. (2017a). Cathodoluminescence analysis for rapid identification of alumina and MgAl2O4 spinel inclusions in steels. Mater Charact 131, 210–216.CrossRefGoogle Scholar
Imashuku, S., Ono, K. & Wagatsuma, K. (2017b). Rapid phase mapping in heat-treated powder mixture of alumina and magnesia utilizing cathodoluminescence. X-Ray Spectrom 46, 131–135.CrossRefGoogle Scholar
Imashuku, S. & Wagatsuma, K. (2017). Portable pyroelectric electron probe microanalyzer with a spot size of 40 μm. Rev Sci Instrum 88, 023117.CrossRefGoogle Scholar
Jin, Y., Liu, Z. & Takata, R. (2010). Nucleation and growth of alumina inclusion in early stages of deoxidation: Numerical modeling. ISIJ Int 50, 371–379.CrossRefGoogle Scholar
Kaushik, P., Pielet, H. & Yin, H. (2009). Inclusion characterization – Tool for measurement of steel cleanliness and process control: Part 2. Ironmak Steelmak 36, 572–582.CrossRefGoogle Scholar
Lobacheva, O., Corcoran, P.L., Murphy, M.W., Ko, J.Y.P. & Sham, T.-K. (2012). Cathodoluminescence, X-ray excited optical luminescence, and X-ray absorption near-edge structure studies of ZnO nanostructures. Can J Chem 90, 298–305.CrossRefGoogle Scholar
Nakajima, T., Kawaguchi, H., Takashima, K. & Ouchi, Y. (1969). Analytical application of X-ray excited optical fluorescence spectra. I. Apparatus and direct determination of rare earths in lanthanum oxide. J Spectosc Soc Jpn 18, 210–217.CrossRefGoogle Scholar
Okuyama, G., Yamaguchi, K., Takeuchi, S. & Sorimachi, K. (2010). Effect of slag composition on the kinetics of formation of Al2O3-MgO inclusions in aluminum killed ferritic stainless steel. ISIJ Int 54, 121–128.Google Scholar
Park, J.H. & Todoroki, H. (2010). Control of MgO·Al2O3 spinel inclusions in stainless steels. ISIJ Int 50, 1333–1346.CrossRefGoogle Scholar
Saitoh, T., Kikuchi, T. & Furuya, K. (1996). Application of laser microprobe mass spectrometry (LAMMS) to a state analysis of nonmetallic Inclusions and precipitates in a Ti-added ultra low carbon steel. ISIJ Int 36(Suppl), S121–S124.CrossRefGoogle Scholar
Tozawa, H., Kato, Y., Sorimachi, K. & Nakanishi, T. (1999). Agglomeration and flotation of alumina clusters in molten steel. ISIJ Int 39, 426–434.CrossRefGoogle Scholar
Yin, H. & Tsai, H.T. (2003). Application of cathodoluminescence microscopy (CLM) in steel research. Proceedings of ISS Tech Conference, Indianapolis. pp. 217–226.Google Scholar
Zhang, L. & Thomas, B.G. (2003). Thomas, state of the art in evaluation and control of steel cleanliness. ISIJ Int 43, 271–291.CrossRefGoogle Scholar
Zheng, L., Malfliet, A., Wollants, P., Blanpain, B. & Guo, M. (2016). Effect of alumina morphology on the clustering of alumina inclusions in molten iron. ISIJ Int 56, 926–935.CrossRefGoogle Scholar