1148 Susumu Imashuku et al.
luminescence colors of nonmetallic inclusions. It should, how- ever, be noted that detection of nonmetallic inclusions which do notemit lightisdifficult for both the XEOL analyzer and the portable EPMA–CL analyzer in the present circumstances.
CONCLUSIONS
We have demonstrated that we can identify MgAl2O4 spinel and Al2O3 particles in air by capturing the XEOL image of a model sample containing MgAl2O4 spinel and Al2O3 parti- cles in the size range from 20 to 50 μm. The X-ray intensity, irradiated from an X-ray tube of a few watts in power, was not sufficient to detect the luminescence of the particles below 30 μm in the model sample. All of the particles could be detected when using an X-ray tube with a few kW in power. Thus, XEOL analysis has potential in the on-line analysis of nonmetallic inclusions in steel if the luminescence colors of the nonmetallic inclusions are known. Thus, the acquisition of luminescence spectra of the nonmetallic inclusions is required to apply XEOL analysis to the practical on-line analysis of these inclusions, but the present study is important with respect to the fact that we first demonstrated that the major nonmetallic inclusions, MgAl2O4 spinel and Al2O3, can be distinguished by XEOL analysis. We also showed that our portable CL spectrometer can identify MgAl2O4 spinel and Al2O3 particles in the same model sample and that our portable EPMA can distinguish between MgAl2O4 spinel and Al2O3 particles whose luminescent colors were detected by the portable CL spectrometer. The beam current of the portable CL spectrometer was not sufficient to detect the luminescence of all the particles in the model sample. We propose that a beam current sufficient to detect the luminescence of particles with sizes above a dozen micrometers would be able to be obtained by optimizing the heating temperature and cooking rate of the LiTaO3 crystal. It would be, therefore, possible to carry out on-site analysis for screening the inclusions using the portable EPMA–CL before precise analysis without knowledge of luminescence colors of the nonmetallic inclusions. These two analyzers of XEOL and EPMA–CL will contribute to the improvement of productivity of steel because they would drastically reduce time for the analysis. We must note that only nonmetallic inclusions producing luminescence can be detected using the present XEOL analyzer and portable EPMA–CL analyzer.
ACKNOWLEDGMENTS
Financial support for the present study was provided by JSPS KAKENHI Grant Number 17H03435 for XEOL analysis and JFE 21st Century Foundation for analysis using the portable CL spectrometer and EPMA.
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.
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.
BELK, J.A. (1963). Inclusion counting methods: The flying spot microscope. J Iron Steel Inst Special Report 77, 25.
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.
BROWNRIDGE, J.D. (1992). PyroelectricX-ray generator. Nature 358,287. 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.
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.
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.
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.
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.
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.
IMASHUKU, S., FUYUNO, N.,HANASAKI,K.&KAWAI, J. (2013a). Portable rare-earth element analyzer using pyroelectric crystal. Rev Sci Instrum 84, 126105.
IMASHUKU, S., IMANISH,A.&KAWAI, J. (2011). Development of miniaturized electron probe X-ray microanalyzer. Anal Chem 83, 8363.
IMASHUKU, S., IMANISH,A.&KAWAI, J. (2013b). Focused electron beam in pyroelectric electron probe microanalyzer. Rev Sci Instrum 84, 073111.
IMASHUKU,S.,KAWAI,J.&WAGATSUMA,K. (2016).Methods to distinguish rare-earth magnets using portable cathodoluminescence spectrometer. Sur Interface Anal 48, 1153–1156.
IMASHUKU, S., OHTANI,I.&KAWAI, J. (2014). Portable analyzer using pyroelectric crystal. J Iron Steel Inst Jpn 100, 905–910.
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.
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.
IMASHUKU,S.&WAGATSUMA, K. (2017). Portable pyroelectric electron probe microanalyzer with a spot size of 40 μm. Rev Sci Instrum 88, 023117.
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.
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.
Page 1 |
Page 2 |
Page 3 |
Page 4 |
Page 5 |
Page 6 |
Page 7 |
Page 8 |
Page 9 |
Page 10 |
Page 11 |
Page 12 |
Page 13 |
Page 14 |
Page 15 |
Page 16 |
Page 17 |
Page 18 |
Page 19 |
Page 20 |
Page 21 |
Page 22 |
Page 23 |
Page 24 |
Page 25 |
Page 26 |
Page 27 |
Page 28 |
Page 29 |
Page 30 |
Page 31 |
Page 32 |
Page 33 |
Page 34 |
Page 35 |
Page 36 |
Page 37 |
Page 38 |
Page 39 |
Page 40 |
Page 41 |
Page 42 |
Page 43 |
Page 44 |
Page 45 |
Page 46 |
Page 47 |
Page 48 |
Page 49 |
Page 50 |
Page 51 |
Page 52 |
Page 53 |
Page 54 |
Page 55 |
Page 56 |
Page 57 |
Page 58 |
Page 59 |
Page 60 |
Page 61 |
Page 62 |
Page 63 |
Page 64 |
Page 65 |
Page 66 |
Page 67 |
Page 68 |
Page 69 |
Page 70 |
Page 71 |
Page 72 |
Page 73 |
Page 74 |
Page 75 |
Page 76 |
Page 77 |
Page 78 |
Page 79 |
Page 80 |
Page 81 |
Page 82 |
Page 83 |
Page 84 |
Page 85 |
Page 86 |
Page 87 |
Page 88 |
Page 89 |
Page 90 |
Page 91 |
Page 92 |
Page 93 |
Page 94 |
Page 95 |
Page 96 |
Page 97 |
Page 98 |
Page 99 |
Page 100 |
Page 101 |
Page 102 |
Page 103 |
Page 104 |
Page 105 |
Page 106 |
Page 107 |
Page 108 |
Page 109 |
Page 110 |
Page 111 |
Page 112 |
Page 113 |
Page 114 |
Page 115 |
Page 116 |
Page 117 |
Page 118 |
Page 119 |
Page 120 |
Page 121 |
Page 122 |
Page 123 |
Page 124 |
Page 125 |
Page 126 |
Page 127 |
Page 128 |
Page 129 |
Page 130 |
Page 131 |
Page 132 |
Page 133 |
Page 134 |
Page 135 |
Page 136 |
Page 137 |
Page 138 |
Page 139 |
Page 140 |
Page 141 |
Page 142 |
Page 143 |
Page 144 |
Page 145 |
Page 146 |
Page 147 |
Page 148 |
Page 149 |
Page 150 |
Page 151 |
Page 152 |
Page 153 |
Page 154 |
Page 155 |
Page 156 |
Page 157 |
Page 158 |
Page 159 |
Page 160 |
Page 161 |
Page 162 |
Page 163 |
Page 164 |
Page 165 |
Page 166 |
Page 167 |
Page 168 |
Page 169 |
Page 170 |
Page 171 |
Page 172 |
Page 173 |
Page 174 |
Page 175 |
Page 176 |
Page 177 |
Page 178 |
Page 179 |
Page 180