Abstract:During the scanning analysis of steel sample by laser-induced breakdown spectroscopy (LIBS), MnS inclusions would cause the abnormal signal both for S and Mn at the same time. Moreover, the signal intensity had linear relationship with the inclusion area. According to the above characteristics and the inspection requirements in German standard DIN 50602, a rating method for MnS inclusions by LIBS was proposed. In experimental method, the fitted curves between signal intensity and inclusion area for both S and Mn elements were obtained based on specimen statistics, and the curves were used as calibration curves. Then the field of view with highest total signal intensity of characteristic elements in inclusion was found within the scanning region and used as the field of view with most inclusions. The inclusion area in the field of view was obtained by inversion calculation with the signal intensity of inclusions according to the calibration curve. Finally, the rating grade was calculated according to the relational expression between rating grade and inclusion area. The contrastive analysis of the proposed LIBS method and traditional metallographic method was implemented on 34CrNiMo6 steel specimen for the main shaft of wind generator. The results showed that, when the content of MnS inclusion was low (n<3), the results of Mn obtained by the LIBS method had significant difference with those obtained by the traditional metallographic method. But the results of S were basically consistent for both methods. When the content of MnS inclusion was high(n≥3), the analysis results of S and Mn by the proposed LIBS method were in good agreement with those obtained by the traditional metallographic method. The proposed method could meet the precision requirements of conventional metallographic examination.
[1] Peter L,Sturm V,Noll R.Liquid steel analysis with laser-induced breakdown spectrometry in the vacuum ultraviolet[J].Applied Optics,2003,42(30): 6199-6204. [2] Hubmer G,Kitzberger R,Mörwald K.Application of LIBS to the in-line process control of liquid high-alloy steel under pressure[J].Analytical and Bioanalytical Chemistry,2006,385(2):219-224. [3] Darwiche S,Benrabbah R,Benmansour M,et al.Impurity detection in solid and molten silicon by laser induced breakdown spectroscopy[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2012,74-75:115-118. [4] Dyar M D,Tucker J M,Humphries S,et al.Strategies for Mars remote laser-induced breakdown spectroscopy analysis of sulfur in geological samples[J].Spectrochimica Acta Part B: Atomic Spectroscopy,2011,66(1): 39-56. [5] Lopez-Moreno C,Palanco C S,Laserna J J,et al.Test of a stand-off laser-induced breakdown spectroscopy sensor for the detection of explosive residues on solid surfaces[J].Journal of Analytical Atomic Spectrometry,2006,21(1): 55-60. [6] Gottfried J L,De Lucia J F C,Munson C A,et al.Double-pulse standoff laser-induced breakdown spectroscopy for versatile hazardous materials detection[J].Spectrochimica Acta Part B: Atomic Spectroscopy,2007,62(12): 1405-1411. [7] Moros J,Lorenzo J A,Laserna J J.Standoff detection of explosives: critical comparison for ensuing options on Raman spectroscopy-LIBS sensor fusion[J].Analytical and Bioanalytical Chemistry,2011,400(10): 3353-3365. [8] Bengtson A.Laser induced breakdown spectroscopy compared with conventional plasma optical emission techniques for the analysis of metals-a review of applications and analytical performance[J].Spectrochimica Acta Part B: Atomic Spectroscopy,2017,134: 123-132. [9] Hudson S W,Craparo J,De Saro,et al.Inclusion detection in aluminum alloys via laser-induced breakdown spectroscopy[J].Metall and Mater Trans B,2018,49: 658-665. [10] MatsudaT,Kashiwakura S,Wagatsuma K.Statistical analysis on the distribution of alumina inclusion particles in ferritic stainless steels in laser-induced breakdown spectrometry using 1-kHz Q-switched Nd: YAG laser[J].Microchemical Journal,2020,153: 104400. [11] Cravetchi I V,Taschuk M,Rieger G W,et al.Spectrochemical microanalysis of aluminum alloys by laser-induced breakdown spectroscopy: identification of precipitates[J].Applied Optics,2003,42(30): 6138-6147. [12] Dubuisson C,Cox A G,McLeod C W,et al.Characterization of inclusions in clean steels via laser ablation-ICP mass spectrometry[J].ISIJ International,2004,44(11): 1859-1866. [13] 杨春,贾云海,张勇.激光诱导击穿光谱分析钢中酸不溶铝含量[J].光谱学与光谱分析,2015,35(3): 777-781. YANG Chun,JIA Yunhai,ZHANG Yong.Determination of acid-insoluble aluminum content in steel by laser-induced breakdown spectroscopy[J].Spectroscopy and Spectral Analysis,2015,35(3): 777-781. [14] Fabienne B B.Laser-induced breakdown spectroscopy and multivariate statistics for the rapid identification of oxide inclusions in steel products[J].Spectrochimica Acta Part B: Atomic Spectroscopy,2016,119(1): 25-35. [15] Zhang Y,Jia Y H,Yang C,et al.Characterization of globular oxideinclusion ratings in steel by laser-induced breakdown spectroscopy[J].Frontiers of Physics,2016,11(6): 115205. [16] 杨春,贾云海,王辉,等.硫化锰夹杂物面积与激光诱导击穿光谱信号强度关系的统计分析[J].分析化学,2018,46(2):265-272. YANG Chun,JIA Yunhai,WANG Hui,et al.Statistical analysis of relation of manganese sulfide inclusion area to signal intensity by laser-induced breakdown spectroscopy[J].Chinese Journal of Analytical Chemistry,2018,46(2): 265-272.