基于激光诱导击穿光谱技术的生铁中硅锰钛偏析的同步分析

到目前为止, 尚没有适用于大型金属材料试样元素偏析定量检测的有效方法。该研究将新兴的激光诱导击穿光谱(LIBS)技术应用于生铁中Si、Mn、Ti元素偏析的同步检测, 选取Si (288.16 nm)、 Mn (293.31 nm) 和Ti (334.94 nm)作为三种元素的定量分析谱线, 同时选取Fe (263.58 nm, 441.51 nm, 370.79 nm)分别作为三种元素的内标谱线, 使用内标法降低基体效应的影响。定标拟合系数R2分别为0.991 7、0.990 3和0.991 2, 因此证明LIBS适用于对生铁中Si、Mn、Ti元素的准确同步定量检测。随后将取自高炉的铁样切割为两个圆形的铁块, 用空间分辨的LIBS装置对样品表面进行面扫描分析并得出元素分布图, 基于元素分布图识别出Si、Mn、Ti元素的偏析区域并计算最大正偏析度和负偏析度。该研究证明了LIBS用于同步检测生铁中Si、Mn、Ti元素偏析的可行性, 同时也揭示了生铁中合金元素的偏析规律, 有利于加深对凝固过程元素迁移和分布的理解和认识。

Abstract

There has been no effective method for detecting the element segregation of large metallic material samples so far. In this research, the newly emerging laser-induced breakdown spectroscopy (LIBS) was applied to quantitatively analyze the segregation of Si, Mn and Ti in pig iron simultaneously. The spectra lines of Si (288.16 nm), Mn (293.31 nm) and Ti (334.94 nm) were selected as the quantitative analysis spectral lines, while lines of Fe (263.58 nm, 441.51 nm, 370.79 nm) were chosen as the internal calibration lines to reduce the influence of matrix effect. The fitting correlation coefficients (R2) were 0.991 7, 0.990 3, 0.991 2, respectively, which proved the ability of LIBS in measuring the concentration of Si, Mn and Ti correctly and simultaneously. A pig iron sample from blast furnace was cut into two round iron samples, whose surface were analyzed with the help of spatial-resolved LIBS subsequently. The element maps revealed the segregation locations of Si, Mn and Ti. The maximum positive and negative segregation degree of three alloy elements was also calculated based on the analysis results of LIBS. The work in this study demonstrates the capability of LIBS for detecting the segregation of alloy elements in pig iron simultaneously. It also reveals the segregation law of alloy elements in pig iron, which is meaningful for the understanding of alloy elements transfer and distribution during solidification process.

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梅亚光, 程宇心, 程树森, 郝中骐, 郭连波, 李祥友, 曾晓雁. 基于激光诱导击穿光谱技术的生铁中硅锰钛偏析的同步分析[J]. 红外与激光工程, 2018, 47(8): 0806003. Mei Yaguang, Cheng Yuxin, Cheng Shusen, Hao Zhongqi, Guo Lianbo, Li Xiangyou, Zeng Xiaoyan. Simultaneous analysis of Si, Mn and Ti segregation in pig iron by laser-induced breakdown spectroscopy[J]. Infrared and Laser Engineering, 2018, 47(8): 0806003.

基于激光诱导击穿光谱技术的生铁中硅锰钛偏析的同步分析

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