基于远程LIBS技术的镍基高温合金成分分析方法的研究

doi:10.3964/j.issn.1000-0593(2022)02-0603-06

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摘要：基于自行设计搭建的远程激光诱导击穿光谱（LIBS）系统，完成了远程LIBS的聚焦特性分析，并对远程 LIBS技术应用于镍基高温合金成分分析的实验方法进行了研究。该LIBS系统具备激光发射光路和信号采集光路同轴且独立变焦的特点，通过自动聚焦，可实现1~10 m的远程分析。研究表明：受激光聚焦焦深的影响，等离子体光信号可探测范围随系统工作距离的增大而增大，即系统对聚焦精确度的要求降低；同时，烧蚀斑点尺寸增大导致的功率密度减小及信号采集立体角的减小，会使得谱线强度随工作距离的增大成四次方反比关系衰减。分别使用无内标的标准曲线法和有内标的标准曲线法建立了GH4169镍基高温合金中Ni，Cr，Nb，Mo，Ti和Al六种元素的标准曲线，有内标的标准曲线的拟合优度R²（0.999 7，0.999 4，0.998 7，0.999 1，0.998 1和0.999 7）明显优于无内标的标准曲线（0.953 2，0.876 6，0.897 4，0.914 5，0.938 4和0.991 6）。对比了LIBS和X射线荧光光谱（XRF）两种分析技术，对于常量元素Ni，Cr，Nb和Mo，两种方法的相对标准偏差分别在1.74%~3.90%以及0.10%~0.52%，相对误差分别在0.21%~0.92%以及0.64%~2.25%；对于微量元素Ti和Al，两种方法的相对标准偏差分别为5.58%，4.15%以及2.39%，5.64%，相对误差分别为2.75%，2.93%以及4.68%，2.39%。由于激光诱导等离子体的不稳定性、烧蚀样品量少的特点，远程LIBS方法的精密度稍逊于XRF方法，但LIBS方法通过重复多次测量，可以有效减小测量误差，表明LIBS技术应用于镍基高温合金的远程在线分析具有一定的可行性。

关键词：激光诱导击穿光谱；远程；焦深；标准曲线法

Abstract：Based on the self-designed remote laser-induced breakdown spectroscopy (LIBS) system, the focusing characteristics of remote LIBS were analyzed, and the experimental method of quantitative analysis of nickel-base superalloy by remote LIBS was studied. In this LIBS system, the laser focusing and the plasma optical signal acquisition optical paths are coaxial and independently focused. Through automatic focusing, the remote analysis of 1~10 m can be achieved. The results show that affected by the depth of focus, the detectable range of plasma optical signal increases with the increase of working distance. That is, the requirement of the LIBS system for focusing accuracy decreases. At the same time, the decrease of power density caused by the increase of ablation spot size and the decrease of signal acquisition solid angle make the spectral line intensity attenuate in inverse proportion to the fourth power as the working distance increases. In this paper, the standard curves of Ni, Cr, Nb, Mo, Ti and Al in GH4169 nickel-based superalloy were established using the standard curve method without internal standard with internal standard. The goodness of fit of the standard curve with internal standard (0.999 7, 0.999 4, 0.999 87, 0.999 1, 0.998 1 and 0.999 7) was significantly better than that of the standard curve without internal standard (0.953 2, 0.876 6, 0.897 4, 0.914 5, 0.938 4 and 0.991 6). Finally, LIBS and XRF were compared. For major elements Ni, Cr, Nb and Mo, the relative standard deviations of the two methods were 1.75%~3.90% and 0.10%~0.52%, and the relative errors were 0.48%~0.92% and 0.64%~2.25%, respectively; for trace elements Ti and al, the relative standard deviations of the two methods were 5.58%, 5.86% and 2.39%, 5.64%, the relative error is 2.75%, 3.14% and 4.68%, 2.39% respectively. Due to the instability of plasma, the precision of the remote LIBS method is slightly lower than that of the XRF method. However, LIBS method can effectively reduce the measurement error through repeated measurements, which indicates that LIBS technology is feasible for remote on-line analysis of nickel-based superalloys.

Key words：Laser-induced breakdown spectroscopy; Remote; Depth of focus; Standard curve method

收稿日期: 2021-01-06 修订日期: 2021-02-01

中图分类号:

O657.319

基金资助: 国家新材料测试评价平台建设项目（TC170A5SU）资助

通讯作者: 刘鹏宇 E-mail: liupengyu@cutc.net

作者简介: 王亚文，女，1995年生，北京有色金属研究总院硕士研究生 e-mail: wangyawen3848@163.com

引用本文:

王亚文，张勇，陈雄飞，刘英，赵珍阳，叶明国，许玉兴，刘鹏宇. 基于远程LIBS技术的镍基高温合金成分分析方法的研究[J]. 光谱学与光谱分析, 2022, 42(02): 603-608.
WANG Ya-wen, ZHANG Yong, CHEN Xiong-fei, LIU Ying, ZHAO Zhen-yang, YE Ming-guo, XU Yu-xing, LIU Peng-yu. Quantitative Analysis of Nickel-Based Superalloys Based on a Remote LIBS System. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2022, 42(02): 603-608.

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