等离子体温度和谱线强度综合校准的CF-LIBS定量分析合金成分  

Quantitative CF-LIBS analysis of alloys via comprehensive calibration of plasma temperature and spectral intensity

作　　者：张雷[1,2] 赵书霞 孙颖[1] 尹王保 董磊[1,2] 马维光 肖连团[1,2] 贾锁堂 

机构地区：[1]山西大学量子光学与光量子器件国家重点实验室山西大学激光光谱研究所,太原030006 [2]山西大学极端光学协同创新中心,太原030006

出　　处：《中国科学：物理学、力学、天文学》2018年第1期116-122,共7页Scientia Sinica Physica,Mechanica & Astronomica

基　　金：国家重点基础研究发展计划(编号:2017YFA0304203);国家自然科学基金(编号:61775125;61475093;61378047;11434007);长江学者和创新团队发展计划(编号:IRT13076);山西省重大科技专项(编号:MD2016-01)资助项目

摘　　要：合金成分直接决定其机械性能和应用领域,对合金中各元素含量的准确、快速检测,对于冶金生产质量控制和材料分类意义重大.本文提出了一种基于等离子体温度和谱线强度综合校准的自由定标激光诱导击穿光谱(CF-LIBS)定量分析方法,选用一个与待测样品基质相同的标准样品,通过二阶迭代计算来对比不同等离子体温度和谱线强度校准系数所对应的元素含量标准误差和,寻找最小标准误差和,优化等离子体温度和次量元素谱线强度校准系数,从而建立定量分析模型,实现对待测样品中主次量元素含量的精确定量分析.基于铜铅合金的检测结果表明,本方法对样品中主量元素Cu,Zn和次量元素Pb的相对测量误差分别为4.4%,6.2%和17.7%,远优于常规CF-LIBS方法.本文提出的新方法有助于推进CF-LIBS技术在冶金生产质量监控和材料鉴别分类中的应用.The chemical composition of alloys directly determines their mechanical behaviors and application fields. Accurate and rapid analysis of each element in alloys plays a key role in metallurgy quality control and material classification processes. A quantitative calibration-free laser-induced breakdown spectroscopy（CF-LIBS） analysis method, which carries out comprehensive calibration of plasma temperature and spectral intensity by using a second-order iterative algorithm and a similar matrix standard sample, is proposed to compare the standard errors that correspond to various plasma temperatures and calibration coefficients. Once the minimal standard error is found, we can optimize both the plasma temperature and the calibration coefficient of the minor element emission line, and establish the quantitative analysis model to realize accurate elemental composition measurements. In our experiments, the ZBY910 copper-lead alloy is selected to be the standard sample. Here, 6 Cu I lines and 5 Pb I lines are utilized to draw the Boltzmann plots,and the plasma temperature is predicted to be in the range of 5000-10000 K. Experimental results show that, the optimal plasma temperature and correction coefficient are found to be 7710 K and 0.61, respectively, as the standard error reaches its minimum of 0.06. Compared to conventional CF-LIBS analysis, the relative errors for major elements Cu and Zn and minor element Pb in the samples have been reduced from 13%, 20%, and 74% to 4.4%, 6.2%, and 17.7%, respectively,which are much superior to those of the conventional CF-LIBS method. This new method has greatly improved the quantitative analysis accuracy of CF-LIBS and realized more accurate measurement of both major and minor elements in alloy samples. It is expected to promote the application of CF-LIBS technology in fields such as metallurgical quality monitoring, material identification, classification, etc.

关 键 词：自由定标激光诱导击穿光谱 元素定量分析 综合校准 

分 类 号：TG115[金属学及工艺—物理冶金] TN249[金属学及工艺—金属学]