激光诱导击穿光谱技术对钕铁硼永磁材料中多元素的定量表征  

Quantitative Characterization of Components in Neodymium Iron Boron Permanent Magnets by Laser Induced Breakdown Spectroscopy(LIBS)

作　　者：刘佳[1,2] 郭飞飞 于雷 崔飞鹏 赵迎 韩冰 沈学静 王海舟[1,2] LIU Jia;GUO Fei-fei;YU Lei;CUI Fei-peng;ZHAO Ying;HAN Bing;SHEN Xue-jing;WANG Hai-zhou(Central Iron and Steel Research Institute,Beijing 10008l,China;NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

机构地区：[1]钢铁研究总院,北京100081 [2]钢研纳克检测技术股份有限公司纳克研究院,北京100081

出　　处：《光谱学与光谱分析》2024年第1期141-147,共7页Spectroscopy and Spectral Analysis

基　　金：国家重点研发计划项目(2021YFB3202400)资助。

摘　　要：“磁王”钕铁硼是现今性能最为优异的永磁体,因其优异的磁性能被广泛应用于工业互联网、新能源、 5G通讯等诸多高新科技领域。目前研究钕铁硼材料中元素成分的主要分析方法有电感耦合等离子体发射光谱(ICP-OES)和X射线荧光光谱(XRF),其中ICP-OES是湿法分析,样品前处理复杂,测试周期长,而XRF法可实现直接分析,但受制于其轻元素的检测能力很难满足对钕铁硼材料中主要轻元素B的分析需求。激光诱导击穿光谱(LIBS)技术具有分析效率高,样品前处理简单,多元素直接分析,适用于现场分析、在线分析等技术优点,使其在快速定量表征方面展现出其独有的优势。运用LIBS分析技术开展对钕铁硼材料中多元素定量表征的直接、快速分析的方法研究,首先针对钕铁硼材料中定量表征的九个元素Nd、 Co、 B、 Dy、 Tb、 Pr、 Cu、 Al、 Ga完成特征谱线的筛选,通过对系统激光器电压、激光剥蚀方式等因素在不同条件下对钕铁硼材料光谱信号稳定性的影响分析,优化并确立了分析条件,最终选用720V的激光器电压,15个预剥蚀脉冲15个剥蚀脉冲的激光剥蚀方式为钕铁硼样品的分析条件;其次,选取8个通过ICP-OES法定值的烧结钕铁硼样品,样品具有元素成分的梯度差异化特征,作为建立分析方法的标准样品,采用标准曲线法通过相对强度与浓度的关联方式,建立钕铁硼样品中Nd、 Co、 B、 Dy、 Tb、 Pr、 Cu、 Al、 Ga九个元素的定量分析校准曲线;最后选取两个烧结钕铁硼试样,运用建立的定量分析方法完成九个元素的定量表征,分析时间小于30 s,其定量结果与ICP-OES法测定结果的比对,具有较好的一致性。运用激光诱导击穿光谱分析技术实现了对钕铁硼材料中多元素成分的直接、同时、快速定量表征,为钕铁硼材料的快速定量表征提供了新的技术思路和表征方法。"Magneto"neodymium iron boron is the most excellent permanent magnet,and it is widely used in the industrial internet,New Energy,5G communications and many other high-tech fields because of its excellent magnetic properties.Currently,the main analytical methods for elements in Nd-Fe-B are Inductively coupled plasma emission spectrometry(ICP-OES)and X-ray fluorescence spectrometry(XRF).ICP-OES is a wet analytical method with complex sample pretreatment and a long testing period,and the XRF method can be used for direct analysis,but it is challenging to meet the analysis demand of the main light element B in Nd-Fe-B because of its detection ability.Laser-induced breakdown spectroscopy(LIBS)technology has many advantages,such as high analysis efficiency,simple sample pretreatment,direct multi-element analysis,suitable for on-site analysis and on-line,etc.,it shows its unique advantage in fast quantitative characterization.In this paper,the LIBS technology is used to study the direct and rapid method for quantitative characterization of multi-elements in Nd-Fe-B.At first,the screening of characteristic spectral lines is completed for nine elements(Nd,Co,B,Dy,Tb,Pr,Cu,Al,Ga)in Nd-Fe-B was characterized quantitatively based on the analysis of the influence of the system laser voltage,laser ablation mode on the spectral signal stability of Nd-Fe-B under different conditions.The analysis conditions are optimized and established,in the end,720 V laser voltage and 15 pre-ablation pulses and 15 ablation pulses are selected as the analytical conditions of Nd-Fe-B samples.Eight Nd-Fe-B samples were determined by the ICP-OES method.The samples had the gradient difference characteristics of element composition and were used as the standard samples for establishing the analytical method.The calibration curves of Nd,Co,B,Dy,Tb,Pr,Cu,Al and Ga in Nd-Fe-B samples were established by standard curve method which was used to correlate the strength ratio with the concentration.At last,two sintered samples of Nd-Fe-B were selected to pe

关 键 词：激光诱导击穿光谱 钕铁硼 定量表征 

分 类 号：O657.3[理学—分析化学]