激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)法测定涂层氧化锆颗粒铌层中24种微量杂质元素

Determination of 24 Trace Impurities in Niobium Coating of Zirconia Particles by Laser Ablation Inductively Coupled Plasma Mass Spectrometry(LA-ICP-MS)

针对涂层氧化锆颗粒涂层分析需求,建立了LA-ICP-MS分析Nb涂层和Zr基质中24种微量杂质元素测定方法,获得了最佳剥蚀条件(激光束斑44μm、能量密度6 J/cm2、剥蚀频率5 Hz),利用NIST610标样作为外标、Nb和Zr作内标分别校正了Nb涂层及Zr基质层。方法检出限1.5μg/g (Fe)、1.16μg/g(Cr)、0.36μg/g(Ni),其他21种元素检出限0.01~695.7μg/g。成功测定了60件Nb涂层和Zr基质样品中24种微量杂质元素,获得了26种元素深度剥蚀信号-时间轮廓图,激光剥蚀涂层时间为16~110 s。建立了涂层厚度测试方法,利用LA-ICP-MS技术结合环境扫描电镜能谱技术测定了球体涂层的厚度,获得了准确的LA深度剥蚀率0.371 4μm/s,并成功测定了60件样品中涂层的厚度(5.942~40.854μm),实现了涂层氧化锆涂层成分定量。

According to the requirements of zirconia particle coating analysis, a method to determine 24 trace impurities in Nb coating and Zr matrix by LA-ICP-MS was established.The best ablation conditions of this method(laser spot 44 μm, energy density 6 J/cm~2,ablation frequency 5 Hz) were obtained.The quantitative analyses of impurities in Nb coating and Zr matrix were corrected by using NIST610 standard sample as the external standard and Nb and Zr standard solutions as the internal standards, respectively.The detection limits were 1.5 μg/g(Fe),1.16 μg/g(Cr),and 0.36 μg/g(Ni),respectively.And the detection limits of other 21 elements were 0.01—695.7 μg/g.24 trace elements in 60 samples of Nb coating and Zr matrix were determined, and the deep denudation signal time profiles of 26 elements were obtained.The laser ablation time of the coating was 16—110 s.The measurement of coating thickness was established by LA-ICP-MS technology combined with environmental scanning electron microscope energy spectrum technology.The erosion rate of LA was 0.371 4 μm/s.The coating thicknesses of 60 samples(5.942—40.854 μm) were determined by this method.In this way, quantitative analysis of impurities in zirconia coating was achieved.