激光剥蚀电感耦合等离子体质谱法测定碳化硅器件中杂质元素  

Quantitative Analysis of Trace Elements in Silicon Carbide Device by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

作　　者：周慧[1,2] 汪正[2] 朱燕[2] 李青[2] 陈奕睿[2] 屈海云[2] 邹慧君[2] 杜一平[1] 胡慧廉[1] 

机构地区：[1]上海市功能性材料化学重点实验室,华东理工大学,上海200237 [2]中国科学院上海硅酸盐研究所,上海200050

出　　处：《分析化学》2014年第1期123-126,共4页Chinese Journal of Analytical Chemistry

基　　金：中国科学院仪器设备功能开发技术创新项目(No.Y27YQ3120G);上海硅酸盐研究所所创新重点项目资助

摘　　要：采用激光剥蚀电感耦合等离子体质谱法（LA—ICP—MS），以NIST玻璃标准物质制作校准曲线，^29Si为内标，相对灵敏度因子（RSF）校准标样和样品间的基体效应，对碳化硅陶瓷器件中9种痕量元素（B，Ti，Cr，Mn，Fe和Ni等）进行定量测定。选择线性扫描方式，激光剥蚀孔径为150μm，氦气和氩气流量为0．7L／min时，信号稳定性和灵敏度最佳。经内标校准后，各元素标准曲线的线性有较大改善，线性相关系数为0．9981～0．9999。以建立的方法对碳化硅标准参考物质（BAM—S003）中的痕量元素进行测定，并与标准参考值进行对比，结果一致，证实了LA—ICP．MS方法应用于碳化硅样品检测的准确性和有效性。采用本方法定量测定碳化硅器件中痕量元素，结果与辉光放电质谱法（GD—MS）测定的结果比较一致。元素B，Ti，Cr，Mn，Fe，Ni，Cu，Sr和La的检出限为0．004～0．08mg／kg，相对标准偏差（RSD）小于5％。Trace elements in silicon carbide SiC device were determined by laser ablation inductively coupled plasma mass spectrometry （LA-ICP-MS） using National Institute of Standards and Technology standard reference materials （NIST SRM） glasses as calibration standards with 29Si as internal standard, and relative sensitivity factor （RSF） to calculate the matrix effect. Stable signal intensity and high sensitivity were obtained when the laser spot size was 150 μm and the flow rate of Ar and He was 0.7 L/min. The correlation coefficients of trace elements have achieved 0. 9981-0. 9999 after internal standard correction. The reliability of the proposed method was confirmed by determining the content of B, Ti, Cr, Mn, Fe, Ni, and Cu in SiC standard reference material （ BAM-SO03 ）. The method was applied for analyzing the SiC device, and the result obtained by the method agreements with those by glow discharge mass spectrometry （GD-MS）. The detection limits ranged from 0. 004 mg/kg to 0.08 mg/kg for B, Ti, Cr, Mn, Fe, Ni, Cu, Sr and La. Relative standard deviation measured at trace element concentrations was less than 5 %

关 键 词：激光剥蚀 电感耦合等离子体质谱 碳化硅 

分 类 号：O657.63[理学—分析化学]