Determination of 14 Metal Impurities in N-Methylpyrrolidone for Integrated Circuits by Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry
摘 要
提出了有机加氧进样系统结合三重四极杆电感耦合等离子体质谱法测定集成电路用N-甲基吡咯烷酮(NMP)中Na、Cd、Pb、Mg、Al、Ca、Cr、Mn、Fe、Co、Ni、Cu、Zn、K等14种金属杂质含量的方法。通过氧气在线燃烧的方式降低了碳沉积对锥口的影响,采用标准加入法匹配基体效应,使用冷等离子体-氨气碰撞反应模式解决了碳元素质谱干扰的问题,如12C12C+对24Mg+的干扰,12C40Ar+对52Cr+的干扰。14种元素的加标回收率为83.2%~123%,14种元素工作曲线的相关系数均大于0.999 0,方法可用于分析杂质元素质量分数低于20.00 ng·kg-1的样品,满足先进制程的质量要求。
Abstract
A method was proposed for determination of 14 metal impurities in N-methylpyrrolidone (NMP), including Na, Cd, Pb, Mg, Al, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, and K, by triple quadrupole inductively coupled plasma mass spectrometry with the organic additional oxygen sampling system. The impact of carbon deposition on the cone was reduced through oxygen online combustion. The standard addition method was used for matching the matrix effect, and the mass interference from carbon element was eliminated by the cold plasma-ammonia gas collision reaction mode, such as the interferences of 12C12C+ on 24Mg+ and 12C40Ar+ on 52Cr+. The spiked recoveries of 14 elements were 83.2%-123%, and the correlation coefficients of calibration curves for 14 elements were better than 0.999 0. This method was applied to the analysis of samples with mass fraction less than 20.00 ng·kg-1, which could meet the quality requirements of advanced production processes.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202309015
所属栏目 专题报道(新型激发光源技术的应用)
基金项目 上海市2020年度“科技创新行动计划”技术标准项目(20DZ2203000);上海市市场监管局科研项目(2021-02)
收稿日期 2022/8/28
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备注李春华,高级工程师,硕士,研究方向为集成电路材料检测
引用该论文: LI Chunhua,GAO Yiming,HAO Ping,TIAN Yuping,CAO Jianxiong,LI Jie. Determination of 14 Metal Impurities in N-Methylpyrrolidone for Integrated Circuits by Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(9): 1073~1076
李春华,高一鸣,郝萍,田玉平,曹建雄,李杰. 三重四极杆电感耦合等离子体质谱法测定集成电路用N-甲基吡咯烷酮中14种金属杂质的含量[J]. 理化检验-化学分册, 2023, 59(9): 1073~1076
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【2】BARBAGINI F, HALDER S, JANSSENS T, et al. Particle removal efficiency and damage analysis on silicon wafers after megasonic cleaning in solvents[J]. Journal of Adhesion Science and Technology, 2009,23(12):1709-1721.
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【4】魏新宇,李现忠,宋阳,等.N-甲基吡咯烷酮中微量Na、Al、K含量分析——有机加氧ICP-MS直接进样法[J].石化技术, 2020,27(6):11-12.
【5】张文媚,吕玉平,闻环,等.有机溶剂稀释-电感耦合等离子体发射质谱法测定原油砷含量[J].广东化工, 2022,49(3):179-181.
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