Chemical Reagents

2025, 09, v.47 29-40

Research Progress on Analysis Technology of Metal Impurities in Electronic Chemical Precursor Materials

LI Geng-yin^1,2 SHI Ze-yuan³ LI Chun-hua¹ XU Jian-guang² ZHANG Xing-yu² WANG Jun² CHANG Yan¹

School of Energy and Materials,Shanghai Second Polytechnic University;China Electronics Standardization Institute; School of Energy and Materials,Shanghai Second Polytechnic University;China Electronics Standardization Institute; School of Energy and Materials,Shanghai Second Polytechnic University;China Electronics Standardization Institute;

Email: changy@simt.com.cn;

DOI: 10.13822/j.cnki.hxsj.2025.0118

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摘要：

随着半导体制程特征尺寸缩小至纳米级，前驱体材料中金属杂质控制已成为影响器件性能和良率的决定性因素。阐述了电子化学品前驱体的定义、分类及标准体系现状。系统梳理了固态、液态和气态前驱体的样品前处理技术，针对不同形态前驱体的特殊性质和分析需求，深入分析了电热板湿法消解、微波消解、灰化法、热挥发-酸溶解法、酸雾消解法、石墨熏蒸法、直接酸消解法、减压蒸馏法、溶液吸收法、气体吸收-水解混合法等关键技术的原理、适用条件和技术要点。论述了电感耦合等离子体质谱(ICP-MS)技术在前驱体分析中面临的质谱干扰和基体效应问题，以及高分辨率质谱、反应/碰撞池技术等解决方案。在分析方法验证与质量保证方面，针对前驱体材料缺乏标准参考物质、基体复杂多变、检测限要求极低等挑战，提出结合测量系统分析(MSA)与传统验证方法的综合策略，通过系统评估重复性、再现性和关键变异因素，确保方法的可靠性。随着半导体工艺迈入5 nm及以下节点，前驱体材料金属杂质分析将向前处理与仪器分析技术融合、人工智能应用、在线监测等方向发展。加强方法标准和标准物质研制，建立完善的质量控制体系，对支撑电子化学品前驱体材料产业发展具有重要意义。

关键词： 电子化学品前驱体; 金属杂质分析; 样品前处理; 电感耦合等离子体质谱; 质谱干扰; 基体效应; 方法验证;

Abstract：

As semiconductor manufacturing processes advance to the nanometer level,the control of metal impurities in precursor materials has become a critical factor affecting device performance and yield. This article first outlined on the definition,classification,and current status of the standard system of electronic chemical precursors. It then systematically reviewed sample pretreatment techniques for solid,liquid,and gaseous precursors. In view of the unique properties and analytical requirements of different precursors forms,the principles,applicable conditions,and technical key points of various methods including wet digestion with electric heating plates,microwave digestion,ashing,thermal volatilization-acid dissolution,acid mist digestion,graphite fumigation,direct acid digestion,vacuum distillation,solution absorption and gas absorption-hydrolysis mixing were discussed in depth.The article further discussed the challenges in inductively coupled plasma mass spectrometry( ICP-MS) for precursor analysis,including spectral interference and matrix effect,and presents solutions such as high-resolution mass spectrometry and reaction/collision cell technology.In terms of analytical method validation and quality assurance,challenges such as the lack of standard reference materials for precursor materials,complex and variable matrices,and extremely low detection requirements were addressed by proposing a comprehensive strategy combining Measurement System Analysis( MSA) and traditional validation methods.By systematically evaluating repeatability,reproducibility,and key variation factors,the reliability of the method was ensured. As semiconductor nodes move into the 5 nm and sub-5 nm era,the analysis of metal impurities in precursor materials was expected to evolve towards integrated pretreatment and analytical technologies,artificial intelligence applications,and real-time online monitoring. Strengthening the research and development of method standards and reference materials and establishing a complete quality control system are of great significance for supporting the development of the electronic chemical precursor materials industry.

KeyWords： electronic chemical precursors; metallic impurity analysis; sample pretreatment; inductively coupled plasma mass spectrometry; mass spectrometric interference; matrix effect; method validation;

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Basic Information:

DOI：10.13822/j.cnki.hxsj.2025.0118

China Classification Code:O657.63;TN40

Citation Information:

[1]李更银,史泽远,李春华,等.电子化学品前驱体材料中金属杂质分析技术研究进展[J].化学试剂,2025,47(09):29-40.DOI:10.13822/j.cnki.hxsj.2025.0118.

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国家市场监督管理总局科技计划项目(2023MK029)

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Chemical Reagents

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