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材料铟中微量元素定量分析基础研究

发布时间:2018-08-25 10:34
【摘要】:铟是一种稀有金属,由于具有优良的物理化学性能和机械性能被广泛应用于制造ITO靶材和电子行业。铟中的杂质元素的含量影响其纯度,进而影响纯铟的应用。随着半导体行业的快速发展,对高纯金属铟的要求也越来越高。因此对铟材料中杂质元素含量快速准确测定的研究日益引起人们的重视。本文综述了铟的性质、用途以及铟中杂质元素的分析检测方法等。以高纯铟丝为基体材料,提出了采用在铟基体中加入高纯金属杂质的方法制备实验室质控样品。制备质控样品的实验研究,分别考察了温度、加热搅拌时间、冷却搅拌时间等参数对铟掺杂杂质均匀性的影响,得到了制备实验室质控样品最合适的工艺条件:温度为280℃、加热搅拌时间3 h、冷却搅拌时间6 min。针对实验室质控样品均匀性研究的测试方法-辉光放电质谱(GD-MS)法进行条件优化,考察了放电电流、放电气体流量、预溅射时间、分辨率等因素的影响,得到了仪器最佳优化条件。采用F检验法对均匀性测试数据进行统计分析,计算得到F值,Al、Fe、Cu、Zn的F值分别为3.27、90、3.98、56.82,均大于临界值2.77,由此判断这些元素在铟基体中是不均匀的;Ag、Cd、Sn、Sb、Pb、Bi的F值分别为2.74、0.82、2.26、0.28、2.75、2.65,均小于临界值2.77,表明这些元素在铟基体中分别相对均匀。利用电感耦合等离子体原子发射光谱仪(ICP-AES)对实验室质控样品进行定值研究,并进行了 ICP-AES法分析谱线的选择、仪器工作条件优化、标液匹配基体与否的影响、精密度和准确度等条件实验。根据Ag、Cd、Sn、Sb、Pb、Bi六个元素的定值结果,计算得到其相对灵敏度因子(RSF),分别为0.79、0.60、1.33、0.88、1.97、0.62,与GD-MS仪器内置相对灵敏度因子进行比较,Sn、Pb这两个元素相差2.5倍以内,Ag、Cd、Sb、Bi这四个元素分别相差3~4倍,表明铟基体对杂质元素的测定结果有较大影响。
[Abstract]:Indium is a rare metal, which is widely used in the manufacture of ITO targets and electronics because of its excellent physical and chemical properties and mechanical properties. The content of impurity elements in indium affects its purity and the application of pure indium. With the rapid development of semiconductor industry, the requirement of high-purity indium is becoming higher and higher. Therefore, rapid and accurate determination of impurity elements in indium materials has attracted more and more attention. The properties, applications and analytical methods of impurity elements in indium are reviewed in this paper. High purity indium wire was used as matrix material to prepare laboratory quality control samples by adding high purity metal impurities into indium matrix. The effects of temperature, heating agitation time and cooling stirring time on the homogeneity of indium doped impurity were investigated. The most suitable process conditions for the preparation of quality control samples were obtained as follows: temperature 280 鈩,

本文编号:2202619

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