辉光放电质谱法测定高纯钨中10种杂质元素

doi:10.13228/j.boyuan.issn1000-7571.011812

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摘要高纯钨广泛应用于电子信息行业,其电子特性很大程度上取决于其杂质含量,因此,有必要对高纯钨中杂质元素进行测定。通过优化辉光放电工艺参数、选择合适的同位素及分辨率,建立了辉光放电质谱法(GDMS)测定高纯钨中10种痕量杂质元素的分析方法。优化后的放电条件为:放电电流3.0 mA,放电气体流量500 mL/min,预溅射时间20 min。为提高痕量杂质元素的检测准确度,利用高纯钨标准样品对10种元素的相对灵敏度因子(RSF)进行了校正,获得了与基体匹配的RSF。方法中10种元素的检出限为0.005~0.019 μg/g,定量限为0.017~0.064 μg/g。按照实验方法测定高纯钨中10种杂质元素,并用电感耦合等离子体质谱法(ICP-MS)的测定结果作为比较以验证准确性。结果表明:样品中杂质元素的含量为0.027~155.07 μg/g,质量分数小于100 μg/g的杂质元素,其结果相对标准偏差(RSD,n=6)均小于30%;质量分数大于100 μg/g的杂质元素,其结果RSD(n=6)小于10%。除Mg、Sn、Pb低于ICP-MS的检出限外,其余各杂质元素的测试结果与ICP-MS结果基本一致。

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关键词 ：辉光放电质谱法(GDMS), 高纯钨, 杂质元素, 相对灵敏度因子(RSF)

Abstract：High-purity tungsten is widely used in the electronic information industry, and its electronic properties significantly depend upon the impurity content. Therefore, it is necessary to measure the impurity elements in high-purity tungsten. An analytical method for the determination of 10 trace impurity elements in high-purity tungsten by glow discharge mass spectrometry (GDMS) was established by optimizing the process parameters of glow discharge as well as selecting appropriate isotopes and resolution. The optimized discharge conditions were obtained as follows: the discharge current of 3.0 mA, the discharge gas flow rate of 500 mL/min, and pre-sputtering time of 20 min. In order to improve the detection accuracy of trace impurity elements, the relative sensitivity factor (RSF) values of 10 elements were calibrated using high-purity tungsten standard samples, and the RSF values matching the matrix were obtained. The limits of detection(LODs) of 10 elements in the method were in range of 0.005-0.019 μg/g, and the limits of quantification were in range of 0.017-0.064 μg/g. Ten impurity elements in high-purity tungsten samples were detected according to the experimental method, and the measurement results by inductively coupled plasma mass spectrometry(ICP-MS) were used as a comparison to verify the accuracy. The results showed that the contents of impurity elements in the sample were in the range of 0.027-155.07 μg/g. For the impurity elements with mass fraction less than 100 μg/g, the relative standard deviations (RSD,n=6) were lower than 30%. For the impurity elements with mass fraction more than 100 μg/g, the relative standard deviations (RSD,n=6) were lower than 10%. Except for Mg, Sn and Pb which were lower than the LODs of ICP-MS, the test results of other impurity elements were basically consistent with those obtained by ICP-MS.

Key words： glow discharge mass spectrometry (GDMS) high-purity tungsten impurity element relative sensitivity factor(RSF)

收稿日期: 2022-03-22

ZTFLH:	O657.63
	TF841.1

基金资助:宁波市关键核心技术应急攻关计划项目(2020G009)

通讯作者: 李明利(1982—),男,教授,博士,主要研究方向为医用金属材料;E-mail:limingli82@126.com

作者简介: 余琼(1984—),女,高级工程师,硕士,主要研究方向为金属材料理化检测;E-mail:yqtjtcm@126.com

引用本文:

余琼, 翟宇鑫, 连危洁, 马兰, 李爽, 李明利. 辉光放电质谱法测定高纯钨中10种杂质元素[J]. 冶金分析, 2022, 42(11): 8-14. YU Qiong, ZHAI Yuxin, LIAN Weijie, MA Lan, LI Shuang, LI Mingli. Determination of ten impurity elements in high-purity tungsten by glow discharge mass spectrometry. , 2022, 42(11): 8-14.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.011812 或 http://yjfx.chinamet.cn/CN/Y2022/V42/I11/8

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