基于激光剥蚀-电感耦合等离子体质谱法的金属镝棒统计分布分析初探

发布时间：2018-02-20 17:13

本文关键词： 激光剥蚀-电感耦合等离子体质谱法(LA-ICP-MS) 固态电迁移统计分布分析稀土材料镝　出处：《冶金分析》2017年05期 　论文类型：期刊论文

【摘要】：高效、高灵敏度的原位微区分析技术开发对于固态电迁移等稀土提纯工艺具有重要意义。实验以固态电迁移提纯后金属镝棒为研究对象,将激光剥蚀-电感耦合等离子体质谱法(LA-ICP-MS)应用于高纯稀土金属的微区分布分析。研究了激光剥蚀速率对样品覆盖率和分析时间的影响,确定了剥蚀速率为50μm/s;考察了剥蚀池及ICP-MS载气流量对待测元素信号强度、氧化物产率及元素分馏效应的影响,确定了载气流量分别为0.60L/min(He)和1.0L/min(Ar)。采用线扫描方式,以基体元素~(158)Dy为内标,获得了不同电迁移区域各杂质元素的二维相对强度分布图,初步探究了各杂质元素的迁移规律。结果显示:在电迁移过程中,Al、Si、Ti、Fe、Mo、W元素从阴极向阳极迁移;Ni、Cu元素从中间区域向两极迁移。这一迁移趋势与辉光放电质谱法(GD-MS)分析结果相一致。同时,LA-ICP-MS还得到更丰富的微区统计分布信息。不同电迁移区域各杂质元素最大偏析度、相对标准偏差(RSD)值及最大偏析位置进一步揭示了各元素的迁移状态,可能与固态电迁移工艺相联系。因此,LA-ICPMS有望为稀土金属提纯工艺解析及优化提供一种新的有效分析手段。
[Abstract]:The development of high efficiency and high sensitivity in situ microanalysis technology is of great significance for the solid state electromigration and other rare earth purification processes. The laser denudation-inductively coupled plasma-mass spectrometry (LICP-MS) was applied to analyze the microdistribution of high purity rare earth metals. The effect of laser denudation rate on sample coverage and analysis time was studied. The denudation rate was determined to be 50 渭 m / s, and the effects of denudation tank and ICP-MS carrier gas flow rate on signal intensity, oxide yield and elemental fractionation effect were investigated. The carrier gas flow rates were 0.60 L 路min ~ (-1) and 1.0 L ~ (-1) 路min ~ (-1) 路min ~ (-1), respectively. The two-dimensional relative strength distribution of impurity elements in different electromigration regions has been obtained by using the matrix element, 158Dy, as the internal standard, and the relative strength distribution of the impurity elements in different electromigration regions has been obtained. The migration rules of various impurity elements were preliminarily investigated. The results showed that the elements of AlAlSiSiTiTiFeMoMoW migrated from cathode to anode from the middle region to the two poles. This migration trend and GD-MSanalysis by Glow discharge Mass Spectrometry (GD-MS) showed that the Cu element was transferred from the cathode to the anode. The results are consistent. At the same time, LA-ICP-MS also gets more information of statistical distribution of microregions. The maximum segregation degree of impurity elements in different electromigration regions is also obtained. The relative standard deviation (RSD) value and the maximum segregation position further reveal the migration state of each element, which may be related to the solid state electromigration process. Therefore, LA-ICPMS is expected to provide a new and effective analytical method for the analysis and optimization of rare earth metal purification process.
【作者单位】：钢铁研究总院金属材料表征北京市重点实验室;北京有色金属研究总院稀土材料国家工程研究中心;
【基金】：国家重点研发计划材料基因工程关键技术与支撑平台专项(2016YFB0700302)
【分类号】：TG115.33

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