Express X-Ray Fluorescence Analysis of Technical-Grade Tantalum and Niobium: from Raw Materials to Products

IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Inorganic Materials Pub Date : 2024-07-19 DOI:10.1134/s0020168524700067
L. Yu. Mezhevaya, M. N. Filippov, O. I. Lyamina, G. E. Mar’ina, A. A. Arkhipenko, V. B. Baranovskaya
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Abstract

The available approaches to detecting impurities in Ta- and Nb-based materials involve transferring a sample into a solution with subsequent isolation of impurities. This procedure is quite complicated and time-consuming. Therefore, it is interesting to study the possibilities of direct, in particular, X-ray fluorescence (XRF), analysis of solid samples of these materials. The conventional XRF scheme, which involves the experimental construction of calibration characteristics for each element being determined, requires a large number of reference samples containing a very wide range of impurities. In this work, a preliminary characterization of samples of technical tantalum and niobium and products based on them has been carried out. It is shown that, for initial materials, the XRF method can establish only a significant absence of impurities; however, even for sintered niobium hydride and tantalum powder, XRF can be used for the express estimation of the composition. It is proposed to use a Spectroscan MAX-GVM crystal diffraction spectrometer for the analysis and to construct the calibration using the standard software that implements the fundamental parameter method. In this case, the resulting impurity contents can differ from reference values by one to two orders of magnitude. Such accuracy is often sufficient to adjust the technology. The limits of the XRF detection of impurities in Ta- and Nb-based materials have been established. For the elements determined by K-series lines (from Ti to Co), the detection limits range within 30–60 ppm; for the elements determined by M-series lines (Ta), the detection limit is approximately 200 ppm; and for L-series lines (Nb), it is from 100 to 150 ppm.

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技术级钽和铌的快速 X 射线荧光分析:从原材料到产品
摘要 检测钽基和铌基材料中杂质的现有方法涉及将样品转移到溶液中,然后分离杂质。这一过程相当复杂且耗时。因此,研究对这些材料的固体样品进行直接分析,特别是 X 射线荧光分析(XRF)的可能性很有意义。传统的 X 射线荧光分析法需要在实验中为每种待测元素建立校准特征,这就需要大量含有各种杂质的参考样品。在这项工作中,我们对工业钽和铌样品以及以它们为基础的产品进行了初步表征。结果表明,对于初始材料,XRF 方法只能确定明显不含杂质;但是,即使对于烧结的氢化铌和钽粉,XRF 也可用于明确估算成分。建议使用 Spectroscan MAX-GVM 晶体衍射光谱仪进行分析,并使用执行基本参数法的标准软件进行校准。在这种情况下,得出的杂质含量可能与参考值相差一到两个数量级。这种精度通常足以调整技术。钽基和铌基材料中杂质的 XRF 检测极限已经确定。对于 K 系列线测定的元素(从钛到钴),检测限在 30-60 ppm 范围内;对于 M 系列线测定的元素(钽),检测限约为 200 ppm;对于 L 系列线(铌),检测限为 100-150 ppm。
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来源期刊
Inorganic Materials
Inorganic Materials 工程技术-材料科学:综合
CiteScore
1.40
自引率
25.00%
发文量
80
审稿时长
3-6 weeks
期刊介绍: Inorganic Materials is a journal that publishes reviews and original articles devoted to chemistry, physics, and applications of various inorganic materials including high-purity substances and materials. The journal discusses phase equilibria, including P–T–X diagrams, and the fundamentals of inorganic materials science, which determines preparatory conditions for compounds of various compositions with specified deviations from stoichiometry. Inorganic Materials is a multidisciplinary journal covering all classes of inorganic materials. The journal welcomes manuscripts from all countries in the English or Russian language.
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