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Preparation and Characterization of Ultra-High-Purity Niobium

  • Extractive & Process Metallurgy
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Abstract

This paper presents a review of the efforts directed to the preparation of ultra-high-purity Nb published during the last 15 years. The interest in high-purity Nb has risen from the need for materials in high temperature and vacuum technology, superconductivity, solid state physics, and its potential in atomic energy fields. Depending on its many applications, the “purity” of Nb is understood in different ways. Based on results of known purification processes for Nb (e.g., liquid-liquid extraction of fluorides, distillation of halogenides, electrolysis in molten salts, electron beam float zone refining, electrotransport, and degassing in ultra high vacuum), an optimized method has been developed, consisting of electrolytic refining which results in single crystals, zone melting, and ultra high vacuum treatments. Material produced by the process has maximum impurity concentrations of 10−l ppm Ta, 2×10−3 ppm W, 4×10−6ppm Co, 2×10−3 ppm Fe, 10−5 ppm Cr, etc., with less than 1 ppm interstitials (C,N,O, except H) and a residual electrical resistivity ratio (RRR) of >104. To accurately determine residual impurity levels, improved analytical techniques were developed. Doping of the produced Nb with selected metallic (Cr,Mo,Hf,Ir) and nonmetallic elements (C, 0) on the ppm level served as both a calibration of the analytical techniques and an effort to tailor the physical properties. General aspects for the development of purification processes for refractory metals, sources of contamination during purification, sample preparation, and application of Nb, as well as the limiting bulk and surface purity of reactive metals are presented here.

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Authors and Affiliations

  1. Max-Planck-Institut für Metallforschung Institut für Werkstoffwissenschaften, Stuttgart, West Germany

    Klaus K. Schulze

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This paper was presented at the Extractive Metallurgy of Refractory Metals Conference at the 1981 AIME Annual Meeting in Chicago, Illinois.

Klaus K. Schulzeis senior scientist at the Max-Planck-lnstitut fur Metallforschung, Stuttgart, West Germany. He received his MSc in iron and steel metallurgy and his PhD in metallurgy from the Technical University of Clausthal in 1967 and 1971 respectively. He joined the MPI in Stuttgart in 1967, and served as a visiting professor at the University of Campinas, Brazil, in 1978. Since 1979 he has been a member of the advisory board of the Foundation for Industrial Technology (FTI) of the Brazilian Government, in the field of refractory metals. His research interests include methods for ultrapurification of metals, metal-gas reactions, thermodynamic properties of refractory metal alloys, analytical chemistry of non-metals, and the toxicology of beryllium. He is a member of TMS.

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Schulze, K.K. Preparation and Characterization of Ultra-High-Purity Niobium. JOM 33, 33–41 (1981). https://doi.org/10.1007/BF03354422

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