The preparation of pure niobium for neutron dosimetry purposes

Abstract

A technique is described for the preparation of high purity niobium for use in fast neutron dosimetry. Based on results of known purification processes for niobium, an optimized method has been developed, consisting of: (1) a double electrolytic refining in an eutectic lithium-, sodium-, potassium-fluoride melt, containing fluoro-potassium niobate (K 2NbF 7), (2) electron beam float zone melting (EBFZM) in ultra high vacuum (UHV) and (3) UHV treatments. Starting with EBFZM of niobium of commercial quality (140 μg/g Ta, 35 μg/g W) the tantalum and tungsten contents were reduced by a first electrolysis to approximately 4 and 4 × 10 −2 μg/g, respectively. For a second electrolytic refining using a salt bath with extremely low tantalum and tungsten contents, this material was subjected to an additional EBFZM process. The niobium metal produced by this step was three times zone melted to reduce those elements (e.g. Fe, Co, Ni, O, N) which increased during the electrolyses. Material produced by this technique has impurity concentrations below 0.4 μg/g of tantalum and 10 −2 μg/g of tungsten. The concentration of the interstitials (C, O, N except H) is below the detection limit of classical analytical methods. A further reduction of the interstitials by annealing treatments in UHV of this material resulted in an electrical residual resistivity ratio (RRR) ρ(295 K)/ ρ(4.2 K) = 24 500 indicating an impurity concentration far below 1 μg/g.