F. Lantelme et al., THE INFLUENCE OF OXIDE ON THE ELECTROCHEMICAL PROCESSES IN K2NBF7-NACL-KCL MELTS, Journal of the Electrochemical Society, 142(12), 1995, pp. 4097-4102
Transient electrochemical techniques showed that in NaCl-KCl melts the
reduction of K2NbF7 occurs through a two-step reaction Nb(V) --> Nb(I
V) --> Nb. When oxide ions were introduced, cyclic voltammetry indicat
ed that the waves corresponding to reduction of the complex NbF72- pro
gressively disappeared. Oxo complexes, such as NbOFn(n-3-) are reduced
at a potential close to that of the Nb(IV) fluoro complexes. Niobium
metal deposition was perturbed by; the formation of niobium suboxides
like NbO or Nb4O5. For molar ratios of oxide to Nb greater than one, a
black layer of niobium oxide, NbO2, appeared at the electrode surface
. The present study confirms the high oxygen affinity of niobium and s
hows that a careful purification of the electrolyte and feeding materi
als is required for producing niobium with a low oxygen content.