Formation of niobium oxides by electrolysis from acidic aqueous solutions on glassy carbon

Abstract

In this study niobium oxide films were formed without peroxo-precursors from three different mixed acidic aqueous solutions on glassy carbon. Linear sweep voltammetry and potential step were techniques used for electrochemical experiments. The simultaneous and consecutive electrochemical reduction of water, nitrate and sulphate ions provided an alkaline environment with oxygen in the near vicinity of the working cathode, which in combination with the present niobium ions, produced niobium oxides and/or oxyhydroxides on the glassy carbon substrate. The formed deposits were analyzed using scanning electron microscopy and energy dispersive spectroscopy and appear to consist of NbO, NbO2 and Nb2O5. Both the niobium and acid concentration of the electrolytes used influenced the morphology and particle size of the deposits. The formation of niobium-fluoride and hydrogen-niobiumoxide complexes is addressed.