Synthesis and characterization of CuNb2O6 from an oxalic precursor via solid state reaction

Abstract

The present paper's objective was to synthesize and characterize both the oxalic niobium precursor (NH4)3NbO(C2O4)3.H2O, and the product of its doping with Cu and calcining, CuNb2O6. In order to obtain the niobium precursor, commercially available niobium oxide (Nb2O5) was subject to fusion with potassium bisulfate (KHSO4). Once leached with water, the powder was complexed with oxalic acid and ammonium oxalate. The as produced material was manually mixed with copper nitrate Cu(NO3)2.2H2O (25% Cu molar) and calcined at 1000°C in a muffle furnace. CuNb2O6 was then obtained. The precursor was characterized by XRD, SEM, FT-IR, XRF, TG/DTG. The calcination product was characterized by XRD, XRF and SEM. Results show that single phase CuNb2O6 could be obtained by this method without Nb2O5 contamination.