Synthesis of Ultra-Fine Columbite Powder MgNb2O6 by the Polymerized Complex Method

Pure MgNb₂O₆ powders with high specific surface area and high crystallinity have been successfully synthesized by the Polymerized Complex (PC) Method. A solution of water, citric acid, ethylene glycol and niobium and magnesium ions, was polymerized at 130°C by the water elimination and was calcined at 400°C for 2 h. The precursor formed was calcined at temperatures from 700°C to 1000°C in air to obtain the columbite phase. Thermal analysis, Raman spectroscopy, x-ray diffraction, adsorption/desorption hysteresis and scanning electron microscopy were used to investigate the polymer decomposition and the columbite phase evolution. No evidence for phase separation of crystalline MgCO₃ and Nb₂O₅ in Raman spectra and x-ray diffraction pattern as distinct intermediates were found, and the MgNb₂O₆ probably is formed through a single-step decomposition of oxycarbonate intermediate, as other double oxide synthesized by the PC Method, as indicated by the thermal decomposition of the precursor.