Thermochimica Acta, Vol.639, 91-97, 2016
Formation mechanism, crystallite growth and electrical conductivity of nano-crystalline CuxFe3-xO4 (0.75 <= x <= 1.25) spinels prepared by glycine-nitrate process
The CuxFe3-xO4 (0.75 <= x <= 1.25) nano-crystalline powders were prepared by an optimized glycine-nitrate process (GNP) followed by calcination. Thermal analysis and X-ray diffraction (XRD) data revealed that formation of CuFe2O4 takes place in three steps. In the first step, iron and copper nitrates decompose to Fe2O3 and Cu, respectively. Then, Cu changes to CuO and finally CuO reacts with Fe2O3 to form CuFe2O4. The optimized GNP process was then applied on CuxFe3-xO4 spinels to find the optimum x value representing a single phase product with the best conductivity. Electrical measurements in air at 650-800 degrees C showed that the highest electrical conductivity, among CuxFe3-xO4 spinels, belonged to stoichiometric CuFe2O4 compound (7.6 S cm(-1) with 1.5% uncertainty at 800 degrees C). The results of annealing exhibited that the resulting CuFe2O4 spinel is thermally stable and its crystallite growth behavior can be explained by the parabolic grain growth law. The activation energy of the crystallite growth was calculated as 363 kJ mol(-1) with 4% uncertainty. (C) 2016 Elsevier B.V. All rights reserved.
Keywords:CuFe2O4;Spinels;Glycine-nitrate process;Electrical conductivity;Crystallite growth;Calcination