Synthesizing CuFe2O4 Spinel Powders by a Combustion-Like Process for Solid Oxide Fuel Cell Interconnect Coatings

The synthesis of CuFe2O4 spinel powders by an optimized combustion-like process followed by calcination is described herein. The samples were characterized using X-ray diffraction (XRD), differential thermal analysis (TG/DTA), scanning electron microscopy (SEM), dilatometry and 4-probe DC methods. Different glycine to nitrate (G/N) ratios of 1 (fuel-deficient), 1.48 (stoichiometric) and 2 (fuel-rich) were employed. Calcining the asprepared powders at 800 and 1000°C for 5 hours showed that the G/N ratio of 2 results in the formation of the desired copper spinel single phase at both calcination temperatures. For G/N=1, formation of CuFe2O4 takes place in three steps. First, iron and copper nitrates decompose to iron oxide and pure copper. Then, copper transforms to copper oxide and finally, copper and iron oxides react with each other to form a copper ferrite spinel phase. The electrical conductivity and the coefficient of thermal expansion of the sintered pelletized samples were 2 S.cm-1 (800°C) and 11×10-6 °C-1 (25-800°C), respectively.

Computer Aided X-Ray Diffraction Intensity Analysis for Spinels: Hands-On Computing Experience

The mineral having chemical compositional formula MgAl2O4 is called “spinel". The ferrites crystallize in spinel structure are known as spinel-ferrites or ferro-spinels. The spinel structure has a fcc cage of oxygen ions and the metallic cations are distributed among tetrahedral (A) and octahedral (B) interstitial voids (sites). The X-ray diffraction (XRD) intensity of each Bragg plane is sensitive to the distribution of cations in the interstitial voids of the spinel lattice. This leads to the method of determination of distribution of cations in the spinel oxides through XRD intensity analysis. The computer program for XRD intensity analysis has been developed in C language and also tested for the real experimental situation by synthesizing the spinel ferrite materials Mg0.6Zn0.4AlxFe2- xO4 and characterized them by X-ray diffractometry. The compositions of Mg0.6Zn0.4AlxFe2-xO4(x = 0.0 to 0.6) ferrites have been prepared by ceramic method and powder X-ray diffraction patterns were recorded. Thus, the authenticity of the program is checked by comparing the theoretically calculated data using computer simulation with the experimental ones. Further, the deduced cation distributions were used to fit the magnetization data using Localized canting of spins approach to explain the “recovery" of collinear spin structure due to Al3+ - substitution in Mg-Zn ferrites which is the case if A-site magnetic dilution and non-collinear spin structure. Since the distribution of cations in the spinel ferrites plays a very important role with regard to their electrical and magnetic properties, it is essential to determine the cation distribution in spinel lattice.