Microstructure of single-phase cobalt and manganese oxide spinel Mn3−xCoxO4 ceramics

This paper reports microstructural studies of single-phase Mn3−xCoxO4 (0.98 ≤ x ≤ 2.93) spinel ceramics using transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDX). These ceramics were obtained by conventional sintering or by spark plasma sintering (SPS) of powders prepared by thermal decomposition of coprecipitated oxalate precursors. For x < 1.78 or x ≥ 1.78, the monophasic ceramics correspond respectively to quadratic (Q) or cubic (C) spinel structure. The ferroelastic character of the structural phase transition from C to Q is highlighted by specific microstructural features. The effect of chemical composition and heat treatment conditions on the microstructure and essentially on the presence and the characteristics of twins were investigated. The coherent twin interfaces are parallel to (1 1 2) planes in the Q cell. Twins can correspond to: tweeds, single lamellae (widths: 5–306 nm) arranged parallel to each other, large lamellae (widths: 69–928 nm) internally twinned and sometimes arranged in cyclic forms (triangular shapes).