Room-temperature synthesis of monodisperse mixed spinel (Co_xMn_1–x)₃O₄ powder by a coprecipitation method

Abstract

Spinel oxide Co₃O₄ has traditionally been synthesized by thermal decomposition of cobaltous salts at temperatures of 250-900°C under oxidizing conditions. Here, we report a solution synthesis route that yields mixed spinel oxide (Co_xMn_1–x)₃O₄ at room temperature in air. (Co_0.75Mn_0.25)₃O₄ solid solutions were synthesized by coprecipitation and oxidation of Co(OH)₂ and Mn(OH)₂ from mixed aqueous solutions of Co- and Mn-salts. The spinel oxide phase was stabilized by crystallization of Mn₃O₄ resulting from the oxidation of Mn(OH)₂ in the mother liquor. While undoped Mn₃O₄ is tetragonal, the (Co_0.75Mn_0.25)₃O₄ solid solution has a cubic symmetry due to the reduced Mn3+ concentration. The resulting powder is spherical with an average particle diameter of ca. 0.1 µm and a narrow size distribution. Transmission electron microscopy (TEM) showed that individual particles are nearly single crystalline but consist of a mosaic of multiple nanocrystallites. This observation supports an aggregation mechanism of formation for the nearly monodispersed particles.

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