The ability of a rapid-heating solvothermal process to synthesize porous nanocrystal assemblies composed of the multiple transition metals was demonstrated. The rapid heating facilitated the quick formation of nascent nanocrystals to generate homogeneous mixed transition-metal oxides. Systematic studies of the synthesis of mixed-metal oxides under various experimental conditions indicated that the present simple method is suitable to develop a wide variety of binary and ternary transition-metal systems such as Co/Mn, Ni/Mn, and Co/Mn/Fe mixed-metal oxides. The products obtained from the rapid heating process were hierarchically assembled porous nanospheres composed of sub-10 nm nanocrystals, which had an extraordinarily high surface area and nano/mesopores. Electrochemical tests revealed the high catalytic ability of the porous nanocrystal assemblies in water oxidation.

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