Ultrafine crystalline spinel powder has been prepared using flame spray pyrolysis of alcoholic solutions of a novel double alkoxide precursor. The particles produced are spherical, dense, single crystals with diameters of 10–100 nm and specific surface areas ranging from 40 to 60 m2/g. Powder production rates of 50–100 g/h are achieved using a bench‐top apparatus. Particle formation appears to occur by rapid oxidation of the organic ligands followed by nucleation and growth from oxide species.

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