The metalo-organic complexes in the precursor solution were obtained through complexation of the metal and Cr+3 ions with an organic amine, i.e., triethanolamine (TEA), and an aqueous solution mixture of sucrose and polyvinyl alcohol (PVA) provided the polymeric matrix for the dispersion of the metalo-organic complexes. Rapid evaporation of the precursor solution resulted in mesoporous carbon-rich precursor powders, which on calcination at temperatures less than 500°C generated the respective nano-sized, metal chromite powders. The average particle sizes, as measured by X-ray line broadening and transmission electron microscopy studies, were around ∼150−200 Å. That the particles had sizes of the same order as those of crystallite indicated the poor agglomeration of crystallites.