Inorganic metal oxides having high surface area and pore volume are prepared by spray drying. The admixture which is spray dried to yield the metal oxides is produced from reactants comprising at least one hydrolyzable metal compound, a sufficient amount of water to at least partially hydrolyze the metal compound and an organic solvent. The admixture is supplied as a plurality of droplets to a reaction zone operated under conditions of temperature and pressure below the critical temperature and pressure of the reactants but sufficient to produce a product comprising metal oxide powders and a gas comprising organic solvent vapors. The powders are separated from the gas in a known fashion and collected. Spray drying of non-aqueous systems unexpectedly produces metal oxides having properties generally intermediate conventionally produced oxides and aerogels.