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Micro/mesoporous nanoparticles, such as SiO2, TiO2, ZnO, ZrO2, and CeO2, were successfully prepared by one-pot single-step reaction in supercritical alcohols from silicate, metal alkoxides, or metal salts with carboxylic acids.1-4 Not only solid but also hollow nanoparticles were prepared by simply changing carboxylic acid, reaction temperature, and/or heating rate of the reaction mixtures.