A sol-gel hydrothermal method was developed to synthesize peroxo-titania powders and their photooxidation performances were conducted in aqueous methanol solution under visible light irradiation. Three kinds of peroxo-titania were developed using TiO(2) and H(2)O(2) containing precursor sol with different dispersion mediums such as NH(3) aq NaOH aq, or pure water. Peroxo-titania powder prepared with NH(3) aq showed highest photooxidation activity. Moreover, we found unique photofunctional properties: together with formaldehyde production, the photo-excited electron also triggers oxygen evolution, although by TiO(2) (Degussa P-25) photocatalysis H(2) evolution was observed from the same solution.