powder was easily prepared from and in an aqueous nitric acid solution at room temperature. The obtained crystal structure depended on the molar ratio of to , which is the concentration and volume of an aqueous nitric acid solution. with monoclinic scheelite structure formed using starting materials, in which the molar ratio of to was 1:1. When the molar ratio was 4:3, with tetragonal zircon structure was obtained. Although with monoclinic scheelite structure was platelike particles reflecting the crystal structure, the thickness of the particle increased with an increase in the concentration of an aqueous nitric acid solution. The obtained with monoclinic scheelite structure showed good photocatalytic performances for evolution and methylene blue degradation under visible-light irradiation.