Abstract: The precursor solution was prepared with AgNO₃ and NH₄VO₃ as raw materials, and solvothermal reacted at different temperatures for different times. Then the products were sintered at 600℃ and the Ag₃VO₄ powder was obtained. The morphology and phase composition of the powder were studied and the relatively optimal reaction temperature and time were determined. The structure and photoluminescence property of the powder were also analyzed. The results show that the relatively optimal reaction temperature of Ag₃VO₄ powder was 180℃ and the time was 12 h. Under this condition, the synthesized Ag₃VO₄ powder was microrod-like with the diameter of 2-3 μm. The powder had a mesoporous structure with the pore size of about 27 nm and the specific surface area of 1 181 m²·g^-1. The fluorescence emission peak of Ag₃VO₄ powder was in the wavelength range of 521-595 nm and the emission peak strength at 553.1 nm was the highest, showing a good photoluminescence property.