A methanol-water mixed solvent was used as a reaction medium for the preparation of Eu 31 -doped YVO 4 phosphor materials. These were synthesized by a solvothermal method at 1501-3001C using a 10 vol% solution of water in methanol as the reaction medium followed by calcination at 10001-12001C. The phase composition and optical properties of the products were characterized by X-ray diffraction, scanning electron microscope, and photoluminescence spectroscopy. The powders obtained were composed of spherical particles B0.5 lm in size, with an internal structure that was different for samples prepared under subcritical and supercritical conditions of methanol. After the calcination, the powders obtained at 2401-3001C retained the initial raspberry-like morphology, whereas the morphology of samples prepared at 1501-2101C changed significantly due to noticeable sintering. The fluorescence intensity exhibited by the prepared samples was higher than the fluorescence intensity shown by one of the best commercial YVO 4 :Eu phosphors having a large particle size.