Spherical YVO4:Eu3+ microstructures were hydrothermally synthesized by the reaction of NH4VO3,Y2O3, and Eu2O3 at 180 degrees C for 24h with the assistance of polyvinyl pyrrolidone (PVP)as a surfactant. The resulting products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and photoluminescence (PL) spectroscopy. The experimental results showed that ball-like YVO4:Eu3+ microspheres with a diameter of about 4-5 mu m, corresponding to the SEM observations, formed at 180 degrees C for 24 h using 0.2 g PVP with the molecular weight of 20,000 g mol(-1). The amount of PVP and the reaction time of hydrothermal processing were found to play a key role in the formation of YVO4:Eu3+ microspheres. It has been observed that the relative luminescence intensities of the as-synthesized samples increased with increasing hydrothermal reaction times due mainly to the increase of crystallinity. (C) 2009 Elsevier B.V. All rights reserved.