In this paper, nanocrystalline YVO4:Eu3+ powders have been successfully synthesized via high-temperature solution-phase synthesis process. The nanocrystalline YVO4:Eu3+ particles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), UV/Nis absorption spectra and luminescence spectra, luminescence decay curve and Fourier transform infrared (FT-IR), X-ray photoelectron spectra (XPS) respectively. The as-prepared nanocrystalline YVO4:Eu3+ particles are well crystallized with ellipsoidal morphology. The emission of YVO4:Eu3+ particles show emission originating from the 5D0 level, with 5D0-7F2 at 616 nm as the most prominent group. The excitation spectrum fits basically with the absorption spectrum from the vanadate ions. FT-IR and XPS spectra indicate that the surface ligands of nanocrystalline particles were oleic acid and oleylamine. The lifetime for the luminescence of Eu3+ in the as-prepared YVO4:Eu3+ samples are shorter than that of the bulk material due to the absorption of organic ligands on the nanoparticle surface.