Abstract: YVO₄:Eu³⁺ nanocrystals with a different Eu³⁺ concentration have been synthesized by precipitation method. X-ray diffraction and luminescence spectra were used to characterize the structure and luminescence properties. The results of XRD indicate that YVO₄: Eu³⁺ nanocrystals obtained at lower temperature is tetragonal zircon structure, and the crystallite size is about 7 nm. The results of excitation and emission spectra show that the broad excitation band is assigned to charge transfer band of Eu-O and V-O, the emissions peaks are from 5D0-7FJ transitions. The quenching concentration in nanocrystalline YVO₄:Eu³⁺ is about 12 %.The luminescence lifetimes of nanoparticles become shorter with the increasing Eu³⁺ ions concentration.