© 2016 by American Scientific Publishers. GdVO 4 :Eu 3+ nanoparticles were synthesized by a solvothermal method at 200°C for 24 h, followed by calcination at 600°C for 3 h. The effects of mixed solvents (water:methanol, water:ethanol, water:ethylene glycol and water:glycerol) on purity, crystallinity, size and agglomeration behavior of the GdVO 4 :Eu 3+ nanoparticles were investigated. The products, characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and energy dispersive X-ray spectroscopy (EDS), were indexed as pure GdVO 4 with tetragonal structure. Field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM) images revealed that the synthesized powders composed of spherical nanoparticles with diameters of about 15-40 nm. The difference in the characteristics of the synthesized nanoparticles could be related to the properties of the solvents used in the present work. The GdVO 4 :Eu 3+ nanoparticles synthesized using the mixed solvent of water:glycerol was smaller in size with soft agglomerations offering the highest photoluminescence (PL) emission intensity. Whereas, the PL intensity of the nanoparticles synthesized using water:ethylene glycol was lower than those of the others probably due to the existence of some defects in the crystals.