Gd2Si2O7:Eu3+ nanoparticles were prepared by the sol-gel method with citric acid as an additive in the precursor solutions. The crystal structure was analyzed by means of X-ray diffraction (XRD). The results indicate that the alpha-Gd2Si2O7 powders in size 35 nm are obtained at a synthesis temperature of 1,100 degrees C, and the doping ion contents do not influence the crystal structure. The excitation and emission spectra of samples were measured. The dependence of photoluminescence intensity and lifetime of level on Eu3+ concentration and synthesis temperature of samples are also discussed.