Gd2Zr2O7 nanoparticles were synthesized by the reverse titration co-precipitation method. The influence of calcining temperature, calcining time, system temperature, pH value, initial concentration and surfactant content on the phase transformation, grain morphology and size was analyzed by XRD, SEM, TEM and TG-DSC. The results show that the five factors of Gd2Zr2O7 have no effect on the phase change, the powders are approximately spherical particles with even particle size of about 40 nm under the condition of calcining at 1100°C for 3 h, when using ammonia as the precipitator to process the experiment by the reverse titration, the co-precipitation temperature is at 0°C, the initial concentration of mother liquor is 0.01 mol/L, the pH value is controlled at 11 and the amount of surfactant(SDBS) is 2wt%.