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This paper prepares pure TiO2 nanoparticles and TiO2 nanoparticles doped with different tin contents using sol-gel method, characterizes the structure of the samples using XRD, UV-Vis and surface photovoltage spectroscopy (SPS), analyzes the effects of annealing temperature and Sn4+ doping amount on the surface photoelectric properties of TiO2 nanoparticles, and discusses the mechanism of the effect of Sn4+ doping on the surface photoelectric properties of TiO2 nanoparticles. The experimental results show that the tin ion doping can significantly increase the surface photovoltage of the TiO2 nanoparticles, while 3 mol% is the optimal doping concentration for tin ion.