TiO 2 nanocrystalline powders with various Zn doping levels from 0 at% to 10 at% were synthesized via sol-gel method with Tetrabutyl orthotitanate (TBOT) and zinc acetate as Ti and Zn source. The samples were characterized by XRD, TEM, EDS and diffuse absorption spectrum. The effect of Zn doping on optical and photocatalytical properties of TiO 2 was systematically investigated. XRD results show that all the prepared powders were Anatase TiO 2 , no ZnO was found when the samples were annealed at 400˚C. EDS analysis confirmed the existence of Zn in the samples. It suggests that Zn was successfully doped into TiO 2 . Average particle size of the prepared Zn-TiO 2 powders was about 6 -7 nm obtained from TEM measurement and Scherer Equation calculation. The nano size powders were used to catalytically decompose methylene blue, and the sample doped with 1 at% Zn showed the best photocatalytic activity, better than that of pure TiO 2 .