The sol-gel method ( Sol-Gel) was used to prepare single crystal ZnO，TiO2 thin films and bilayer ZnO·TiO2 composite films on glass substrates and silicon substrates respectively，using zinc acetate ( Zn ( CH3COO) 2H2O) and tincture of titanium tincture ( Ti( OC4H9 ) 4 ) as zinc source and titanium source．The results showed that the monolayer intrinsic ZnO and TiO2 films grew along ( 02) and ( 101) crystal planes respectively，and the preferred orientation growth was the most obvious when the concentrations of intrinsic ZnO and TiO2 were 0．45 mol /L and 0．65 mol /L respectively．The ( 101) and ( 04) characteristic peaks of ZnO· TiO2 composite films were obvious，and the crystallization quality of double-layer ZnO·TiO2 composite films was the best when 0． 45 mol /L /0． 55 mol /L． The film surface was the flattest，the particles were evenly distributed and the adhesion was the least．The absorption of ultraviolet light was the strongest，and the band gap is 3．39 eV．