Activated carbon (AC)-supported TiO2 catalysts were prepared by sol-gel and metal organic chemical vapor deposition (MOCVD) in order to investigate effect of preparation methods on the structure and catalytic performance of TiO2/AC catalysts. It was found that both methods yield "egg-shell" TiO2/AC catalysts, that is to say, the TiO2 coatings were mainly on the surface of AC supports. The TiO2 coating by sol-gel was only coated on the external surface of AC. In contrast, TiO2 by MOCVD was deposited on the surface of AC through the heterogeneous reaction, forming a TiO2 + AC hybrid film (about 3 mu m) as evidenced by SEM and N-2 adsorption tests. The hybrid TiO2 + AC film could capture the intermediates produced during the degradation of the target pollutant resulting in efficient mineralization. The TiO2/AC catalysts by MOCVD exhibited a Ti-O-C bond, which correlated with the good stability of TiO2 as observed on the corresponding samples. These results indicate MOCVD is a better choice for the preparation of TiO2/AC catalysts. (c) 2007 Elsevier B.V. All rights reserved.