In order to more easily separate TiO2 photocatalyst from the treated wastewater, TiO2 film was immobilized on the surface of activated carbon fibers (ACFs) by employing two kinds of coating procedures, dipcoating, and hydrothermal treatment. The effects of coating procedures on microstructure of TiO2-coated ACFs (TiO2/ACFs), such as morphology, porous property, crystal structure, and light absorption characteristics were investigated in detail. The adhesion property between TiO2 film and ACFs was evaluated by ultrasonic vibration, and the photocatalytic activity of TiO2/ACFs was tested by the photocatalytic decoloration of methylene blue solution. The results show that hydrothermal treatment presented many advantages to obtain high-performance TiO2/ACFs photocatalyst in comparison with dip-coating. Hydrothermal treatment could improve the binding property between TiO2 films and ACFs, which endowed the as-obtained TiO2/ACFs photocatalyst with improved reusable performance, and TiO2/ACFs synthesized by hydrothermal treatment presented higher photocatalytic activity. (c) 2012 Elsevier Inc. All rights reserved.