Abstract A series of TiO 2/ACF samples were prepared by sol–gel-adsorption method and were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and nitrogen adsorption. SEM showed that calcined temperature had an important influence on final structure morphologies of TiO 2 films. XRD analysis implied that all samples presented anatase structure, carbon surfaces located under TiO 2 film could influence the crystalline degree of TiO 2. Nitrogen adsorption measurement indicated that some pores located in activated carbon fiber (ACF) were covered by TiO 2 film. Photocatalytic degradations of methyl orange solution and acid fuchsine solution showed that dye compounds could be removed rapidly from water by TiO 2/ACF samples because of dual functions: absorption of ACF and photocatalytic degradation of TiO 2 film, and there was a matched relation between pore diameter of immobilized sample and molecular size of dye compound.