Photocatalysts TiO₂/AC and TiO₂/ACF codoped with Fe and N irons were prepared via the sol-gel method, with butyl titanate as the precursor and, respectively, with activated carbon （AC） and activated carbon fiber （ACF） as the support. The products were then characterized by means of SEM, XRD and UV-Vis. Moreover, the influences of ion-codoping amount, inhibitor species, calcination temperature, carrier species and reuse times on the photocatalytic activities of the catalysts were experimentally investigated, with toluene as a model contamination. The results indicate that （ 1 ） the dispersive effect of TiO₂ on ACF is better than that on AC ; （2） TiO₂embeds into AC pores in the form of paricle but coats ACF surface in the form of film, and the two products are both in an anatase phase ; （3） the codoping of Fe and N ions significantly enhances the adsorption of visible light ; and （4） after a sintering for 2h at 500 ℃ with acetic acid as the inhibitor, the prepared TiO₂/ACF with an ions dosage of 8% possesses the highest photocatalytic activity for gas-phase toluene degradation even if it has been reused for many times.