A novel TiO2-xNx/CNFs heterostructured photocatalyst was facilely fabricated by stabilization, NH4OH pretreatment and carbonization of electrospun TiO(OAc)(2)/PAN hybrid nanofibers. The uniformly aligned CNFs were interspersed with 25 wt% of anatase TiO2-xNx nanoparticles, in which the x value or doped N atomic ratio was similar to 0.52%. The TiO2-xNx/CNFs had a considerable surface area of 130 m(2)/g and extraordinary mesoporous morphology. Owing to the synergistic effect between high adsorption capacity of CNFs and excellent vis-photocatalytic activity of TiO2-xNx nanoparticles, the TiO2-xNx/CNFs showed higher photocatalytic efficiency than referenced TiO2/CNFs and TiO2-xNx powders. (C) 2008 Elsevier B.V. All rights reserved.