One-dimensional 2,9,16,23-tetra-nitrophthalocyanine iron(II) (TNFePc)/TiO2 nanofiber heterostructures have been successfully obtained by a simple combination of electrospinning technique and solvothermal process. The as-obtained products were characterized by field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray (EDX) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and IR spectrum. The results revealed that the TNFePc nanosheets were successfully grown on the primary TiO2 nanofibers. And, the coverage density of the secondary TNFePc nanostructures could be controlled by adjusting the experimental parameters. Photocatalytic tests displayed that the H2O2 assisted TNFePc/TiO2 nanofiber heterostructures (TNFePc/TiO2-H2O2) possessed a much higher degradation rate of methyl orange than the pure TiO2 and TNFePc/TiO2 nanofiber without H2O2 under visible light. Moreover, the TNFePc/TiO2 nanofiber heterostructures could be easily recycled without the decrease of the photocatalytic activity due to their one-dimensional nanostructural property of TiO2 nanofibers. (C) 2012 Elsevier B.V. All rights reserved.