Hierarchical Cd1-xZnxS/TiO2 heterostructures were successfully synthesized by the combination of an electrospinning technique and hydrothermal method. These heterostructures were characterized for the morphological, structural and optical properties by scanning electron microscopy (SEM), energy-dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectra (XPS) and UV-visible (UV-vis) diffused reflectance spectroscopy (DRS). The photocatalytic investigations showed that the Cd1-xZnxS/TiO2 heterostructures possessed enhanced photocatalytic efficiency in photodegradation of Rhodamine B (RhB) under visible light irradiation (degradation efficiency reaches 91% during 60 min), compared with the pristine TiO2 nanofibers (26.5%), hierarchical CdS/TiO2 heterostructures (81.6%), Cd1-xZnxS/P25 composites (77.8%) and pure Cd1-xZnxS nanoparticles (77.3%). The enhanced photocatalytic performance can be ascribed to the beneficial microstructure and synergistic effects of coupled Cd1-xZnxS/TiO2 heterostructures. (C) 2013 Elsevier B.V. All rights reserved.