To improve the photocatalytic activity of ZnC-SnO2 (Z-S) coupled nanofibers, mesoporous ZnO-SnO2 (M-Z-S) coupled nanofibers were prepared via electrospinning technique. The samples have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), nitrogen adsorption-desorption isotherm analysis and surface photovoltage spectroscopy (SPS). Methyl orange (MC) was used to evaluate the photocatalytic properties based on the samples. Experimental results showed that the further improved photocatalytic performance had been observed on the M-Z-S coupled nanofibers. (C) 2009 Elsevier B.V. All rights reserved.