One-dimensional (1D) CuO/In 2 O 3 heterostructured nano¯bers with the diameter of about 300 nm were successfully prepared through combining a facile single-capillary electrospinning with sintering process, and investigated by thermogravimetric and di®erential scanning calorimetry (TG-DSC), X-ray di®raction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) techniques, etc. The photocatalytic activities were examined by degrading methylene blue (MB) under 500W xenon lamp, halogen lamp and mercury lamp irradiation, respectively. The heterostructured nano¯bers exhibited a higher photocatalytic activity than P25-TiO 2 under 500W xenon lamp irradiation due to the enhanced absorption for visible light and the e±cient electron-hole separation and transportation. The single CuO micro¯bers and In 2 O 3 nano¯bers were also prepared as the control groups by the same method.