NiO, ZnO and NiO-ZnO/polysulfone composite nanofibers have been fabricated by electrospinning technique using a solution containing metal acetate and polysulfone. Metal oxide/polysulfone composite fibers were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, UV-VIS absorption and emission spectra, and rheological measurements. The crystallinity of these nanofibers improved with the increase in annealing temperature. XRD data revealed that ZnO nanofibers with pure wurtzite structure and NiO nanofibers having a pure crystalline structure with cubic phase were obtained. The emission spectra of metal oxide/polysulfone nanofibers were analyzed as a function of excitation wavelength. (C) 2014 Elsevier B.V. All rights reserved.