Composite nanofibers with a weight ratio of 30%NiO-70%SiO2 and diameters ranging from 80 to 100 nm were successfully prepared by electrospinning a precursor mixture of polyvinyl alcohol (PVA)/silica/nickel acetate followed by calcination treatment of the electrospun polymer/inorganic composite fibers. The resulting NiO/SiO2 composite nanofibers were characterized by TG-DTA, FT-IR spectroscopy, X-ray diffraction and scanning electron microscopy. The results revealed that the crystalline phase of NiO nanoparticles were formed at a temperature higher than 600 degrees C. The SEM results show that the morphology of the fibers is affected greatly by the calcination temperature. (C) 2009 Elsevier Ltd. All rights reserved.