For the first time, nanofibers of PVA/nickel acetate/zinc acetate composite were prepared by using sol-gel processing and electrospinning technique. By high temperature calcinations of the above precursor fibers, nanofibers of NiO/ZnO composite with diameters of 50-150 nm could be successfully obtained. The fibers were characterized by TG/DTA, IR, XRD and SEM. The results showed that the crystallinity and the morphology of the fibers were largely influenced by the calcination temperature. (C) 2004 Elsevier B.V. All rights reserved.