Thin PVA/cobalt acetate composite fibers were prepared by using sol-gel processing and electrospinning technique. After calcination of the above precursor fibers, Co3O4 nanofibers with a diameter of 50-200 nm were successfully obtained. The fibers were characterized by scanning electron microscopy, FT-IR, wide-angle X-ray diffraction, respectively. The results showed that the crystalline phase and morphology of the as-prepared fibers were largely influenced by the calcination temperature. (C) 2003 Elsevier B.V. All rights reserved.