Thin PVA/manganese acetate composite fibers were prepared by using sol-gel processing and electrospinning technique. After calcinations of the above precursor fibers, Mn2O3 and Mn3O4 nanofibers with a diameter of 50-200 nm could be successfully obtained. The fibers were characterized by TG-DTA, Scanning electron microscopy, FT-IR, WAXD, respectively. The results showed that the crystalline phase and morphology of nanofibers were largely influenced by the calcination temperature. (C) 2004 Elsevier Inc. All rights reserved.