Thin PVA/magnesium acetate composite fibres were prepared by using sol-gel processing and electrospinning technique. After calcinations of the above precursor fibres, MgO nanofibres with a diameter of 50-150 nm could be successfully obtained. The fibres were characterized by SEM, FT-IR, XRD, respectively. The results showed that the crystalline phase and morphology of MgO fibres were largely influenced by the calcination temperature. (c) 2006 Springer Science + Business Media, Inc.