Thin PVA/nickel acetate composite fibers were prepared by using sol-gel processing and electrospinning technique. After the calcination of the above precursor fibers,NiO nanofibres with a diameter of 50—100 nm could be successfully obtained. The fibers were characterized by TG-DTA, FT-IR,WAXD and SEM respectively. The results showed that the crystalline phase and morphology of NiO fibres were greatly influenced by the calcination temperature. [WT5HZ]