Thin PVA/zirconium oxychloride composite fibers were prepared by using sol-gel processing and electrospinning technique. After calcining the above precursor fibers,ZrO 2 nanofibers with a diameter of 70—100 nm were successfully obtained. The ZrO 2 nanofibers were characterized by XRD,TG-DTA,FTIR,and SEM,respectively. The results show that the crystallinity and morphology of ZrO 2 fibers are largely influenced by the calcination temperature.