A thin PVA/FeCl3 composite fiber was prepared by using sol-gel processing and electrospinning techniques. A nanofiber of α-Fe2O3 with the diameter of 50150 nm was obtained via high temperature calcination of the PVA/FeCl3 composite fiber. The material was characterized by infra-red（IR） spectroscopy, X-ray diffraction（XRD）, and scanning electron microscopy（SEM）. The results show that the fiber after the calcination at 700 ℃ was a pure α-Fe2O3 nanofiber.
