Abstract: Blending the nano-tin (Sn) and polyacrylonitrile (PAN) to prepare Sn/PAN nanofibers by electrospinning. And using a scanning electron microscope and X-ray diffraction method, characterize the average diameter of fiber, distribution of diameter, distribution of Sn in the fiber and the degree of crystallinity after Sn electrospinning. The results showed that the degree of crystallinity increased after PAN electrospinning; the fiber diameter decreases with the spinning voltage increases or the distance increases; when the electrostatic spinning voltage is 14kV, solidification distance is 14cm, the average diameter of fiber is small and the distribution is uniform; Sn reunions when added to the PAN electrospinning, degree of crystallinity decreased; with the PAN stretched in the electrostatic field, lattice of Sn distorted. After electrostatic spinning, the XRD diffraction peaks of Sn slightly offset than the standard peaks.