In this paper, nickel nanofibers were prepared by electrospinning polyvinyl alcohol/nickel nitrate precursor solution followed by high temperature calcination in air and deoxidation in hydrogen atmosphere. The thermal stability of the as-electrospun PVA/Ni(NO3)(2) composite nanofibers were characterized by TG-DSC. The morphologies and structures of the as-prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field-emission scanning electronmicroscope (FE-SEM) and field-emission transmission electron microscopy (FE-TEM). The hysteresis loops (M H loops) were measured by Physical Property Measurement System (PPMS). The results indicate that: the PVA and the nickel nitrate were almost completely decomposed at 460 degrees C and the products were pure nickel nanofibers with face-centered cubic (fcc) structure. Furthermore, the as-prepared nickel nanofibers had a continuous structure with rough surface and high degree of crystallization. The average diameter of nickel nanofibers was about 135 nm. The nanofibers showed a stronger coercivity of 185 Oe than value of bulk nickel. (C) 2013 Elsevier Ltd. All rights reserved.