In this paper, iron nanofibers were successfully produced by electrospinning of ferric nitrate-PVA solutions to corresponding PVA/Fe(NO(3))(3) composite nanofibers followed by calcinations and reduction. The thermal stability of the as-prepared PVA/Fe(NO(3))(3) composite nanofibers were investigated by TG-DSC. The morphologies and structures of the as-prepared samples were also characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The results obtained indicated that: the thermal transformation of ferric nitrate and the decomposition of PVA in PVA/Fe(NO(3))(3) composite nanofibers ended at 310 degrees C and 460 degrees C respectively. The as-prepared iron nanofibers showed a continuous morphology and a very high degree of crystallization. Furthermore, the average diameter was about 180 nm. (C) 2011 Elsevier B.V. All rights reserved.