Carbon/manganese ferrite (C/MnFe2O4) composite nanofibers were fabricated using electrospinning technique followed by carbonization process under mixed of air and argon atmosphere at 400, 600 and 800 degrees C, respectively. The prepared composite nanofibers were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), vibrating sample magnetometry (VSM) and X-ray absorption spectroscopy (XAS) including X-ray absorption near edge structure ()(XANES) and extended X-ray absorption fine structure (EXAFS). After calcination at 800 degrees C, the composite nanofibers of C/MnFe2O4 were obtained with a mean diameter of nanofibers of approximately 700-800 nm. The structure of MnFe2O4 was successfully studied using XAS technique and was found to be cubic spinel with a coupling of Mn-2/Mn3+ and Fe3+ oxidation states. All composite nanofibers exhibited ferromagnetic behavior especially after being calcined at 800 degrees C. This ferromagnetic properties were related to the distribution of cations over tetrahedral and octahedral sites as revealed by EXAFS results. (C) 2015 Elsevier B.V. All rights reserved.