The composite fibers were prepared by an electrospinning the solutions mixed manganese ferrite sol with polyvinyl acetate (PVAc). The manganese ferrite sol was obtained from manganese(II) nitrate and iron(Ill) nitrate nonahydrate molecular precursor based on a sol-gel procedure. Manganese ferrite (MnFe2O4) nanofibers, were prepared by calcining the above composite fibers in air at 400, 600 and 800 degrees C, respectively. The obtained nanofibers were characterized by SEM, FT-IR, XRD, and extended X-ray absorption fine structure (EXAFS). After being calcined at 800 degrees C, the fibers became continuous crystallites as a result of the complete decomposition of PVAc. The morphology of manganese ferrite was found to be cubic spinel structure containing eight oxygens and 12 metal atoms in the unit cell, referred from the results of EXAFS. Also, the magnetic properties of the calcined samples were characterized by using a vibrating sample magnetometer (VSM). (c) 2008 Elsevier Ltd. All rights reserved.