A novel synthetic process has been developed to fabricate the magnetic alloy/spinel ferrite composite nanofibers. By employing the electrospinning technique and subsequent partial reduction, Fe-Ni alloy/ nickel ferrite composite nanofibers with an average diameter of around 170 nm were successfully prepared. The synthesized composite nanofibers consist of the face centered cubic and body centered cubic phases of Fe-Ni alloy and the spinel phase of nickel ferrite, and have novel magnetic properties with much enhanced coercivity and saturation magnetization as compared with the pristine nickel ferrite nanofibers. (C) 2010 Elsevier Ltd. All rights reserved.