Among the reported nanostructural shapes, nanofibers have special interest due to the long axial ratio which has a distinct impact on many chemical and physical properties. In this study, synthesis of the desirable maghemite iron oxide (c-Fe 2 O 3 ) nanofibers is introduced. Calcination of electrospun mats composed of ferrous acetate and poly(vinyl alcohol) in argon atmosphere resulted in producing maghemite nanofibers. Detailed characterization affirmed that the obtained c-Fe 2 O 3 nanofibers are free of other iron oxides. Due to the axial ratio impact, the synthesized nanofibers which have an average diameter of *70 nm do have magnetic properties resemble c-Fe 2 O 3 nanoparticles having an average diameter of *5 nm. Accordingly, the produced nanofibers are considerable candidate for biomagnetic separation of the biomaterials. The prepared c-Fe 2 O 3 nanofibers can be easily handled as they were obtained in the form of strong mats. Electrical properties study indicated that the introduced nanofibers behave as a semiconducting material. Moreover, the synthesized c-Fe 2 O 3 nanofibers have band gap energy of *4.2 eV. Based on the simplicity, effectiveness, highyield, and low-cost features of the utilized preparation process and the studied physiochemical properties of the obtained product, the synthesized c-Fe 2 O 3 nanofibers might have considerable application fields.