Tetragonal copper ferrite (CuFe 2O 4) nanofibers were fabricated by electrospinning method using a solution that contained poly(vinyl pyrrolidone) (PVP) and Cu and Fe nitrates as alternative metal sources. The as-spun and calcined CuFe 2O 4/PVP composite samples were characterized by TG-DTA, X-ray diffraction, FT-IR, and SEM, respectively. After calcination of the as-spun CuFe 2O 4/PVP composite nanofibers (fiber size of 89 ± 12 nm in diameter) at 500 °C in air for 2 h, CuFe 2O 4 nanofibers of 66 ± 13 nm in diameter having well-developed tetragonal structure were successfully obtained. The crystal structure and morphology of the nanofibers were influenced by the calcination temperature. After calcination at 600 and 700 °C, the nature of nanofibers changed which was possibly due to the reorganization of the CuFe 2O 4 structure at high temperature, and a fiber structure of packed particles or crystallites was prominent. Crystallite size of the nanoparticles contained in nanofibers increases from 7.9 to 23.98 nm with increasing calcination temperature between 500 and 700 °C. Room temperature magnetization results showed a ferromagnetic behavior of the calcined CuFe 2O 4 samples, having their specific saturation magnetization ( M s) values of 17.73, 20.52, and 23.98 emu/g for the samples calcined at 500, 600, and 700 °C, respectively.