Magnetic nanofibers of ZnFe2O4/γ-Fe 2O3 composite were synthesized by electrospinning from a solgel solution containing a molar ratio (Fe/Zn) of 3. The effects of the calcination temperature on phase composition, particle size and magnetic properties have been investigated. Zinc ferrite fibers were obtained by calcinating the electrospun fibers in air from 300 to 800 °C and characterized by thermogravimetric analyses, Fourier transformed infrared spectroscopy, X-ray photoemission spectroscopy, X-ray diffraction, vibration sample magnetometry and magnetic force microscopy. The resulting fibers, with diameters ranging from 90 to 150 nm, were ferrimagnetic with high saturation magnetization as compared to bulk. An increase in the calcination temperature resulted in an increase in particle size and saturation magnetization. The observed increase in saturation magnetization was most likely due to the formation and growth of ZnFe2O4/γ-Fe 2O3 diphase crystals. The highest saturation magnetization (45 emu/g) was obtained for fibers calcined at 800 °C. © 2011 Elsevier B.V.