Zinc ferrite (Fe2O3/ZnO) nanocomposites were successfully synthesized by simple co-precipitation method via iron (III) nitrate 9-hydrate (Fe(NO3)3.9H2O) and zinc nitrate hexahydrate (Zn(NO3)2.6H2O) as precursor in the presence of cetyltrimethylammonium bromide (CTAB) surfactant. The samples were characterized by high resolution transmission electron microscopy (HRTEM), field effect scanning electron microscopy (FESEM), X-ray diffraction (XRD), X-ray florescence (XRF) and Fourier transform infrared spectroscopy (FTIR) in different temperature. The XRD results showed that Fe-doped ZnO was single-phased with a hexagonal wurtzite structure ZnO and spinel phase of rhombohedral α-Fe2O3. The particle size of as-prepared sample was in the range size of 30-40 nm and annealed one was around 37 nm in diameter at 500 oC for 3 hours. The TEM studies showed the rod-like shaped nanosized particles. The sharp peaks in FTIR spectrum determined the element of Fe-Zn nanoparticles. The result of XRF analysis showed the peaks of iron and ferrite elements with less Cl, F and Ni impurities.