In this paper, α-Fe2O4@ZnO nanoparticles (NPs) were synthesized by coprecipitation method in the presence of PVP and EG surfactants. The samples were charactrized by x-ray fluorescence (XRF), x-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), and fourier transform infrared spectroscopy (FTIR). The XRD results exhibited rhombohedral α-Fe2O3 and wurtzite structure of ZnO. The SEM images showed that the NPs changed from rod-shape to nanoleaves particles after heat treatment. The TEM studies displayed the formation of Fe2O3@ZnO core-shell of as-synthesized NPs. The stretching vibrations peaks in FTIR in the wavenumber of 532 cm-1 and 473 cm-1 ascribed to the Fe and Zn groups. The XRF data indicated decreasing of the Fe weight percent from 22 %Wt. to 25 %Wt., after heat treatment.