Powders of magnetic iron oxide nanoparticles (Mg0.2Ca0.8Fe2O4) were prepared by a sol–gel method using ethylene glycol and nitrates of Fe, Ca and Mg as starting materials. Those powders were heat treated at different temperatures (573, 673, 773 and 873K). In order to evaluate the effect of the heat treatment temperature on the nanoferrites properties, X-ray diffraction (XRD), vibrating sample magnetometry (VSM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) techniques were used. It was found that the reaction products exhibit nanometric sizes and superparamagnetic behavior. It is also demonstrated that, as the heat treatment temperature increases, the particle size and the saturation magnetization of the nanoferrites are increased.