Core/shell type nanoparticles with an average diameter of 20nm were synthesized by chemical precipitation method. Firstly, Monodisperse Fe3O4 nanoparticles were synthesized by solvethermal method. FeSO47H2O and NaBH4 were respectively dissolved in distilled water, then moderated Fe3O4 particles and surfactant(PVP) were ultrasonic dispersed into the FeSO47H2O solution. The resulting solution was stirred 2 h at room temperature. Fe could be deposited on the surface of monodispersed Fe3O4 nanoparticles to form core-shell particles. The particles were characterized by using various experimental techniques, such as transmission electron microscopy (TEM), X-ray diffraction (XRD), AGM and DTA. The results suggest that the saturation magnetization of the nanocomposites is 100 emu/g. The composition of the samples show monodisperse and the sides of the core/shell nanoparticles are 20-30nm. It is noted that the formation of Fe3O4/Fe nanocomposites magnetite nanoparticles possess superparamagnetic property.