Abstract: Nano-zinc and nano-Fe3O4 particles were prepared by using roller vibration dry method at room temperature and chemical coprecipitation respectively,and then ZnFe2O4 nano-particles were obtained through the hydrolysis reaction of zinc and Fe3O4.The particles were characterized by XRD,TEM and Mssbauer spectra.The results show that the average paticle sizes of nano-zinc,nano-Fe3O4 and nano-ZnFe2O4 were 40,20 and 40 nm respectively.The particle size of ZnFe2O4 was homogenous when the reaction temperature was 300 ℃,however,Fe2O3 appeared obviously.According to the Mssbauer spectra,there were 3 sextets.