Abstract:?β-FeSi2 films were formed on Si substrate from Fe/Si nano-multilayers by magnetron sputtering. The samples were characterized by X-ray diffraction, Raman scattering, and Atom Force Microscopy (AFM). Research results indicate that ?-FeSi2 films were formed with the Fe/Si ratio of 1/2 under the annealing temperature of 750 ℃, the average size of the grains is about 50nm, and the grains present a uniform distribution. It was also revealed that if the thickness ratio of Fe/Si is 1/1 or 3/10, ε- Fe/Si. When the annealing temperature is increased to be 1000 ℃, high temperature phase ?-FeSi2 is formed.