Abstract. Fe-Si alloy with a large Si content of 6.5 wt. % is obtained in nanocrystalline state by mechanical alloying of elemental iron and silicon powders. The mechanical alloying process was carried out using a high energy ball mill in argon atmosphere. Samples were collected after 0.5, 1, 2, 4, 6 and 8 hours of ball milling. The X-ray diffraction (XRD) studies indicate that after 4 hours of milling the Fe-Si alloy is formed. The powder magnetisation decreases upon increasing the milling time up to 4 hours as a consequence of the Fe-Si alloy formation. Upon heating, the DSC studies show the Fe 3 Si compound formation in the samples milled for milling times lower than 6 hours. Also, the Curie temperature of the alloy was evidenced.