Abstract. Fe₆₀Co₄₀ alloys were fabricated by the mechanical alloying process with the periods of 1, 2, 4, 6, 12 and 24 hours, respectively. The structural variations during the formation of the alloy were examined by the X-ray diffraction and the extended X-ray absorption fine structure. The activation for structural transform begins in 6 hour milling. Substantial structural changes were observed in 12 hour milling. The alloying process was almost completed in 24 hours. EXAFS analysis showed that BCC shells appeared in the alloy milled for 6 hours. The magnetization increased as milling time increased.