Structural and magnetic properties of Fe₅₀Mn₅₀ nanocrystalline alloys prepared by the mechanical alloying technique (using commercial Fe and Mn powders as the precursors) are studied as a function of milling time, 1hr to 48 hrs. The nano-crystallite size and shape are examined by using scanning electron microscopy (SEM). The effect of milling time on structural characterization was investigated using X-ray diffractometer (XRD) and extended X-ray absorption fine structure spectroscopy (EXAFS). Both XRD and EXAFS studies showed that the alloying process should be completed after 36 hrs milling. Concerning the magnetic behavior, the data obtained from superconducting quantum interference devices (SQUID) exhibited both magnetic saturation (M_s) and coercivity (H_c) depend strongly on the milling time, which are related to the changes in the crystallite size and magnetic dilution.