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In the present study, the nanostructured Fe(Al,Cu) solid solution was synthesized by mechanical alloying (MA) process of the elemental powders. The powder mixtures were milled in a planetary ball mill for various periods of time, up to 50 h. The structural and mechanical properties of the samples were studied by using X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM/EDX) and Vickers microhardness test. Results indicated that after 10 h of milling, all Al and Cu atoms were dissolved into the Fe lattice to form bcc-Fe(Al,Cu) solid solution. The particle morphology of the alloys was followed the cold welding, fracturing and steady state stages during milling times. Both particle size and crystallite size were reduced to ~500 nm and ~6 nm, respectively after 50 h of milling. However, the microhardness values increased with the increasing milling time.