Mechanical alloying, cold pressing, and sintering were used for synthesizing bulk copper, copper‐iron, and copper‐iron‐silicon carbide nanomaterials. The precipitation of iron during sintering of the supersaturated mechanically alloyed powder significantly enhanced the thermal stability of the nanocomposite against grain growth. Moreover, the hardness of sintered composites was found to increase with increasing milling time, which was attributed to the work‐hardening, crystallite refinement, and increasing the relative density (decrease in porosity). Although the addition of silicon carbide did not affect the mean crystallite size of the bulk samples, it effectively increased the hardness of the nanocomposite based on its composite strengthening effect.