An effective powder metallurgy route has been used to develop new Al/B4C (0, 0.5, and 1 wt. %) nanocomposites. Following 4 h of optimized mechanical milling, particle size measurements verified for the pure Al, Al/B4C (0.5 wt. %), and Al/B4C (1 wt. %) samples as 65, 54, and 51 nm, respectively and these values are well corroborated to the crystal size measurement by XRD for the respective samples. Then the compacted (at 200 MPa) samples were sintered at an argon atmosphere at 550 °C for 3 h. Because of the homogeneous dispersion of 1 wt. % B4C in Al, the intensity of the Al peaks is significantly reduced in the XRD pattern of Al/1 wt. % B4C composite, which indicates the proper composite formation between Al and B4C. It is marked that the reinforcement of B4C enhanced the morphology of pure Al. Reinforcement of only 1 wt. % B4C in Al was found to enhance its microhardness value from 45 to 112 VHN (about 148 % increment).