Al/B4C composites with 0 wt.%, 5 wt.% and 10 wt.% of B4C were prepared by powder metallurgy and their properties were characterised successfully. Investigation of the effect of milling times (4, 8, 12, 16 hours) on microstructure, phase identification, hardness and neutron attenuation coefficient of composites has been studied. The results showed that hardness increased with increased of milling time, with maximum hardness obtained at 16 hours milling time. The increment is slower as the composition of B4C increased. The hardness of Al/10%B4C, Al/5%B4C and Al/0%B4C were 81.7, 78.7 and 61.2 HRB respectively. Morphology of scanning electron microscopy (SEM) showed that microstructures play important role in controlling the hardness. Meanwhile, x-ray diffraction (XRD) analysis showed the phases and crystalline present in composites with an indication that crystalline of the grain increased as the milling time increased. Neutron absorption of Al/10%B4C composites showed that this composite has the highest attenuation coefficient, thus indicating that it is the best composites for neutron shielding.