Al/AlN composites were synthesized by mechanical alloying using process control agents(PCAs). Three different PCAs which contain N element, were examined to see the effectiveness of ball-milling and the nitridation during sintering. Among examined PCAs, $C_8H_6N_4O_5$ was the most effective to facilitate ball-milling and to form nitrides during a subsequent sintering. By a proper control of ball-milling and sintering, we could obtained surface-hardened Al-based composites.