The exhaust gas from vehicle engines and industrial boilers contains considerable amount of harmful nitrogen monoxide(NO) which causes air pollusion and acid rain. To remove NO catalytic reduction processes using Cu ion exchanged ZSM-5 zeolite have been widely studied. In this study, an attempt was made to fabricate Cu/zeolite catalyst by using high energy ball mill. The catalytic performance of ball milled Cu/ZSM-5 zeolites is analyzed and optimum copper contents was determined. The processing variables were reaction temperature and copper contents. Complete removal of NO gas was obtained at the temperature of 553 K on 10wt.% CU/ZSM-5 mechanically alloyed composite powders. Mechanically alloyed CU/ZSM-5 catalyst showed homogeneous distribution of Cu in ZSM-5.