In order to obtain the nano size composite powders by mechanical alloying method for useful composite catalysis, the effects of mechanical alloying time on the formationof composite powders were analyzed. The phase transformation behaviors were experimented as the heat treating temperature increased. Homogeneous 10wt% Cu-rutile type composite powders were synthesized in 40 hours by mechanical alloying. After 60 hours mechanical alloying 50 nm size powders were obtained. Both the phase of mechanically alloyed 10 wt% and pure powders were not transformed to anatase after annealing at the temperature range between 350 to 500 . The intermetallic compound of O was formed after 10 hours mechanical alloying, however it could be considered that this intemetallic phase dose not prevent the transformation of rutile to the anatase phase after heat treatment at the temperature between 350 and .