Cu/C films were prepared at ambient temperature under a Cu(hfac)(2)-Ar-H-2 atmosphere in order to obtain metallized polymer by using electron cyclotron resonance metal organic chemical vapor deposition(ECR-MOCVD) coupled with a direct current (DC) bias system. DC bias selectively attracts the positively charged copper ions and then makes them deposit on the polymer substrate. Structural analysis of the films by ECR showed that fine copper grains were embedded in an amorphous polymer matrix. The electrical properties of the films were closely related to the process parameters such as microwave power, magnet current, H-2/Ar mole ratio and periodic negative voltage. The increase in H-2 contents, microwave power, magnet current and the negative voltage brought on copper-rich film formation with low electrical resistance. On the other hand carbon-rich films with low sheet electrical resistance were prepared with lower values for process parameters described above. Formation of Cu/C films depends strongly on the periodic negative pattern of DC bias and the electrical sheet resistance of the films was controlled in the 10(8)-10(0) ohm/sq range by process parameters of the ECR-MOCVD system.