This paper deals with the effects of the surfactant and preplate process (sensitization and activation) on electroless copper plating on carbon nano-fiber (CNF). Ultrasonic irradiation was applied both during dispersion of CNF and during electroless plating containing preplate process. The dispersion of CNF and flatness of the plated copper film were discussed based on the changes in surfactant concentration and preplate process time. It was clearly shown that high concentration of surfactant and long time of preplate process could promote the agglomeration of CNF and uneven copper plating on CNF.