In general, conventional carbon fiber surface pretreatment, with palladium, silver, and other precious metals as activators, increases its surface activity by initiating redox reactions for metallization, whereas it exhibits a high cost and poor economy. In this study, copper-nickel mixed colloids with low cost served as the activators, and sodium borohydride (NaBH4) and sodium hydroxide (NaOH) were employed as sensitizing reducing agents to successfully plate copper on the surface of carbon fibers. Subsequently, the morphology of the treated samples was characterized through SEM and XPS to explore the pretreatment process of the carbon fiber surface. The results indicated that the carbon fiber exhibited the optimal debinding effect at 55°C and the heating time was longer than 120 min. The result indicated that coarsening effect of 65% concentrated nitric acid was the optimal. The activation effect of copper-nickel mixed colloid was the optimal, and the surface quality of the coating was the optimal.