AbstractA new nickel activation process was developed for metalizing the carbon fiber (CF) surface with electroless nickel plating. The oxidation and activation processes were examined using X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectrometry (EDS), and X-ray Diffractometry (XRD). XPS analysis showed that HNO3 oxidation improved the O/C ratio of the CF surface, which resulted in an increase in the amount of oxygen-containing groups. As activation time increased, both Nio cluster and Ni-P deposits increased. More than 50 mg of Nio clusters formed on the surface of 1g CF. SEM observations illustrated that particles and island-like shapes were developed from the Nio cluster, which helped to initiate the electroless nickel-plating on the CF surface. A continuous and compact coating with a thickness of about 2 to 3 μm was obtained. EDS results showed that the nickel and phosphorus content in the deposits was 97.34 wt.% and 2.66 wt.%, respectively. XRD indicated that the Ni-P coating was crystalline and the maximum deposition on 1 g CFs was as high as 9000 mg. As the results of the observations reveal, the activation method is a feasible alternative to Pd activation.