A new procedure of surface activation without using palladium salt is proposed for electroless nickel plating (Ni-P) on carbon fiber. The optimal formula and technical conditions for palladium-free activated electroless Ni-P were obtained by orthogonal experiments. The effects of nitric acid processing time on the quality of nickel coating was investigated .The effects of varying concentrations of Ni2 + on the rate of weight gain during the Ni2 + complex adsorption process were also analyzed and the kinetic equation of the process was established. The theoretical values calculated by the equation were proven to be consistent with the experimental verification. The material characteristics of the deposited layers were analyzed by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX) and X-ray diffraction (XRD). The tensile strength of the carbon fibers was analyzed by the Weibull method, and this showed that when the thickness of the Ni-P coating reached 0.150μm, the tensile strength reached a maximum value. The experimental results showed that the nickel deposition on the carbon fiber surface obtained by this method, had the same uniformity, compactness and adhesive properties as the one by conventional electroless Ni-P.