Nickel-coated carbon fibers (NCFs) were fabricated by electroless plating. Sufficient activation sites were vital to deposit a continuous and uniform coating layer. The reaction mechanism and the effect of catalyzation time on the quality of the plating layer were especially discussed. The morphology and coating thickness of the NCFs, particle-size and phosphorus content in the coating layer, formation of the Ni 3 P phase, and its evolution with annealing temperature were examined by field emission scanning electron microscope (FESEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD).In recent years, the study of nickel-coated carbon fibers has attracted considerable attention. The nickel coating layer enables the carbon fibers (CFs) to avoid chemical erosion sequentially enhancing the stability of the composite and also endues the composite with improved performance such as higher electrical conductivity, magnetism, excellent mechanical properties, and good adhesion between the composite and resin or metal. [1] Due to high strength and modulus, high electrical conductivity and magnetism, low weight and high aspect ratio, NCFs have been applied in many fields, such as electromagnetic interference (EMI) shielding, microwave absorption, and as reinforcing materials in plastics, ceramics, or metals. [2,3] Specifically, NCFs act as the conductive fibers to improve the electrical conductivity of polymers in EMI shielding and as electromagnetic wave absorber dispersed in an insulating matrix for microwave absorption.The CFs, however, usually have poor adhesion with nickel coatings due to the nature of their smoothness and chemical inertness. More and various functional groups, such as -COOH, -OH, and -O, are normally introduced on the fiber surface to improve the interfacial adhesion between the CF and the nickel coating. There are basically two routes to enhance the bonding properties of CFs, i.e., oxidative and nonoxidative. The oxidative treatments are extensively used, including air oxidation, [4] chemical oxidation [5][6][7][8] such as nitric acid treatment, [9,10] electrochemical oxidation, [11] plasma or ozone treatment, [12,13] etc. The nonoxidative treatments involve deposition of more active forms of carbon, such as the highly effective whiskerization, the deposition of pyrolytic carbon, or the grafting of the polymers on the fiber surface. [14] The treatment of immersing CFs in nitric acid, a simple and low cost process, can increase the acidic functional groups on the fiber surface and therefore enhance the interfacial adhesion of the fiber and the nickel coating.Little work, to our knowledge, has been done on the effect of the catalyzation time on the quality of the electroless-plated coating layer. Here, we especially investigate this effect and give a possible reaction mechanism of this process. The influence of plating time on the coating thickness, the element components in the coating, and the phase evolution of the coating with annealing temperature were also studied.The PAN (po...