Carbon fibers (CFs) were plated with nickel-phosphorus (Ni-P) using an electroless plating process. The effects of the process parameters such as heat treatment temperature, heat treatment time, and the pH of the plating bath on electroless Ni-P plating were investigated. The structure, elemental composition, and thermal and electrical properties of Ni-P plated CFs (MCF) were characterized by X-ray diffraction (XRD), a four-probe volume resistivity tester, and an infrared thermal imaging camera, respectively. The XRD indicated the presence of amorphous and crystalline phases of Ni and Ni-P. The MCF were able to perform at high temperatures because of their higher thermal conductivity. A heat treatment temperature of 300 °C, a heat treatment time of 4 h, and a pH of 8.5 were found to be optimum for obtaining MCF with desirable thermal and electrical properties.