Catalytically graphitized electrospun carbon nanofibers were plated with nickel using a commercial electroless bath for the first time. The nanofiber fabrication process was performed in the presence of nickel as the graphitization catalyst at a temperature of 1400 °C. Raman spectroscopy and X-ray diffraction studies confirmed the achievement of a satisfactory degree of graphitization for the carbon nanofibers. After sensitization and activation processes, the nanofibers were submerged for 20 min in the electroless bath at a temperature of 45 °C and a pH value of 9. Results from scanning electron microscopy and X-ray diffraction showed that a pure, crystalline and uniform nickel coating of 186 nm thickness was formed on the surface of the nanofibers.