Expanded graphite decorated with nickel oxide particles (EG NiO ) has been synthesized through electrochemical oxidation of natural graphite in an aqueous nickel nitrate solution followed by a heat treatment. EG NiO was used to prepare nickel/carbon composites using two techniques: (a) hydrogen reduction of nickel oxide particles loaded on the expanded graphite surface and (b) pyrolysis of coal tar pitch-impregnated EG NiO blocks. The EG NiO as well as the nickel/carbon composites have been characterized by X-ray diffraction, scanning and transmission electron microscopy, energy dispersive X-ray spectroscopy and selected area electron diffraction.