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Carbon nanofibers are very stiff, strong and light materials composed from tightly packed layers of graphite sheets stacked parallel one near the other in a regular pattern and aligned along the fiber axis. This study presents a facile approach to prepare composite Ni/C nanofibers through electrospinning of polymer solution. A mixed solution of polyacrylonitrile (PAN) in dimethylformamide (DMF) solvent along with Ni(CH 3 COO) 2 was the precursor solution used to obtain composite Ni/C nanofibers. The amount of Ni salt was varied in order to study the influence of Ni percent on the composite fibers properties, particularly the pores dimension and the specific surface area. The composition and the structure of materials were investigated through elemental analysis and scanning electron microscopy (SEM). In addition, thermal gravimetric analysis (TGA) was performed to complete the composition study and the thermal degradation profile.