Electrospun fibers with different concentrations of polyacrylonitrile (PAN) were synthesized and the results are reported in this study. The aim was to obtain carbon nanofibers for manufacturing gas diffusion layers for proton exchange membrane (PEM) fuel cells. The electrospun fibers obtained were carbonized at 1200 degrees C, 1300 degrees C, and 1400 degrees C, in order to have nanofibers with more than 96% of carbon atoms. The scanning electron microscopy (SEM) results revealed an increase in the diameter from 400-700 nm at 1200 degrees C to 1000-1400 nm at 1300 degrees C and 1400 degrees C. The Raman measurements disclose a higher degree of crystallinity for the sample carbonized at elevated temperatures. The surface area was estimated from the Brunauer-Emmett-Teller (BET) method and the results revealed an increase from 40.69 m(2)g(-1) to 66.89 m(2)g(-1) and 89.92 m(2)g(-1) as the carbonization temperature increased. Simultaneously, the pore volume increased with increasing carbonization temperature. The Fourier-transform infrared spectroscopy (FTIR) spectra reveal that during carbonization treatment, C equivalent to N triple bonds are destroyed with the appearance of C=N double bonds. Decreasing the I-D/I-G intensities' ratio from similar to 1.07 to similar to 1.00 denotes the defects reduction in carbonaceous materials due to the graphitization process. Therefore, the carbon fibers developed in optimum conditions are appropriate to be further used to produce gas diffusion layers for Proton-exchange membrane fuel cells (PEMFC).