In this study, using Fe/CaCO3 as catalyst, P-dopes Carbon spheres have been prepared from acetylene and triphenyl phosphine precursors using chemical vapor deposition method and the morphology of the product has been confirmed using field emission scanning electron microscope (FESEM) images. Then, nickel nanoparticles have been deposited on the surface of the prepared carbon spheres using the reduction of nickel salt ant the product was confirmed using ICP, EDS and elemental mapping analyses. Moreover, the changes in the structure and properties of carbon spheres have been analyzed using FE-SEM, EDS, Raman, UV-Vis, TEM, TGA and XRD methods and the hydrophobicity of the product was analyzed using static drop test. The final product has been employed for the catalytic reduction of nitrobenzene to aniline. TLC method was used to follow the reaction and UV-Vis spectroscopy was used to determine the yields. The reaction was carried out using 20 mol% of catalyst, hydrazine as the reducing agent in 2h with 95% yield.To determine the versatility of this method, several nitrobenzene derivatives (including nitrophenols) have been successfully synthesized. Finally, the recyclability of the reaction was investigated and the results showed only 20% decreasing in the yield after 6 runs.