In this study, sulfur doped carbon nanotubes were synthesized using chemical vapor deposition (CVD), cobalt and spinel cobalt catalysts with acetylene and sulfur precursors. The variation of reaction temperature was considered to study of its effect on the morphology of the product. The obtained electron microscope images obtained from these products confirmed the tubular structure of the sulfur doped products. The insertion of sulfur atom in the structure of carbon nanotubes showed some changes in the properties and structure of these products, which were investigated using FESEM, TEM, TGA, EDS, XRD and RAMAN methods. Moreover, the vettability of product was studied by static drop test.Finally the electrocatalytic ability of sulfur-doped carbon nanotubes in hydrogen evolution reactionwas investigated, and the results showed the appropriate electrocoactive activity of these compounds.