In this study, Ni, Zn and Ni/Zn ferrites catalysts were synthesized by co-precipitation method. Then, the effect of process temperature on the growth and morphology of the sulfur-doped carbon nanomaterials on these catalysts in chemical vapor deposition method were investigated. In this method, setting temperature at 600 and 800 °C leads to formation of nanofibers and carbanions spheres, respectively. In addition, the activity of Ni, Zn and Ni/Zn ferrites catalysts for the growth and morphology of the synthesized sulfur-doped nanofibers at 600 °C was investigated. In this research, according to FE-SEM images, carbon nanofibers grown on nickel ferrite catalyst had more uniform morphology than carbon nanofibers grown on zinc and nickel-zinc ferrite catalysts, so they were selected for further investigation. In the second part of this research, the catalytic activity of copper, brass, and zinc foil on the morphology of the produced sulfur-doped nano-carbons on these foils at 600 °C were studied. The sulfur-doped carbon nano-sheets and porous nano-carbons were formed on the copper and brass foils, respectively. The efforts for achieving nano-carbons on the zinc foil, because of low temperature melting point and restriction in chemical vapor deposition, was failed. The catalysts and products were characterized by FT-IR, UV-Vis, Raman, FE-SEM, EDS, TEM, XPS, XRD and TGA methods. Finally, the gold nanoparticles decorated on the sulfur-doped carbon nanofibers and porous nano-carbons by the mean of electrochemical deposition and the activity of them for morphine sensing by cyclic voltammetry and square wave voltammetry were investigated. The results show the efficient applicability of this configuration for electrochemical sensing of morphine. It is worthy to mention that, the sulfur-doped porous nano-carbons shows the better efficiency than the carbon nanofibers for sensing morphine in this method.