In the first of this research, the hybrids of MoS 2 and star polybenzimidazole (PBI) are fabricated based on triazine cycles. The nano hybrid, structure and composite are utilized as substrate to hydrogen evolution reaction (HER). To fallowing attempt to elimination of platinum from HER, the MoS 2 sheets are decorated with star PBI. Then, the nano catalysts are characterized with different methods such as thermo gravimetry, transmission electron microscopy, field-emission scanning electron microscopy and X-ray diffraction techniques. Electrochemical studies shade light open the fact that the onset potential is only (160 mV vs.RHE) with a small Tafel slope of 50.6 mV dec -1 for HER. Consequently, these novel hybrids are comparable with Pt and Pt composite in HER. In the second part of this thesis, the graphene oxide was synthesized based of reported methods and it was characterized with different techniques. Then, the surface of the graphene oxide was doped with nitrogen by used of ammonium hydroxide. In addition, both surface of the graphene oxide and nitrogen doped graphene oxide (GO and NGO) are decorated with lanthanum- nickel layered doubled hydroxide (LDH). Then, one novel strategy was designed and developed for fabricated of gold nanoparticels by galvanic exchange of nickel's LDH sheets. However, in this section, the La-Ni/LDH sheets and Au nanoparticels are fabricated on reduce GO and reduce NGO as novel strategy for elimination of Pt from electrocatalyst in water splitting. The electrochemical characterizations reveal the fact that the onset potential of only (–80 mV vs. RHE) and current exchange density ~10 mA.cm -2 with a small Tafel slope of 60 mV dec-1 for HER. The synthetic extraordinary electrocatalysts are comparable or better than different platinum compounds and transition metal sulfides in several aspects.