In this thesis, Ni/BG, NiCu/BG, NiCo/BG, NiCr/BG, NiZn/BG, NiMn/BG and NiFe/BG electrocatalysts were prepared and after characterization, the composites were employed as the hydrogen evolution reaction (HER) electrocatalysts in alkaline medium. In order to characterize the prepared samples, several techniques were employed such as FTIR, XRD, SEM, TEM, Raman and EDX analysis. In the first section, the non-platinum electrocatalyst (PdNiFeCo/C-Ceria) and commercial platinum (10 wt% Pt/C) were coated on the nickel foam and activity of them compared to the bare nickel foam. The non-platinum electrocatalyst showed a low Tafel slope (79 mV dec -1 ) and low overpotential (4 mV) in HER. Also, the performance of electrocatalyst as the cathode electrode was investigated in an anion exchange membrane (AEM) electrolyzer. In the second section, a mixture of graphene/graphite as support was prepared by ball milling procedure at different times and nano particles of nickel were grown into the mixture graphene/graphite substrate. The results indicated that by raising the time of the ball milling from 0 to 270 min, the HER activity of electrocatalyst first increased, and then decreased according to the increase of active sites and then agglomeration of Ni nanoparticles. Ni nanoparticles supported on the mixture with 180 min ball milling exhibited the highest HER activity with a low overpotential (118 mV), a small Tafel slope (84 mV dec -1 ). The third section was devoted to the preparation of Ni- based binary composites with available 3d row transition metals (Co, Fe, Mn, Cr, Cu and Zn) on the best mixture of hybrid graphene/graphite support with 180 min ball milling. The results showed that the Ni-Cu alloy (Ni: Cu mol ratio= 4:1) had the highest catalytic activity with a low overpotential (100 mV) and a small total resistance (167 ? cm 2 ) due to high catalytically active surface area and intrinsic catalytic activity. Also, the Ni-Cu alloy was employed as the cathode in AEM electrolyzer and showed a loss voltage of 0.03 V during 50 h operation. In the last section, composites of Ni and Cu with Ni mol ratio of 0, 25, 50, 75 and 100 are prepared into the hybrid graphene/graphite substrate with 180 min ball milling. It was found that the electrocatalytic activity for the HER depended on the composition of Ni and Cu, where Ni25Cu75 alloy exhibited considerably higher HER activity than other composites. The obtained results of this thesis introduce the investigated samples as the promising electrocatalysts which could be employed in the cathode side of water electrolyzer in alkaline media.