One of the most important topics of sustainable development is the concept of “pure energy”. Extensive research activities have been carried out in order to find the most suitable fuel for the generation of “energy of the future”. A supreme example of “pure energy” carriers is hydrogen, because its oxidation leads only to the formation of water. Water electrolysis is one of the best methods for producing high purity hydrogen. Improving the performance of the cathode electrode, which is the site of hydrogen evolution reaction, and finding low cost catalysts with high stability, good performance, rather than expensive metals and noble metals as the hydrogen electrode, are the subject of many research in the world today. In this thesis, in order to construct an appropriate electrode for hydrogen production, various catalysts such as nickel, tungsten, cobalt, molybdenum and nickel-molybdenum, nickel-cobalt and nickel-tungsten alloys have been deposited on nickel foam substrate. The results show that nickel-molybdenum alloy exhibited better hydrogen evolution reaction (HER) activity at a current of 160 mA at -1.7 volts than these catalysts. Crystallographic structure of the prepared catalysts was investigated with X-ray diffraction analysis. The morphology of the obtained samples was characterized by scanning electron microscopy (SEM). In the next part of this thesis, the bath condition was optimized, which included the effect of pH, change in the ratio of nickel and molybdenum, changes in the concentration of boric acid and tri sodium citrate, T 1 and T 2 times and the amount of charge that was sitting on the catalyst bed. The results showed that pH=9.5, 3:1 Ni:Mo molar ratio, a concentration of 0.3 molar sodium tricitrate and a concentration of 0.05 molar boric acid are the best values. The chronocoulometry technique was used, too. The parameters of the chronocoulometry method were investigated and the times of 6 and 10 seconds and the charge of 100 coulombs were optimized. After the charge on the catalyst reached 100 coulombs, the catalyst was prepared for electrochemical studies. Finally, the catalyst was tested in an optimum condition in an anion-exchange membrane cell at ambient, 40° C and 60° C temperature, and was compared with an unmodified (pure) bed. The results demonstrated that the catalyst modified by nickel-molybdenum alloy was better than the unmodified (pure) catalyst at all three temperatures. For example, a modified catalyst had a Cell voltage of 1.3 V at 60° C and 1A, which is 2.5 V for an unmodified catalyst, under the same conditions.