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 stainless steel. The electrochemical behavior of nano-catalysts was evaluated by electrochemical methods such as cyclic voltammetry (CV) and linear sweep voltammetry (LSV). The results show that nickel-molybdenum alloy exhibited better hydrogen evolution reaction (HER) activity at a current of 180 mA at -1.6 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). From the SEM micrographs it can be seen that the surface of nickel-molybdenum alloy is rough and uniform. In the third 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, T1 and T2 times and the amount of charge that was sitting on the catalyst bed. The results showed that pH=9.5, 2: 1 ratio of molybdenum: nickel, a concentration of 0.25 molar sodium tricitrate and a concentration of 1 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 3 and 10 seconds and the charge of 100 coulombs were optimized. In this technique voltages of -0.862 and -1.303 volts were used. After the charge on the catalyst reached 100 coulombs, the catalyst was prepared for electrochemical studies. Electrochemical measurements were carried out in a typical three electrode cell in 1 M NaOH aqueous solution. The as-prepared nickel-molybdenum alloy deposited on stainless steel, Ag/AgCl electrode and Pt foil were used as the working electrode, reference electrode and counter electrode, respectively. HER startup potential with using this electrode is -0.650 volts vs. Ag/AgCl electrode which is compatible with commercial electrodes. Finally, the catalyst was tested in an optimum condition in an anion-exchange membrane cell at ambient temperature, 40° C and 60° C, 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 1.7 V at 60° C and 1 A, which is 2.5 V for an unmodified catalyst, under the same conditions.