Ni and alloys of Ni (with Fe, Co, Mo) still represent the most suitable electrodes for HER in alkaline media. Bimetallic nanoparticles of NiFe and NiCo were fabricated by coprecipitation and thermal reduction by oleylamine. The process of co-precipitation involves NaOH as a precipitation agent to precipitate the metal-based nitrates, while thermal reduction process involves the synthesis of metal-containing compounds using oleylamine, which act as reducing agent, surfactant, and solvent. Different synthesis conditions in terms of composition were studied. Structural characterization of nanoparticles was carried out using scanning electron microscopy, energy dispersive x-ray, X-ray diffraction, Raman spectroscopy and BET surface area. Electrochemical behavior of nanoparticles was investigated using rotating disk electrode. The electrochemical characterization studied the effect of catalyst composition on the electrochemical behavior of the catalyst.Recent developments in alkaline membrane technology have led to the possibility of using anion-exchange membranes containing alkaline ions (OH -, CO3 2-, HCO3 -) in water electrolysis. This technology has the potential of combining the advantage of nonprecious catalysts of the alkaline process, with the advantages of PEMEL, e.g. fast power-up/power-down rates, low parasitic energy losses, and low energy consumption, in other words consolidating the best of both technologies (3).