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Electrocatalytically active nanocomposites play a vital role in energy generation, conversion, and storage technologies. Transition metal-based catalysts such as nickel and iron and their pnictide (phosphide), and chalcogenide (selenide) compounds exhibit good activity for hydrogen evolution reaction (HER) in the alkaline environment. In this study, transition metals-based catalysts (Ni-P-Se, Fe-P-Se, and Ni-Fe-P-Se) solutions were prepared using a simple one-pot method. Prepared solutions were deposited on Ni foam, and different characterization techniques were used to determine the composition, structure, and morphology of as-prepared catalysts. Furthermore, it was found that Ni-Fe-P-Se as a cathode material showed better HER performance compared to other investigated materials with the overpotential value of 316 mV at 10 mA cm-2 current density and 89 mV dec-1 Tafel slope value. The stability tests of the as-prepared catalyst confirmed that the synergistic effect between various elements enhances the electrocatalytic performance for up to 24 hours, providing a fair, stable nature of Ni-Fe-P-Se based sample.