The focus of this work is the development and study of nickel-based and transition metal-based electrocatalysts to improve the efficiency of green hydrogen production. Given the global need to reduce greenhouse gas emissions and transition to sustainable energy sources, green hydrogen is becoming a key element in the decarbonization of the energy sector. The aim of this work is to examine the impact of material surface treatment and system geometry on the catalytic activity of different materials for the hydrogen evolution reaction (HER) under alkaline conditions. The experimental part involves testing the catalytic activity of materials such as nickel, platinum and cobalt-chromium-molybdenum alloy (CoCrMo) using electrochemical impedance spectroscopy (EIS) and polarization measurements. The experiments were conducted in a standard three-electrode system in a 1 M NaOH solution (pH = 14) at room temperature. Normalizing the electrocatalyst surface to an electrochemically active surface allowed for a more accurate assessment of their efficiency and comparison of catalysts with different materials and morphological characteristics. The results showed that platinum, based on kinetic parameters, has the best catalytic activity, with the reaction proceeding via the Volmer-Heyrovsky mechanism. The polished platinum RDE demonstrated better efficiency compared to the unpolished one, indicating the influence of surface treatment on the catalytic activity of the material. Nickel and the CoCrMo alloy exhibited similar catalytic characteristics, with the reaction following the Volmer-Tafel mechanism, where the Volmer step determines the reaction rate.