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In this work, the solvothermal solidification method has been used to be prepared as a homogenous CuSn-organic nano-composite (CuSn-OC) to use as a catalyst for alkaline water electrolysis for cost-effective H₂ generation. FT-IR, XRD, and SEM techniques were used to characterize the CuSn-OC which confirmed the formation of CuSn-OC with a terephthalic acid linker as well as Cu-OC and Sn-OC. The electrochemical investigation of CuSn-OC onto a glassy carbon electrode (GCE) was evaluated using the cyclic voltammetry (CV) method in 0.1 M KOH at room temperature. The thermal stability was examined using TGA methods, and the Cu-OC recorded a 91.4% weight loss after 800 °C whereas the Sn-OC and CuSn-OC recorded 16.5 and 62.4%, respectively. The results of the electroactive surface area (ECSA) were 0.5, 0.42, and 0.33 m² g⁻¹ for the CuSn-OC, Cu-OC, and Sn-OC, respectively, and the onset potentials for HER were −420, −900, and −430 mV vs. the RHE for the Cu-OC, Sn-OC, and CuSn-OC, respectively. LSV was used to evaluate the electrode kinetics, and the Tafel slope for the bimetallic catalyst CuSn-OC was 190 mV dec⁻¹, which was less than for both the monometallic catalysts, Cu-OC and Sn-OC, while the overpotential was −0.7 vs. the RHE at a current density of −10 mA cm⁻².