Using fossil fuels as a main source of energy has resulted in various environmentally hazardous effects, including global warming, climate change, and environmental pollution. Consequently, the development of a sustainable and clean source of energy became of urgent need. Water electrolysis has captured considerable attention as the main technology of hydrogen fuel production. It is particularly enticing due to its eco-friendliness and sustainability. Self-supported electrocatalysts for oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) have prominent roles in water electrolysis. Growing self-supported metal oxides, hydroxides1, phosphates2, sulfides3, etc. that possess high electrical conductivity, electrocatalytic activity, and structural stability have attracted attention lately. FeNi-based catalysts are considered one of the most promising electrocatalysts for water electrolysis in alkaline solutions. However, improving their catalytic activity and stability is one of the research targets before further practical applications. Nickel foam is widely used as a self-supported electrocatalyst due to its high surface area, low cost, and exceptional catalytic activity, with several studies focused on the deposition of nickel-iron materials on nickel foam for the development of a bifunctional catalyst for water electrolysis4. However, very few studies used NiFe mesh or foam to grow a self-supported catalyst material5.In this study, surface-engineered NiFe foam electrodes were developed by facile control of the Ni/Fe surface ratio via chemical leaching and oxidation with NaOH and NaClO4 followed by electrochemical activation, aiming to design a bifunctional electrocatalyst for both OER and HER. Results revealed that varying the ratios of NaOH and NaClO4 induced significant alterations to the surface composition (different Ni/Fe), and hence the active sites for OER and HER. The physicochemical and structural properties of the NiFe foam were characterized using glancing angle X-ray diffraction (GAXRD), X-ray photoelectron spectroscopy (XPS), and scanning electron microscope (SEM). Further, the catalytic activity of the modified electrode was assessed utilizing cyclic voltammetry, linear sweep voltammetry, chronopotentiometry, and electrochemical impedance spectroscopy. References F. Dionigi and P. Strasser, Advanced Energy Materials, 6, 1600621 (2016).Y. Yu et al., Journal of Colloid and Interface Science, 607, 1091–1102 (2022).A. Shankar, R. Elakkiya, and G. Maduraiveeran, New J. Chem., 44, 5071–5078 (2020).H.-S. Hu, S. Si, R.-J. Liu, C.-B. Wang, and Y.-Y. Feng, International Journal of Energy Research, 44, 9222–9232 (2020).C. Sun et al., ACS Appl. Energy Mater., 4, 8791–8800 (2021).