The production of energy from fossil fuels generates greenhouse gases, leading to global warming and various environmental impacts. Extensive research into sustainable alternative fuels has identified hydrogen (H2) as a viable option. With net zero carbon emissions, hydrogen presents a promising solution for sustainable and renewable energy. This study employs a simple gel-matrix method to fabricate Ni-Fe alloy-based nanocomposites in alkaline media (1 M KOH). Achieving outstanding performance in hydrogen generation through the hydrogen evolution reaction (HER) and oxygen evolution reaction (OER), with impressive turn-over frequencies (TOF) of 2.98 s−1 at 177 mV and 1.48 s−1 at 219 mV. Nanocomposite’s unique structure enhances electroactive surface area (347.5 cm2/gram), extending electrocatalytic active sites and durability to 60 h. It shows excellent performance, characterized by low Tafel slopes of 50 mV/dec and 37 mV/dec, and minimal overpotentials of 219 mV for the oxygen evolution reaction (OER) and 177 mV for the hydrogen evolution reaction (HER), reaching a current density of 10 mA cm−2. This study presents a method for synthesizing high-performance, sustainable metal-alloy/garnet hybrid electrocatalysts, offering a new frontier in design of next-generation materials for advanced energy conversion technologies.
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