The development of economically viable, binder-free bifunctional electrocatalysts is essential for enhancing the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER) within the overall water-splitting process. In this research, a bi-functional Mn-Co-P@Ni-Co/NF catalyst for HER and OER was developed using a binder-free and facile two-step electrodeposition technique. First, a three-dimensional (3D) Ni-Co film was produced using the dynamic hydrogen bubble template (DHBT) method to increase the active surface area. Next, an Mn-Co-P compound with a nanosheet structure was deposited onto the 3D microporous nanostructured Ni-Co substrate through a potentiostatic method (chronoamperometric). Characterization techniques such as transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), and energy-dispersive X-ray spectroscopy (EDS) validated the successful formation of Mn-Co-P nanosheets on the 3D microporous nanostructured Ni-Co substrate, demonstrating notable bifunctional electrocatalytic activity with overpotentials of 75 mV for HER and 309 mV for OER at a current density of 10 mA cm−2, accompanied by Tafel slopes of 79 mV dec−1 for HER and 56 mV dec−1 for OER. The stability of the electrode was evaluated at current densities of −100 mA cm−2 for HER and 100 mA cm−2 for OER, revealing a reliable and stable performance over a duration of 50 h. Furthermore, the two-electrode assessment of the Mn-Co-P@Ni-Co/NF catalyst during overall water splitting indicated a required potential of 1.53 V at a current density of 10 mA cm−2. This research underscores an effective and economical strategy for developing advanced electrodes that are essential for applications in electrochemical energy conversion and storage.

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