Establishing proper intrinsic catalysts with nanostructured high active surfaces endows the paramount electrocatalytic activity. A Ni-Se@Cu-Ni/NF catalyst for hydrogen and oxygen evolution reactions (HER and OER) is prepared via an efficient two-step pulse current (PC) electrodeposition method. The initial 3D film of Cu-Ni is synthesized via the dynamic hydrogen bubble template (DHBT) method to attain further active surface area. Then, Ni-Se film is prepared by direct current (DC) and PC electrodeposition. Morphological, chemical, and electrocatalytic characteristics of the Ni-Se electrodeposited films are evaluated. X-ray photoelectron spectroscopy and high-resolution transmission electron microscopy results show a NiSe/NiSe2 nanofilm on the 3D microporous nanostructured Cu-Ni substrate which reveals an efficient bifunctional electrocatalytic behavior with overpotentials of 74 and 272 mV in the current density of 10 mA cm−2, and Tafel slopes of 78 and 50 mV dec−1 for HER and OER, respectively. The two-electrode examination with NiSe/NiSe2@Cu-Ni/NF catalyst in overall water splitting indicates a required potential of 1.57 V in the current density of 10 mA cm−2.

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