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A bubble-releasing assisted pulse electrodeposition method was developed to create metallic alloy, NiFe, nanotube arrays in one step. The NiFe alloy nanotube array exhibited excellent bifunctional electrolytic activities, achieving low overpotentials of 100 mV for the hydrogen evolution reaction and 236 mV for the oxygen evolution reaction at 10 mA cm–2, both in 1 M KOH at room temperature. For overall water splitting, the NiFe alloy nanotube array delivered 10 mA cm–2 at an ultralow cell voltage of 1.58 V, among the top tier of the state-of-the-art bifunctional electrocatalysts. The NiFe alloy nanotube array also exhibited ultrastability at high current densities, experiencing only a minor chronoamperometric decay of 6.5% after a 24 h operation at 400 mA cm–2. The success of the present binder-free nanotube array-based electrode can be attributed to the much enlarged reaction surface area, one-dimensionally guided charge transport and mass transfer offered by the nanotube structure, and improved product crystallinity provided by the pulse current electrodeposition. The nanotube array structure proves to be a promising new architecture design for electrocatalysts.

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