A recent approach for solar‐to‐hydrogen generation has been water electrolysis using efficient, stable, and inexpensive bifunctional electrocatalysts within strong electrolytes. Herein, the direct growth of 1D NiCo2S4 nanowire (NW) arrays on a 3D Ni foam (NF) is described. This NiCo2S4 NW/NF array functions as an efficient bifunctional electrocatalyst for overall water splitting with excellent activity and stability. The 3D‐Ni foam facilitates the directional growth, exposing more active sites of the catalyst for electrochemical reactions at the electrode–electrolyte interface. The binder‐free, self‐made NiCo2S4 NW/NF electrode delivers a hydrogen production current density of 10 mA cm–2 at an overpotential of 260 mV for the oxygen evolution reaction and at 210 mV (versus a reversible hydrogen electrode) for the hydrogen evolution reaction in 1 m KOH. This highly active and stable bifunctional electrocatalyst enables the preparation of an alkaline water electrolyzer that could deliver 10 mA cm–2 under a cell voltage of 1.63 V. Because the nonprecious‐metal NiCo2S4 NW/NF foam‐based electrodes afford the vigorous and continuous evolution of both H2 and O2 at 1.68 V, generated using a solar panel, they appear to be promising water splitting devices for large‐scale solar‐to‐hydrogen generation.

Electrochemical oxygen evolution and reduction reactions have received great attention due to their importance in several key technologies such as fuel cells, electrolyzers, and metal–air batteries. Here, we present a simple approach to the preparation of cobalt sulfide nanoparticles in situ grown on a nitrogen and sulfur codoped graphene oxide surface. The particle size and phase were controlled by changing the treatment temperature. Cobalt sulfide nanoparticles dispersed on graphene oxide hybrids were successfully prepared by a solid-state thermolysis approach at different temperatures (400, 500, and 600 °C) using cobalt thiourea and graphene oxide. X-ray diffraction studies revealed that hybrids prepared at 400 and 500 °C result in pure CoS2 phase, whereas the hybrid prepared at 600 °C exhibits Co9S8 phase. X-ray photoelectron spectroscopy studies revealed that nitrogen and sulfur simultaneously codoped on the graphene oxide surface, and these sites act to anchor the CoS2 nanoparticles strongly on the GO surface. The strong coupling between CoS2 and N,S-GO was reflected in the improvement of the oxygen electrode potential. CoS2(400)/N,S-GO showed an outstanding oxygen electrode activity with a potential of about 0.82 V against a reversible hydrogen electrode in alkaline medium, which is far better than the performance of precious catalysts such as Pt/C (1.16 V), Ru/C (1.01 V), and Ir/C (0.92 V).

A significant decrease in performance was observed for commercial Pt/C due to electrochemical oxidation of the carbon support and subsequent detachment and agglomeration of Pt particles. The Pt/TiO(2) cathode catalyst exhibited excellent fuel cell performance and ultrahigh stability under accelerated stress test conditions and can be considered as a promising alternative for improving the reliability and durability of PEMFCs.

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