1e:T4be,Rational design of the catalysts is impressive for sustainable energy conversion. However, there is a grand challenge to engineer active sites at the interface. Herein, hierarchical transition bimetal oxides/sulfides heterostructure arrays interacting two-dimensional MoO_x/MoS₂ nanosheets attached to one-dimensional NiO_x/Ni₃S₂ nanorods were fabricated by oxidation/hydrogenation-induced surface reconfiguration strategy. The NiMoO_x/NiMoS heterostructure array exhibits the overpotentials of 38 mV for hydrogen evolution and 186 mV for oxygen evolution at 10 mA cm^-2, even surviving at a large current density of 500 mA cm^-2 with long-term stability. Due to optimized adsorption energies and accelerated water splitting kinetics by theory calculations, the assembled two-electrode cell delivers the industrially relevant current densities of 500 and 1000 mA cm^-2 at record low cell voltages of 1.60 and 1.66 V with excellent durability. This research provides a promising avenue to enhance the electrocatalytic performance of the catalysts by engineering interfacial active sites toward large-scale water splitting.1f:T537,Engineering single-atom electrocatalysts with high-loading amount holds great promise in energy conversion and storage application. Herein, we report a facile and economical approach to achieve an unprecedented high loading of single Ir atoms, up to ∼18_wt%, on the nickel oxide (NiO) matrix as the electrocatalyst for oxygen evolution reaction (OER). It exhibits an overpotential of 215 mV at 10 mA cm^-2 and a remarkable OER current density in alkaline electrolyte, surpassing NiO and IrO₂ by 57 times and 46 times at 1.49 V vs RHE, respectively. Systematic characterizations, including X-ray absorption spectroscopy and aberration-corrected Z-contrast imaging, demonstrate that the Ir atoms are atomically dispersed at the outermost surface of NiO and are stabilized by covalent Ir-O bonding, which induces the isolated Ir atoms to form a favorable ∼4+ oxidation state. Density functional theory calculations reveal that the substituted single Ir atom not only serves as the active site for OER but also activates the surface reactivity of NiO, which thus leads to the dramatically improved OER performance. This synthesis method of developing high-loading single-atom catalysts can be extended to other single-atom catalysts and paves the way for industrial applications of single-atom catalysts.20:T610,

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