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Developing cost‐effective and highly efficient oxygen evolution reaction (OER) electrocatalysts is vital for the production of clean hydrogen by electrocatalytic water splitting. Here, three dimensional nickel‐iron layered double hydroxide (NiFe LDH) nanosheet arrays are in‐situ fabricated on self‐supporting nitrogen doped graphited foam (NGF) via a one‐step hydrothermal process under an optimized amount of urea. The as prepared NiFe LDH/NGF electrode exhibits a remarkable activity toward OER with a low onset overpotential of 233 mV and a Tafel slope of 59.4 mV dec −1 as well as a long‐term durability. Such good performance is attributed to the synergy among the doping effect, the binder‐free characteristic, and the architecture of the nanosheet array.

Platinum-based single-atom catalysts (SACs) are among the most promising candidates for the practical applications of electrochemical hydrogen evolution reaction (HER), but their catalytic efficiency remains to be further enhanced. Herein, a welldesigned nanoarray-structured nitrogen-doped graphite foil (NNGF) substrate is introduced to support Pt SACs in Pt−N 4 construction (Pt 1 /NNGF) for HER. Within NNGF, the constructed nanoarray-structured surficial layer for supporting Pt SACs could enhance the exposure of active sites to the electrolyte and improve the reaction and diffusion kinetics; meanwhile, the retained graphite structures in bulk NNGF provide not only the required electrical conductivity but also the mechanical stability and flexibility. Because of such double-layer structures of NNGF, stable Pt−N 4 construction, and binder-free advantages, the Pt 1 / NNGF electrode exhibits a low overpotential of 0.023 V at 10 mA cm −2 and a small Tafel slope of 29.1 mV dec −1 as well as an excellent long-term durability.