1f:T472,A fundamental understanding of the origin of oxygen evolution reaction (OER) activity of transition-metal-based electrocatalysts, especially for single precious metal atoms supported on layered double hydroxides (LDHs), is highly required for the design of efficient electrocatalysts toward further energy conversion technologies. Here, we aim toward single-atom Au supported on NiFe LDH (^sAu/NiFe LDH) to clarify the activity origin of LDHs system and a 6-fold OER activity enhancement by 0.4 wt % ^sAu decoration. Combining with theoretical calculations, the active behavior of NiFe LDH results from the in situ generated NiFe oxyhydroxide from LDH during the OER process. With the presence of ^sAu, ^sAu/NiFe LDH possesses an overpotential of 0.21 V in contrast to the calculated result (0.18 V). We ascribe the excellent OER activity of ^sAu/NiFe LDH to the charge redistribution of active Fe as well as its surrounding atoms causing by the neighboring ^sAu on NiFe oxyhydroxide stabilized by interfacial CO₃^2- and H₂O interfacing with LDH.20:T50b,Abstract The oxygen evolution reaction (OER) has aroused extensive interest from materials scientists in the past decade by virtue of its great significance in the energy storage/conversion systems such as water splitting, rechargeable metal–air batteries, carbon dioxide (CO 2 ) reduction, and fuel cells. Among all the materials capable of catalyzing OER, layered double hydroxides (LDHs) stand out as one of the most effective electrocatalysts owing to their compositional and structural flexibility as well as the tenability and the simplicity of their preparation process. For this reason, numerous efforts have been dedicated to adjusting the structure, forming the well‐defined morphology, and developing the preparation methods of LDHs to promote their electrocatalytic performance. In this article, recent advances in the rational design of LDH‐based electrocatalysts toward OER are summarized. Specifically, various tactics for the synthetic methods, as well as structural and composition regulations of LDHs, are further highlighted, followed by a discussion on the influential factors for OER performance. Finally, the remaining challenges to investigate and improve the catalyzing ability of LDH electrocatalysts are stated to indicate possible future development of LDHs.21:T4e3,Water splitting is widely considered to be a promising strategy for clean and efficient energy production. In this paper, for the first time we report an in situ growth of iron–nickel nitride nanostructures on surface-redox-etching Ni foam (FeNi3N/NF) as a bifunctional electrocatalyst for overall water splitting. This method does not require a specially added nickel precursor nor an oxidizing agent, but achieves well-dispersed iron–nickel nitride nanostructures that are grown directly on the nickel foam surface. The commercial Ni foam in this work not only acts as a substrate but also serves as a slow-releasing nickel precursor that is induced by redox-etching of Fe3+. FeCl2 is a more preferable iron precursor than FeCl3 for no matter quality of FeNi3N growth or its electrocatalytic behaviors. The obtained FeNi3N/NF exhibits extraordinarily high activities for both oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) with low overpotentials of 202 and 75 mV at 10 mA cm–2, Tafel slopes of 40 and 98 mV dec–1, respectively. In addition, the presented FeNi3N/NF catalyst has an extremely good durability, reflecting in more than 400 h of consistent galvanostatic electrolysis without any visible voltage elevation.22:T4c6,Electrochemical oxidation of biomass-derived platform molecules can enable the production of value-added oxygenated commodity chemicals under mild conditions in a distributed fashion using renewable electricity; however, very few efficient, robust, and inexpensive electrocatalysts are available for such electrochemical oxidation. Here we demonstrate that earth-abundant NiFe layered

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