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Alkaline water splitting, especially the anion-exchange-membrane based water electrolysis, is an attractive way for low-cost and scalable H2 production. Green electricity-driven alkaline water electrolysis is requested to develop highly-efficient electrocatalysts...

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Constructing 3D hierarchical architecture consisting of 2D hybrid nanosheets is very critical to achieve uppermost and stable electrochemical performance for both lithium‐ion batteries (LIBs) and hydrogen evolution reaction (HER). Herein, a simple synthesis of uniform 3D microspheres assembled from carbon nanosheets with the incorporated MoO2 nanoclusters is demonstrated. The MoO2 nanoclusters can be readily converted into the molybdenum carbide (Mo2C) nanocrystals by using high temperature treatment. Such assembling architecture is highly particular for preventing Mo‐based ultrasmall nanoparticles from coalescing or oxidizing and endowing them with rapid electron transfer. Consequently, the MoO2/C hybrids as LIB anode materials deliver a specific capacity of 625 mA h g−1 at 1600 mA g−1 even after 1000 cycles, which is among the best reported values for MoO2‐based electrode materials. Moreover, the Mo2C/C hybrids also exhibit excellent electrocatalytic activity for HER with small overpotential and robust durability in both acid and alkaline media. The present work highlights the importance of designing 3D structure and controlling ultrasmall Mo‐based nanoparticles for enhancing electrochemical energy conversion and storage applications.

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