The exploration of anode materials for lithium ion batteries (LIBs) or sodium ion batteries (SIBs) represents a grand technological challenge to meet the continuously increased demand for the high-performance energy storage market. Here we report a facile and reliable synthetic strategy for in situ growth of few-layer MoS nanosheets on reduced graphene oxide (rGO) cross-linked hollow carbon spheres (HCS) with formation of three-dimensional (3D) network nanohybrids (MoS-rGO/HCS). Systematic electrochemical studies demonstrate, as an anode of LIBs, the as-developed MoS-rGO/HCS can deliver a reversible capacity of 1145 mAh g after 100 cycles at 0.1 A g and a revisible capacity of 753 mAh g over 1000 cycles at 2 A g. For SIBs, the as-developed MoS-rGO/HCS can also maintain a reversible capacity of 443 mAh g at 1 A g after 500 cycles. The excellent electrochemical performance can be attributed to the 3D porous structures, in which the few-layer MoS nanosheets with expanded interlayers can provide shortened ion diffusion paths and improved Li/Na diffusion mobility, and the hollow porous carbon spheres and the outside graphene network are able to improve the conductivity and maintain the structural integrity.

Electrosynthesis of formic acid/formate is a promising alternative protocol to industrial processes. Herein, a pioneering pair‐electrosynthesis tactic is reported for exclusively producing formate via coupling selectively electrocatalytic methanol oxidation reaction (MOR) and CO2 reduction reaction (CO2RR), in which the electrode derived from Ni‐based metal–organic framework (Ni‐MOF) nanosheet arrays (Ni‐NF‐Af), as well as the Bi‐MOF‐derived ultrathin bismuthenes (Bi‐enes), both obtained through an in situ electrochemical conversion process, are used as efficient anodic and cathodic electrocatalysts, respectively, achieving concurrent yielding of the same high‐value product at both electrodes with greatly reduced energy input. The as‐prepared Ni‐NF‐Af only needs quite low potentials to reach large current densities (e.g., 100 mA cm−2@1.345 V) with ≈100% selectivity for anodic methanol‐to‐formate conversion. Meanwhile, for CO2RR in the cathode, the as‐prepared Bi‐enes can simultaneously exhibit near‐unity selectivity, large current densities, and good stability in a wide potential window toward formate production. Consequently, the coupled MOR//CO2RR system based on the distinctive MOF‐derived catalysts displays excellent performance for pair‐electrosynthesis of formate, delivering high current densities and nearly 100% selectivity for formate production in both the anode and the cathode. This work provides a novel way to design advanced MOF‐derived electrocatalysts and innovative electrolytic systems for electrochemical production of value‐added feedstocks.

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The hybrid of cobalt nanoparticles embedded in N-rich carbon nanotubes (Co@NCNT) derived from a Co-based metal–organic framework exhibits outstanding multifunctional electrocatalytic performance toward a set of important electrochemical reactions.