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Single‐layered MoS2 is a promising anode material for lithium‐ion batteries (LIBs), sodium‐ion batteries (SIBs), and potassium‐ion batteries (PIBs) due to its high capacity and isotropic ion transport paths. However, the low intrinsic conductivity and easy‐agglomerated feature hamper its applications. Here, a charge‐driven interlayer expansion strategy that Co2+ replaces Mo4+ in the doping form to endow MoS2 layers with negative charges, thus inducing electrostatic repulsion, together with the insertion of gaseous groups, to drive interlayer expansion which once breaks the confinement of interlayer van der Waals force, single‐layered MoS2 is obtained and uniformly dispersed into carbon matrix arising from the transformation of carbonaceous gaseous groups under high vapor pressure, is proposed. Co atom doping helps enhance the intrinsic conductivity of single‐layered MoS2. Carbon matrix effectively prevents agglomeration of single‐layered MoS2. The doped Co atoms can be fully transformed into ultrasmall Co nanoparticles during conversion reaction, which enables strong spin‐polarized surface capacitance and thus significantly boosts ion transport and storage. Consequently, the prepared material delivers superb Li/Na/K‐ion storage performances, which are best in the reported MoS2‐based anodes. The proposed charge‐driven interlayer expansion strategy provides a novel perspective for preparing single‐layered MoS2, which shows huge potential for energy storage. Single‐layered MoS2 has great potential in energy storage but suffers from low intrinsic conductivity and easy‐agglomerated feature. Here, a charge‐driven interlayer expansion strategy is proposed. The interlayer electrostatic repulsion induced by Co doping breaks the interlayer van der Waals force to fabricate Co‐doped single‐layered MoS2, which uniformly disperses in carbon matrix and shows superior lithium/sodium/potassium‐ion transport and storage capability.

Fe3O4 is widely investigated as an anode for ambient sodium‐ion batteries (SIBs), but its electrochemical properties in the wide operation‐temperature range have rarely been studied. Herein, the Fe3O4 nanoparticles, which are well encapsulated by carbon nanolayers, are uniformly dispersed on the graphene basal plane (named Fe3O4/C@G) to be used as the anode for SIBs. The existence of graphene can reduce the size of Fe3O4/C nanoparticles from 150 to 80 nm and greatly boost charge transport capability of electrode, resulting in an obvious size decrease of superparamagnetic Fe nanoparticles generated from the conversion reaction from 5 to 2 nm. Importantly, the ultra‐small superparamagnetic Fe nanoparticles (≈2 nm) can induce a strong spin‐polarized surface capacitance effect at operating temperatures ranging from −40 to 60 °C, thus achieving highly efficient Na‐ion transport and storage in a wide operation‐temperature range. Consequently, the Fe3O4/C@G anode shows high capacity, excellent fast‐charging capability, and cycling stability ranging from −40 to 60 °C in half/full cells. This work demonstrates the viability of Fe3O4 as anode for wide operation‐temperature SIBs and reveals that spin‐polarized surface capacitance effects can promote Na‐ion storage over a wide operation temperature range. Fe3O4 is widely investigated as an anode for ambient SIBs, but its sodium storage performance in wide operation‐temperature range has rarely been studied. This work reveals that Fe nanoparticles generated from Fe3O4 in conversion reaction induce strong spin‐polarized surface capacitance effect to boost sodium storage over a wide operating temperature of −40–60 °C.