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Developing multicomponent composite materials with delicate morphology and tailored structure is of vital importance for designing advanced sodium‐ion batteries (SIBs). Herein, a confinement‐structured Fe2Mo3O8@C@MoS2 with local‐expanded interlayer spacing is designed via high‐temperature phase transition from FeMoO4 to Fe2Mo3O8 and the tactically introducing dopamine molecules into the interlayer of MoS2 nanosheets. By analysis of the in situ generated solid electrolyte interphase film in different electrolytes, the favorable compatibility of Fe2Mo3O8@C@MoS2 in ether‐based electrolytes is well illustrated. Importantly, the sodium storage mechanism and detailed structural evolution of Fe2Mo3O8 are established for the first time by in situ X‐ray diffraction. Furthermore, theoretical calculations indicate the unique structure facilitates internal charge transfer and enhances Na+ adsorption ability. Thanks to the unique confinement structure, local‐expanded interlayers and robust framework, the Fe2Mo3O8@C@MoS2 composite achieves a high reversible specific capacity of 636 mAh g‒1 at 0.1 A g‒1, excellent rate capability (301 mAh g‒1 at 5.0 A g‒1) and ultralong cycling stability (365 mAh g–1 after 6000 cycles at 2.0 A g–1). The study provides an essential understanding of the Na storage mechanism of Fe2Mo3O8 and a promising strategy for constructing high‐performance anodes for SIBs. [ABSTRACT FROM AUTHOR]

Limited by sluggish reaction kinetics, insufficient electrode utilization and severe volume deformation, designing nickel‐based materials with high capacity and rate capability is still a challenge. Herein, a carbon nanotubes threaded NiSe2/Co3Se4 quantum dots embedded in carbon nanospheres with rich Se vacancies both in NiSe2 and Co3Se4 is elaborately designed via MOF template method. The formation mechanism of the Se vacancies is elucidated for the first time, which is ascribed to the release of gas during the decomposition of organic ligand inhibits the ordered arrangement of atoms. The CNT‐V‐NiCoSe possesses many significant superiorities, such as sufficiently exposed active sites, high electrode utilization, favorable charge‐carrier migration, and relaxed structure deformation. Consequently, the CNT‐V‐NiCoSe electrode shows top‐level specific capacity (384 mAh g−1 at 1 A g−1), ultrahigh rate capability (209 mAh g−1 at 150 A g−1) and remarkable cycling durability. The CNT‐V‐NiCoSe//Zn battery achieves maximum energy density of 615.6 Wh kg−1 and maximum power density of 81.7 kW kg−1. Density functional theory calculations elucidate the Se vacancies improve the density of states at Fermi level, facilitates internal charge transfer, and enhances OH− adsorption ability. This study provides guidance for the preparation of high‐performance electrode materials with rich vacancies by template method. [ABSTRACT FROM AUTHOR]