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This study reports an amorphous Zn_xMo₃S₁₃chalcogel, reveals its local structure, and shows outstanding Li/Zn_xMo₃S₁₃electrochemical performance enabled by its amorphous structure, Zn-mediated polysulfide anchoring, and a stable SEI layer. 

Abstract Chalcogel represents a unique class of meso‐ to macroporous nanomaterials that offer applications in energy and environmental pursuits. Here, the synthesis of an ion‐exchangeable amorphous chalcogel using a nominal composition of K₂CoMo₂S₁₀(KCMS) at room temperature is reported. Synchrotron X‐ray pair distribution function (PDF), X‐ray absorption near‐edge structure (XANES), and extended X‐ray absorption fine structure (EXAFS) reveal a plausible local structure of KCMS gel consisting of Mo⁵⁺₂and Mo⁴⁺₃clusters in the vicinity of di/polysulfides which are covalently linked by Co²⁺ions. The ionically bound K⁺ions remain in the percolating pores of the Co–Mo–S covalent network. XANES of Co K‐edge shows multiple electronic transitions, including quadrupole (1s→3d), shakedown (1s→4p + MLCT), and dipole allowed 1s→4p transitions. Remarkably, despite a lack of regular channels as in some crystalline solids, the amorphous KCMS gel shows ion‐exchange properties with UO₂²⁺ions. Additionally, it also presents surface sorption via [S∙∙∙∙UO₂²⁺] covalent interactions. Overall, this study underscores the synthesis of quaternary chalcogels incorporating alkali metals and their potential to advance separation science for cations and oxo‐cationic species by integrating a synergy of surface sorption and ion‐exchange.