Wei Zhang, Chengjun Lei, Yunting Wu, Tiankun Zhou, Jianmin Zhao, X. C. Li, Xin He, Xiao Liang
Lithium metal batteries (LMBs) promise ultrahigh energy density, but deep eutectic electrolytes (DEEs) suffer from intrinsically low lithium-ion transference numbers ( ), an overlooked weakness that exacerbates concentration polarization and interfacial instability, especially under high-voltage operation. Here, we report a supramolecular DEE comprising 18-crown-6 (18C6) and lithium nonafluorobutanesulfonate (LiNFSA) that achieves quasi-single-ion conduction ( = 0.88) and a 5.3 V stability window—benchmarks unprecedented for DEEs. Results reveal that the Li + –18C6 chelation, combined with the bulky, charge-delocalized and geometrically mismatched NFSA - anion, suppresses correlated cation–anion migration, resulting in high- conduction. The optimized electrolyte (LNC-2.5) enables uniform LiF-rich solid–electrolyte interphases and cathode–electrolyte interphases, effectively mitigating dendrite growth, side reactions, and transition-metal dissolution. In high-voltage LMBs, it enables long-term cycling stability and low polarization, with nearly 100% capacity retention over 450 cycles using LiMnFePO 4 cathodes, while maintaining broad compatibility with LiCoO 2 , LiFePO 4 , organic cathodes, and pouch-cell configurations. This work establishes a supramolecular design principle to couple selective Li + transport with interfacial durability for safe, high-performance LMBs. • Introduces a universal dual supramolecular and anion-engineering design principle for achieving high- electrolytes. • Demonstrates a of 0.88 with 5.3 V electrochemical stability, a record high among all reported DEEs. • LNC-2.5 promotes the formation of LiF-enriched SEIs and CEIs, resulting in stable interphases and high-voltage compatibility.