Chelin Jeon, Yiseul Yoo, Eunji Kwon, Sang Hyuk Gong, Mingony Kim, Sang‐Ok Kim, Hyung‐Seok Kim, Hun‐Gi Jung, Kyung Yoon Chung, Yoon Seok Jung, Seungho Yu
Fluorinated halide solid electrolytes (FHSEs) enable integration with high-voltage layered oxides in all-solid-state sodium-ion batteries (ASSSIBs). Here, we demonstrate high-voltage ASSSIBs by pairing a fluorine-substituted UCl 3 -type chloride solid electrolyte, Na 0.6 Ta 0.2 La 0.8 Cl 3.7 F 0.3, with a P2-type Na 0.8 Li 0.1 Ni 0.2 Mn 0.7 O 2 cathode. The ASSSIB achieves reversible oxygen redox up to 4.6 V and delivers 132 mAh g –1 with long-term cycling stability, surpassing the performance of liquid electrolytes and nonfluorinated halide counterparts. Electrochemical and structural analyses reveal that, in liquid-electrolyte cells, oxygen redox above 4.2 V becomes irreversible due to solvent oxidation and surface-layer formation, while phase transitions further degrade structural reversibility. In contrast, the FHSE preserves the P2 framework and stabilizes oxygen-redox activity, enabling higher capacity and long-term cycling stability. Supported by integrated theoretical calculations, electrochemical analyses, and advanced characterizations, this work presents a viable strategy for advancing high-voltage ASSSIBs. Overall, FHSEs enable stabilized oxygen redox above 4.2 V and realize durable, high-energy ASSSIBs.