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Conventional aprotic ether and ester solvents contain polarizable C\u2500H bonds that trigger parasitic proton transfer reactions on the high\u2010voltage cathode surface, driving exothermic electrolyte decomposition and impairing battery cycling stability and safety. Here, we show that deuterium substitution at polarizable C\u2013H moieties introduces kinetic and thermodynamic isotope effects to retard proton transfer and lower solvent oxidation Gibbs free energy. Consequently, the deuterated electrolytes exhibit improved anodic stability and mitigated decomposition during high\u2010voltage charge\u2013discharge of layered oxide cathodes, forming a compact and robust cathode\u2013electrolyte interphase with suppressed CO\n                    <jats:sub>2<\/jats:sub>\n                    release. The deuterated solvents also have lower combustion enthalpies than their protiated analogs, which translates to substantially reduced heat generation as confirmed by calorimetric measurements. Using deuterated tetrahydrofuran and dimethyl carbonate as model solvents, we validate that such electrolytes enable reversible cathode electrochemistry, as well as markedly improved cycling performance and thermal safety of Li||LiNi\n                    <jats:sub>0.8<\/jats:sub>\n                    Co\n                    <jats:sub>0.1<\/jats:sub>\n                    Mn\n                    <jats:sub>0.1<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    batteries. This subatomic modification strategy offers a rational electrolyte design framework toward high\u2010performance batteries.\n                  <\/jats:p>","DOI":"10.1002\/anie.6024891","type":"journal-article","created":{"date-parts":[[2026,8,23]],"date-time":"2026-08-23T17:49:51Z","timestamp":1787507391000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Deuterated Aprotic Electrolytes Enable Rechargeable Lithium Batteries With High (Electro)Chemical and Thermal Stability"],"prefix":"10.1002","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0009-0003-5257-2748","authenticated-orcid":false,"given":"Yu\u2010Hui","family":"Zhu","sequence":"first","affiliation":[{"name":"CAS Key Laboratory of Molecular Nanostructure and Nanotechnology CAS Research\/Education Center For Excellence in Molecular Sciences Beijing National Laboratory for Molecular Sciences (BNLMS) Institute of Chemistry Chinese Academy of Sciences (CAS) Beijing P. 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