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Combining high\u2010throughput experiments with first\u2010principles simulations, we unveil that 2D perovskites are intrinsically susceptible to thermal degradation due to the deprotonation of spacer cations and subsequent escape of hydrogen iodide. Through artificial intelligence analysis of 278 distinct perovskites, we identify the surface electrostatic properties and molecular polarity of spacer cations as the key descriptors governing thermal resilience. Finally, we discover a bi\u2010cationic 2D perovskite that integrates low\u2010polarity phenylethylammonium with high\u2010polarity pentafluorophenylethylammonium (5FBA), synergistically resolving phase segregation and thermal degradation beyond what either cation can achieve alone. The bi\u2010cationic 3D\/2D perovskite film stack shows suppressed ion migration owing to the robust interaction between 5FBA and 3D perovskite. Consequently, the resulting PSCs retain over 92% of their initial efficiency after 1500\u00a0h of thermal aging at 85\u00b0C and over 90% after 2000\u00a0h of continuous operation under 1\u2010Sun illumination.<\/jats:p>","DOI":"10.1002\/adma.75134","type":"journal-article","created":{"date-parts":[[2026,9,24]],"date-time":"2026-09-24T07:47:39Z","timestamp":1790236059000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Synergy of Low\u2010 and High\u2010Polarity Cations for Stabilizing 2D Perovskites"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3199-3100","authenticated-orcid":false,"given":"Hongbin","family":"Xiao","sequence":"first","affiliation":[{"name":"National Key Laboratory of Electronic Films and Integrated Devices School of Integrated Circuit Science and Engineering University of Electronic Science and Technology of China  Chengdu 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