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This bottleneck can be alleviated by deploying aqueous\u2010organic biphasic electrolytes, which leverage the pronounced difference in polybromide solubility between two immiscible phases to achieve effective confinement. However, a profound mechanistic understanding of ion\u2010specific functions in such systems remains elusive, and the full\u2010cell performance still falls short of commercial requirements. Herein, we systematically investigate the ion\u2010manipulated solvation environment and biphasic equilibrium of the electrolytes that correlate with the electrochemical behavior of ZBBs. Beyond anion\u2010driven phase separation, cations dictate ion\u2010pairing interactions that govern component distribution across the two phases. Compared to monovalent and trivalent counterparts, divalent cations strike an optimal thermodynamic\u2013kinetic balance, achieving a trade\u2010off between polybromide confinement and electrode reaction kinetics. Furthermore, a dual\u2010functional zwitterion is demonstrated to concurrently suppress polybromide shuttle and stabilize zinc deposition. The resulting biphasic ZBBs deliver an energy density of 40.6 Wh L\n                    <jats:sup>\u22121<\/jats:sup>\n                    and sustain a cycling life over 1000 cycles, considerably outperforming reported biphasic systems. Coupled with a low system\u2010level cost of \u223c$100 kWh\n                    <jats:sup>\u22121<\/jats:sup>\n                    , the biphasic ZBBs represent a compelling technology for grid\u2010scale energy storage.\n                  <\/jats:p>","DOI":"10.1002\/adma.72591","type":"journal-article","created":{"date-parts":[[2026,2,21]],"date-time":"2026-02-21T10:45:08Z","timestamp":1771670708000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Manipulating Ion Chemistry in Biphasic Electrolytes Toward Durable High\u2010Energy Zinc\u2013Bromine Batteries"],"prefix":"10.1002","volume":"38","author":[{"given":"Yilang","family":"Liu","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pei","family":"Tang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chuhao","family":"Ye","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Caiyang","family":"Zhi","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chengang","family":"Pei","sequence":"additional","affiliation":[{"name":"School of Chemistry and Materials Yangzhou University  Yangzhou Jiangsu P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jian","family":"Zhu","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xingbin","family":"Yan","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8479-7210","authenticated-orcid":false,"given":"Qingyun","family":"Dou","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Sun Yat\u2010Sen University  Guangzhou P. R. 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