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Herein, we propose a dynamic covalent disulfide\u2010mediated confinement assembly strategy, wherein thioctate is integrated into poly(acrylic acid) networks to demonstrate the biomimetic phase evolution process. The resultant polymer exhibits thermal\u2010induced hyperhardening transition from a soft hydrogel to a rigid glassy material, with a record\u2010breaking 27\u00a0000\u2010fold increase in modulus, from 8 \u00d7 10\n                    <jats:sup>\u22124<\/jats:sup>\n                    to 22\u00a0MPa. The significant mechanical reinforcement is attributed to thermal\u2010driven hydrophobic aggregation of 1,2\u2010dithiolane motifs. The local concentrated monomers further trigger the disulfide\u2010mediate ring\u2010opening polymerization into covalently crosslinked microspheres, which effectively reinforce poly(acrylic acid) backbones via dynamic reconstruction of calcium (II) \u2010carboxyl coordination. The potential application of soft actuators featuring composite architectures is demonstrated by integrating the rapid hyperhardening transition and prolonged mechanical stability of the hydrogels, as well as robust interfacial bonding capability via disulfide exchange. This universal phase evolution strategy based on dynamic covalent chemistry establishes an ideal material platform for developing multi\u2010mode, on\u2010demand regulation of high\u2010performance adaptive materials.\n                  <\/jats:p>","DOI":"10.1002\/adma.202523672","type":"journal-article","created":{"date-parts":[[2026,3,8]],"date-time":"2026-03-08T18:37:55Z","timestamp":1772995075000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Disulfide\u2010Mediated Confinement Assembly Enabling Thermal\u2010Hyperhardening Hydrogels via Phase Evolution"],"prefix":"10.1002","volume":"38","author":[{"given":"Jun\u2010Yu","family":"Shen","sequence":"first","affiliation":[{"name":"Key Laboratory For Advanced Materials and Joint International Research Laboratory of Precision Chemistry and Molecular Engineering Feringa Nobel Prize Scientist Joint Research Center Frontiers Science Center For Materiobiology and Dynamic Chemistry Institute of Fine Chemicals School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai P.R. 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