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Here, we investigate the structural evolution of a sulfur\u2010rich polymer into a hybrid sulfur\u2010carbon via inverse vulcanization and thermal condensation. Multiscale analyses reveal a stepwise transformation, beginning with the emergence of sulfur radicals at \u223c175\u00b0C, followed by the progressive development of a carbon matrix above 300\u00b0C that stabilizes the radical species. Around 450\u00b0C, a transitional phase forms, consisting of conjugated carbon clusters covalently bonded to sulfur chains. This hybrid structure confines sulfur within pseudo\u2010graphitic nanodomains, effectively suppressing polysulfide dissolution and enhancing redox stability. DFT simulations show how sulfur confinement modulates Na\u2010S reaction energetics, while electrochemical testing confirms high sulfur utilization, delivering \u223c1000\u00a0mAh  and 1200\u00a0Wh , setting a new performance benchmark for room\u2010temperature Na\u2500S batteries. These findings provide critical insights into the correlation between structural evolution and electrochemical performance, offering design principles for next\u2010generation sulfur\u2010based electrodes.<\/jats:p>","DOI":"10.1002\/adma.202513346","type":"journal-article","created":{"date-parts":[[2026,1,19]],"date-time":"2026-01-19T09:37:21Z","timestamp":1768815441000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Unravelling the Secret of Sulfur Confinement and High Sulfur Utilization in Hybrid Sulfur\u2010Carbons"],"prefix":"10.1002","volume":"38","author":[{"given":"Tim","family":"Horner","sequence":"first","affiliation":[{"name":"Department of Colloid Chemistry, Max Planck Institute of Colloids and Interfaces Potsdam Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Enis O\u011fuzhan","family":"Eren","sequence":"additional","affiliation":[{"name":"Department of Colloid Chemistry, Max 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