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Thus, a novel zinc\u2013manganese composite sorbent supported on three\u2013dimensional carbon nanofiber aerogels (Zn\u2013MnCAs) is proposed to synergistically enhance the desulfurization efficiency through structural design and active phase regulation. The carbon nanofiber aerogel supporter possesses a dual\u2013interpenetrating network structure, high porosity (&gt;99%), and excellent anti\u2013shrinkage properties. Its three\u2013dimensional and open\u2013pore structure significantly promotes gas mass transfer, with a permeability 28 times higher than that of traditional nanofiber membranes. Meanwhile, the loading content of MnO\n                    <jats:sub>2<\/jats:sub>\n                    and its desulfurization performance are remarkably improved after redox reaction. On this basis, by further optimizing the zinc salt concentration in the hydrothermal solution, the Zn\u2013MnCAs sorbent exhibits outstanding performance in desulfurization evaluation, achieving a sulfur capacity of 10.3\u00a0g S\/100\u00a0g sorbent and a zinc utilization rate as high as 91.1%. In situ XRD, EXAFS, and DFT calculations reveal that the presence of highly dispersed and abundant ZnO is the main reason for the enhanced performance. This work provides a new material design concept for developing desulfurization sorbents with high performance.\n                  <\/jats:p>","DOI":"10.1002\/anie.8536023","type":"journal-article","created":{"date-parts":[[2026,5,20]],"date-time":"2026-05-20T08:43:31Z","timestamp":1779266611000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Synergistic Tuning of Structure and Active Phases in Zn\u2013Mn Loaded Carbon Nanofiber Aerogel for High\u2013Efficiency Desulfurization"],"prefix":"10.1002","volume":"65","author":[{"given":"Yangjie","family":"Sun","sequence":"first","affiliation":[{"name":"State Key Laboratory of Clean and Efficient Coal Utilization Taiyuan University of Technology  Taiyuan P.R. China"},{"name":"Key Laboratory of Coal Science and Technology Ministry of Education Taiyuan University of Technology  Taiyuan P.R. 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