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However, traditional recycling processes often face challenges, such as high-energy consumption, complex procedures, and excessive use of corrosive reagents. In this study, an advanced liquid-phase reduction-driven strategy is employed to selectively extract Li from spent LiNixCoyMn1\u2013x\u2013yO2 (NCM) batteries and regenerate the NCM cathode materials. During the delithiation process, Li+ is leached into the liquid phase from spent NCM material, while the Ni, Co, and Mn elements remain in the solid phase, with N2H4\u00b7H2O serving as the sole reagent. Under optimal reaction conditions, the Li leaching efficiency reaches 98.9%. Thermodynamic analysis and XRD results reveal that the delithiation reaction involves the transformation of spent NCM into a layered Ni\u2013Co\u2013Mn hydroxide (Ni\/Co\/Mn(OH)2). Additionally, the Li-rich leachate can be recovered as Li2CO3 products, while the Ni-, Co-, and Mn-enriched residues serve as the precursor for regenerating NCM cathode materials. The regenerated NCM exhibits a discharge-specific capacity of 183.0 mAh g\u20131 at 1C with a retention rate of 79.9% after 300 cycles. Overall, this work provides novel insights into the efficient closed-loop recycling of spent NCM batteries by leveraging the delithiation conversion technique.<\/jats:p>","DOI":"10.1021\/acsami.5c07151","type":"journal-article","created":{"date-parts":[[2025,7,14]],"date-time":"2025-07-14T09:03:21Z","timestamp":1752483801000},"page":"41946-41957","source":"Crossref","is-referenced-by-count":3,"title":["Closed-Loop Recycling\nof Spent LiNi\n                    <i>x<\/i>\n                    Co\n                    <i>y<\/i>\n                    Mn1\u2013\n                    <i>x<\/i>\n                    \u2013\n                    <i>y<\/i>\n                    O2 Batteries Based on\nLiquid-Phase Reduction-Driven Delithiation Conversion"],"prefix":"10.1021","volume":"17","author":[{"given":"Baichao","family":"Zhang","sequence":"first","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lu","family":"Yang","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Fangjun","family":"Zhu","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xinyu","family":"Hu","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chuanyong","family":"Niu","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hanrui","family":"Ding","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shuo","family":"Chen","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ningyun","family":"Hong","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wentao","family":"Deng","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guoqiang","family":"Zou","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8201-4614","authenticated-orcid":true,"given":"Hongshuai","family":"Hou","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5405-7913","authenticated-orcid":true,"given":"Xiaobo","family":"Ji","sequence":"additional","affiliation":[{"name":"Central South University , , ,","place":["Changsha, China, 410083"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2025,7,14]]},"reference":[{"issue":"14","key":"2026072521110033300_cit1","doi-asserted-by":"publisher","first-page":"7020","DOI":"10.1021\/acs.chemrev.9b00535","article-title":"Sustainable recycling technology\nfor Li-ion batteries and beyond: challenges and future prospects","volume":"120","author":"Fan","year":"2020","journal-title":"Chem. 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Evidence for layered cobalt-manganese particles\non alumina and silica","volume":"113","author":"Tan","year":"1991","journal-title":"J. Am. Chem. Soc."},{"key":"2026072521110033300_cit28","doi-asserted-by":"publisher","first-page":"193","DOI":"10.1016\/j.wasman.2023.02.034","article-title":"Recover value metals from spent lithium-ion\nbatteries via a combination of in-situ reduction pretreatment and\nfacile acid leaching","volume":"161","author":"Zhang","year":"2023","journal-title":"Waste Manag."},{"issue":"31","key":"2026072521110033300_cit29","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201701385","article-title":"Interfacial\nCharge Engineering in Ferroelectric-Controlled Mott Transistors","volume":"29","author":"Chen","year":"2017","journal-title":"Adv. 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Chem.\nRes."},{"issue":"50","key":"2026072521110033300_cit45","doi-asserted-by":"publisher","first-page":"16997","DOI":"10.1021\/acssuschemeng.1c05809","article-title":"Restoring surface defect\ncrystal\nof Li-lacking LiNi0.6Co0.2Mn0.2O2 material particles toward more efficient\nrecycling of lithium-ion batteries. ACS Sustainable","volume":"9","author":"Yang","year":"2021","journal-title":"Chem. 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