{"paper_id":"0ac0192c-ea46-4757-b85d-ad05d6e68cd1","body_text":"Recycling of Lithium from Cathod of Lithiumion Batteries using Direct Lithiation | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Recycling of Lithium from Cathod of Lithiumion Batteries using Direct Lithiation Pratik Bhattacharyya This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-9210779/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract The increasing deployment of lithium-ion batteries (LIBs), particularly lithium iron phosphate (LiFePO₄, LFP) systems, necessitates the development of efficient and sustainable recycling methods. Conventional recycling approaches are often energy-intensive, multi-step, and economically unfavorable for LFP materials. In this work, a simple, low-cost, and environmentally sustainable strategy for the regeneration of spent Li₁₋ₓFePO₄ cathodes is presented. The process involves delamination of the cathode material via water treatment, followed by two regeneration routes: (i) direct re-lithiation using a lithium-based eutectic solvent composed of lithium acetate and ethylene glycol in the presence of organic reducing agents, and (ii) a two-step oxidative leaching using FeCl₃ followed by reductive re-lithiation. Among the reducing agents evaluated, hydroquinone demonstrated superior redox reversibility and regeneration efficiency. The direct re-lithiation process, performed under ambient conditions, successfully restored the olivine LiFePO₄ structure with minimal structural degradation. Electrochemical evaluation revealed significantly improved discharge capacity and cycling stability compared to the spent material. In contrast, the two-step approach resulted in lower electrochemical performance and increased process complexity. The proposed method offers a scalable, energy-efficient, and sustainable pathway for LFP recycling, contributing to the advancement of circular battery technologies. Environmental Engineering Electrochemistry Renewable Resources Direct re-lithiation Oxidative leaching Re-lithiation Surface morphology Xrd Electrochemical impedance spectroscopy of restored LiFePO4 and Rate capability Full Text Additional Declarations The authors declare no competing interests. Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {\"props\":{\"pageProps\":{\"initialData\":{\"identity\":\"rs-9210779\",\"acceptedTermsAndConditions\":true,\"allowDirectSubmit\":true,\"archivedVersions\":[],\"articleType\":\"Research Article\",\"associatedPublications\":[],\"authors\":[{\"id\":611308853,\"identity\":\"e89e32f7-873b-4fcf-846a-f964c765ffee\",\"order_by\":0,\"name\":\"Pratik Bhattacharyya\",\"email\":\"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA5ElEQVRIiWNgGAWjYBACAzD5wyaBgYH5AJAlIUOMFsYGxp40oBa2BJAWHuK0MLAdBirnAdtIWIu5RO7xxzw8aXnm/Wc+v7pRY8HDwH746AZ8Wixn5CU281jYFMvcyN1mnXMM6DCetLQbeB12I8ewGWhL4gwJ3m3GOWxALRI8ZkRoYTucOIP/zDPjnH8kaWHIYX6c20aEFsueN4Yz5/akFUtIpJkx5/ZJ8LAR8os5e47Bhzc/bPIk+A8//pzzrU6On/3wMbxaQIAJGhdsEmCSkHIQYPwBoZk/EKN6FIyCUTAKRh4AAIBPRu6etR62AAAAAElFTkSuQmCC\",\"orcid\":\"https://orcid.org/0009-0000-9521-3444\",\"institution\":\"Bhaskar Engineering College, Hyderabad\",\"correspondingAuthor\":true,\"prefix\":\"\",\"firstName\":\"Pratik\",\"middleName\":\"\",\"lastName\":\"Bhattacharyya\",\"suffix\":\"\"}],\"badges\":[],\"createdAt\":\"2026-03-24 10:51:07\",\"currentVersionCode\":1,\"declarations\":{\"humanSubjects\":false,\"vertebrateSubjects\":true,\"conflictsOfInterestStatement\":false,\"humanSubjectEthicalGuidelines\":false,\"humanSubjectConsent\":false,\"humanSubjectClinicalTrial\":false,\"humanSubjectCaseReport\":false,\"vertebrateSubjectEthicalGuidelines\":true},\"doi\":\"10.21203/rs.3.rs-9210779/v1\",\"doiUrl\":\"https://doi.org/10.21203/rs.3.rs-9210779/v1\",\"draftVersion\":[],\"editorialEvents\":[],\"editorialNote\":\"\",\"failedWorkflow\":false,\"files\":[{\"id\":105344055,\"identity\":\"0e554ca2-4207-4cce-8c40-40bc89de2a77\",\"added_by\":\"auto\",\"created_at\":\"2026-03-25 03:31:07\",\"extension\":\"pdf\",\"order_by\":1,\"title\":\"\",\"display\":\"\",\"copyAsset\":false,\"role\":\"manuscript-pdf\",\"size\":610678,\"visible\":true,\"origin\":\"\",\"legend\":\"\",\"description\":\"\",\"filename\":\"DOC20260324WA0007..pdf\",\"url\":\"https://assets-eu.researchsquare.com/files/rs-9210779/v1_covered_e648ea8d-9f97-4ca1-aa5b-91f3743e155f.pdf\"}],\"financialInterests\":\"The authors declare no competing interests.\",\"formattedTitle\":\"\\u003cp\\u003eRecycling of Lithium from Cathod of Lithiumion Batteries using Direct Lithiation\\u003c/p\\u003e\",\"fulltext\":[],\"fulltextSource\":\"\",\"fullText\":\"\",\"funders\":[],\"hasAdminPriorityOnWorkflow\":false,\"hasManuscriptDocX\":false,\"hasOptedInToPreprint\":true,\"hasPassedJournalQc\":\"\",\"hasAnyPriority\":true,\"hideJournal\":true,\"highlight\":\"\",\"institution\":\"Bhaskar Engineering College, Hyderabad \",\"isAcceptedByJournal\":false,\"isAuthorSuppliedPdf\":true,\"isDeskRejected\":\"\",\"isHiddenFromSearch\":false,\"isInQc\":false,\"isInWorkflow\":false,\"isPdf\":true,\"isPdfUpToDate\":true,\"isWithdrawnOrRetracted\":false,\"journal\":{\"display\":true,\"email\":\"info@researchsquare.com\",\"identity\":\"researchsquare\",\"isNatureJournal\":false,\"hasQc\":true,\"allowDirectSubmit\":true,\"externalIdentity\":\"\",\"sideBox\":\"\",\"snPcode\":\"\",\"submissionUrl\":\"/submission\",\"title\":\"Research Square\",\"twitterHandle\":\"researchsquare\",\"acdcEnabled\":true,\"dfaEnabled\":false,\"editorialSystem\":\"\",\"reportingPortfolio\":\"\",\"inReviewEnabled\":false,\"inReviewRevisionsEnabled\":true},\"keywords\":\"Direct re-lithiation, Oxidative leaching Re-lithiation, Surface morphology, Xrd ,Electrochemical impedance spectroscopy of restored LiFePO4 and Rate capability\",\"lastPublishedDoi\":\"10.21203/rs.3.rs-9210779/v1\",\"lastPublishedDoiUrl\":\"https://doi.org/10.21203/rs.3.rs-9210779/v1\",\"license\":{\"name\":\"CC BY 4.0\",\"url\":\"https://creativecommons.org/licenses/by/4.0/\"},\"manuscriptAbstract\":\"\\u003cp\\u003eThe increasing deployment of lithium-ion batteries (LIBs), particularly lithium iron phosphate (LiFePO₄, LFP) systems, necessitates the development of efficient and sustainable recycling methods. 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