Eco-Friendly Synthesis of Hierarchical Heterostructured CsV3O8/V2O5 Composite Cathode: Lattice Stabilization and Vanadium Dissolution Resistance for Long-Life Aqueous Zinc-Ion Batteries

Eco-Friendly Synthesis of Hierarchical Heterostructured CsV3O8/V2O5 Composite Cathode: Lattice Stabilization and Vanadium Dissolution Resistance for Long-Life Aqueous Zinc-Ion Batteries | 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 Eco-Friendly Synthesis of Hierarchical Heterostructured CsV 3 O 8 /V 2 O 5 Composite Cathode: Lattice Stabilization and Vanadium Dissolution Resistance for Long-Life Aqueous Zinc-Ion Batteries Hari Bandi, Shanthappa R, Sowjanya Vallem, Daniel Ioan Stroe, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7856694/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 07 Feb, 2026 Read the published version in Advanced Composites and Hybrid Materials → Version 1 posted 9 You are reading this latest preprint version Abstract Developing durable and high-capacity cathode materials is key to advancing aqueous zinc-ion batteries (ZIBs). Herein, we propose a hierarchical heterostructured CsV 3 O 8 /V 2 O 5 composite (HH–CsVO/VO) cathode synthesized via a simple, cost-effective, and eco-friendly ambient-temperature stirring method. The incorporation of Cs + ions into the VO framework induces significant lattice compression, compressive strain, and new V coordination environments, leading to mixed-valence V states (V 5+ /V 4+ /V 3+ ), as confirmed by solid-state 51 V nuclear magnetic resonance (NMR) spectroscopy and ex-situ X-ray photoelectron spectroscopy (XPS) analyses. This structural modulation is accompanied by band gap narrowing (2.71 → 2.19 eV) and a reduced work function (5.00 → 4.14 eV), enhancing redox kinetics and Zn²⁺ intercalation pathways. Raman and Fourier-transform infrared spectroscopy analyses reveal Cs-induced lattice distortion and compressive strain, while ultraviolet photoelectron spectroscopy confirms interfacial electronic modulation. Ex-situ X-ray diffraction and XPS demonstrate highly reversible phase evolution and structural stability during cycling. The HH–CsVO/VO electrode delivers a high reversible capacity of 482.7 mAh g -1 after 200 cycles at 0.3 A g -1 and maintains 240.63 mAh g -1 after 3000 cycles at 3 A g -1 , outperforming pristine VO. Notably, the composite exhibits suppressed voltage polarization and significantly reduced V dissolution, supported by immersion tests and stable cycling. Although Cs–O bonding is not vibrationally active, it is proposed to stabilize vanadyl surface groups and limit dissolution. This study introduces a previously unreported vanadate heterostructure and demonstrates how interfacial engineering and electronic structure modulation can enable high-performance, sustainable aqueous ZIB cathodes. CsV3O8/V2O5 composite Eco-friendly synthesis Vanadium dissolution suppression hierarchical heterostructured cathode Aqueous zinc-ion battery Full Text Additional Declarations No competing interests reported. Supplementary Files Supplementarymaterial.docx Cite Share Download PDF Status: Published Journal Publication published 07 Feb, 2026 Read the published version in Advanced Composites and Hybrid Materials → Version 1 posted Editorial decision: Revision requested 08 Dec, 2025 Reviews received at journal 08 Dec, 2025 Reviews received at journal 30 Nov, 2025 Reviewers agreed at journal 25 Nov, 2025 Reviewers agreed at journal 24 Nov, 2025 Reviewers invited by journal 21 Nov, 2025 Editor assigned by journal 19 Nov, 2025 Submission checks completed at journal 17 Oct, 2025 First submitted to journal 14 Oct, 2025 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. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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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-7856694","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":531033208,"identity":"ed26676f-665c-4de5-b42a-a3f7500c2474","order_by":0,"name":"Hari Bandi","email":"","orcid":"","institution":"Kyung Hee University","correspondingAuthor":false,"prefix":"","firstName":"Hari","middleName":"","lastName":"Bandi","suffix":""},{"id":531033209,"identity":"41a10472-f653-43e7-a472-f2e3fad8fd1a","order_by":1,"name":"Shanthappa R","email":"","orcid":"","institution":"Kyung Hee 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Batteries\u003c/p\u003e","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":true,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":true,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"advanced-composites-and-hybrid-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"achm","sideBox":"Learn more about [Advanced Composites and Hybrid Materials](https://link.springer.com/journal/42114)","snPcode":"42114","submissionUrl":"https://submission.nature.com/new-submission/42114/3","title":"Advanced Composites and Hybrid Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"CsV3O8/V2O5 composite, Eco-friendly synthesis, Vanadium dissolution suppression, hierarchical heterostructured cathode, Aqueous zinc-ion battery","lastPublishedDoi":"10.21203/rs.3.rs-7856694/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7856694/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eDeveloping durable and high-capacity cathode materials is key to advancing aqueous zinc-ion batteries (ZIBs). Herein, we propose a hierarchical heterostructured CsV\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e8\u003c/sub\u003e/V\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5 \u003c/sub\u003ecomposite (HH–CsVO/VO) cathode synthesized via a simple, cost-effective, and eco-friendly ambient-temperature stirring method. The incorporation of Cs\u003csup\u003e+\u003c/sup\u003e ions into the VO framework induces significant lattice compression, compressive strain, and new V coordination environments, leading to mixed-valence V states (V\u003csup\u003e5+\u003c/sup\u003e/V\u003csup\u003e4+\u003c/sup\u003e/V\u003csup\u003e3+\u003c/sup\u003e), as confirmed by solid-state \u003csup\u003e51\u003c/sup\u003eV nuclear magnetic resonance (NMR) spectroscopy and ex-situ X-ray photoelectron spectroscopy (XPS) analyses. This structural modulation is accompanied by band gap narrowing (2.71 → 2.19 eV) and a reduced work function (5.00 → 4.14 eV), enhancing redox kinetics and Zn²⁺ intercalation pathways. Raman and Fourier-transform infrared spectroscopy analyses reveal Cs-induced lattice distortion and compressive strain, while ultraviolet photoelectron spectroscopy confirms interfacial electronic modulation. Ex-situ X-ray diffraction and XPS demonstrate highly reversible phase evolution and structural stability during cycling. The HH–CsVO/VO electrode delivers a high reversible capacity of 482.7 mAh g\u003csup\u003e-1 \u003c/sup\u003eafter 200 cycles at 0.3 A g\u003csup\u003e-1\u003c/sup\u003e and maintains 240.63 mAh g\u003csup\u003e-1\u003c/sup\u003e after 3000 cycles at 3 A g\u003csup\u003e-1\u003c/sup\u003e, outperforming pristine VO. Notably, the composite exhibits suppressed voltage polarization\u003cstrong\u003e \u003c/strong\u003eand significantly reduced V dissolution, supported by immersion tests and stable cycling. Although Cs–O bonding is not vibrationally active, it is proposed to stabilize vanadyl surface groups and limit dissolution. This study introduces a previously unreported vanadate heterostructure and demonstrates how interfacial engineering and electronic structure modulation can enable high-performance, sustainable aqueous ZIB cathodes.\u003c/p\u003e","manuscriptTitle":"Eco-Friendly Synthesis of Hierarchical Heterostructured CsV3O8/V2O5 Composite Cathode: Lattice Stabilization and Vanadium Dissolution Resistance for Long-Life Aqueous Zinc-Ion Batteries","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-11-06 06:53:58","doi":"10.21203/rs.3.rs-7856694/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-12-08T15:32:07+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-12-08T11:09:46+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-12-01T01:12:30+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"63314025917032708715964621163853634421","date":"2025-11-25T12:08:38+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"204853399116874400758789788916952450092","date":"2025-11-24T19:49:29+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-11-21T15:11:56+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-11-19T13:22:35+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-10-17T06:59:09+00:00","index":"","fulltext":""},{"type":"submitted","content":"Advanced Composites and Hybrid Materials","date":"2025-10-14T09:10:45+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"advanced-composites-and-hybrid-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"achm","sideBox":"Learn more about [Advanced Composites and Hybrid Materials](https://link.springer.com/journal/42114)","snPcode":"42114","submissionUrl":"https://submission.nature.com/new-submission/42114/3","title":"Advanced Composites and Hybrid Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"2120b188-9d48-48fb-bbb0-69c46e6c63e5","owner":[],"postedDate":"November 6th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2026-02-09T16:06:20+00:00","versionOfRecord":{"articleIdentity":"rs-7856694","link":"https://doi.org/10.1007/s42114-026-01644-7","journal":{"identity":"advanced-composites-and-hybrid-materials","isVorOnly":false,"title":"Advanced Composites and Hybrid Materials"},"publishedOn":"2026-02-07 15:59:22","publishedOnDateReadable":"February 7th, 2026"},"versionCreatedAt":"2025-11-06 06:53:58","video":"","vorDoi":"10.1007/s42114-026-01644-7","vorDoiUrl":"https://doi.org/10.1007/s42114-026-01644-7","workflowStages":[]},"version":"v1","identity":"rs-7856694","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7856694","identity":"rs-7856694","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}