Near-Quantitative Electrocatalytic Oxidation of HMF to FDCA over a NiMoCu Heterojunction Catalyst

Near-Quantitative Electrocatalytic Oxidation of HMF to FDCA over a NiMoCu Heterojunction Catalyst | 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 Near-Quantitative Electrocatalytic Oxidation of HMF to FDCA over a NiMoCu Heterojunction Catalyst Dongyu Cao, Haitao Gao, Tianyi Wang, Jinbo Chen This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-9109966/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 10 You are reading this latest preprint version Abstract The conversion of 5-hydroxymethylfurfural (HMF) into the high-value-added product 2,5-furandicarboxylic acid (FDCA) requires efficient and stable electrocatalysts. A three-dimensional porous nanosheet -structured nickel-molybdenum-copper (NiMoCu) ternary catalyst was fabricated on nickel foam via a two-step electrodeposition strategy followed by alkaline heat treatment.Multiple heterointerfaces (MoO₃-CuO/NiOOH) were confirmed to form through the homogeneous integration of Ni, Mo, and Cu elements at the nanoscale, as evidenced by comprehensive characterization (XRD, Raman, TEM, and XPS). Simultaneously, the incorporation of Cu refined the grain size of MoO₃ to 8.2 nm and facilitated the in situ formation of amorphous NiOOH (containing Ni³⁺ species). Moreover, the interfacial electron transfer effect optimized the charge transport pathway, thereby promoting efficient 5-hydroxymethylfurfural oxidation reaction (HMFOR).At1.47 V vs. RHE, the catalyst demonstrated record-breaking performance for HMF electric oxidation, achieving 99% HMF conversion, nearly 100% FDCA selectivity, 98% FDCA yield, and a Faradaic efficiency of 98%. Notably, it retained over 90% of its initial FDCA yield after four consecutive reaction cycles, corresponding to a minimal activity decay of less than 10%.The superior catalytic performance of the NiMoCu ternary catalyst originates from the effective synergy of its three metallic components. Specifically, Ni³⁺ species serve as dynamicactive sites that efficiently drive the reaction, while Mo⁶⁺ species stabilize the Ni³⁺ valence state and accelerate charge migration. Concurrently, the incorporation of Cu selectively suppresses the competing oxygen evolution reaction (OER contribution < 2%). This work presents an effective strategy for designing highly efficient and stable catalysts dedicated to the electrocatalytic conversion of the key biomass platform compound, HMF. 5-Hydroxymethylfurfural (HMF) Electrocatalytic oxidation NiMoCu ternary catalyst Heterojunction 2 5-Furandicarboxylic acid (FDCA) Full Text Additional Declarations No competing interests reported. Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 13 Apr, 2026 Reviews received at journal 25 Mar, 2026 Reviewers agreed at journal 22 Mar, 2026 Reviewers agreed at journal 21 Mar, 2026 Reviews received at journal 20 Mar, 2026 Reviewers agreed at journal 20 Mar, 2026 Reviewers invited by journal 19 Mar, 2026 Editor assigned by journal 15 Mar, 2026 Submission checks completed at journal 15 Mar, 2026 First submitted to journal 12 Mar, 2026 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. We do this by developing innovative software and high quality services for the global research community. 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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-9109966","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":610299441,"identity":"b15039a1-ef4f-44bc-8ab8-6be63d2707e3","order_by":0,"name":"Dongyu Cao","email":"","orcid":"","institution":"Zhejiang Sci-Tech University","correspondingAuthor":false,"prefix":"","firstName":"Dongyu","middleName":"","lastName":"Cao","suffix":""},{"id":610299442,"identity":"d77071f2-562e-46c2-b397-d7ea932ffa5e","order_by":1,"name":"Haitao Gao","email":"","orcid":"","institution":"Zhejiang Sci-Tech University","correspondingAuthor":false,"prefix":"","firstName":"Haitao","middleName":"","lastName":"Gao","suffix":""},{"id":610299444,"identity":"e445fad7-2332-468f-83a7-663b5fad97b0","order_by":2,"name":"Tianyi Wang","email":"","orcid":"","institution":"Zhejiang University","correspondingAuthor":false,"prefix":"","firstName":"Tianyi","middleName":"","lastName":"Wang","suffix":""},{"id":610299446,"identity":"6af4f1e3-80ba-496d-ad74-492c05530a12","order_by":3,"name":"Jinbo Chen","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA0ElEQVRIiWNgGAWjYBACxmYGNiB1gIGBvYENLNBAvBaeA2wgirAWIIBqkUggUgtzO++xBx9q7siZS7499vgDg43shgPMzx7gdxhfuuGMY8+MLWfnpRscYEgz3nCAzdwAvxYeM2nehsOJG27nmEkcYAAyDvCwSRCjpX7DzTMgLf+J15JgcIMHpOUAUVrMgX45bLjhTI65wRmDZOOZh9nM8Gox7D9jBgyxw/IGx4GMigo72b7jzc/wa2lA4YKCihmfeiCQJyA/CkbBKBgFo4CBAQBotkuOOGTflwAAAABJRU5ErkJggg==","orcid":"","institution":"NingboTech University","correspondingAuthor":true,"prefix":"","firstName":"Jinbo","middleName":"","lastName":"Chen","suffix":""}],"badges":[],"createdAt":"2026-03-13 04:08:19","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-9109966/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-9109966/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":105564214,"identity":"41bea75d-ebc0-484b-8b97-eae0ab49ddbf","added_by":"auto","created_at":"2026-03-27 12:49:01","extension":"pdf","order_by":1,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1098007,"visible":true,"origin":"","legend":"","description":"","filename":"NearQuantitativeElectrocatalyticOxidationofHMFtoFDCAoveraNiMoCuHeterojunctionCatalys.pdf","url":"https://assets-eu.researchsquare.com/files/rs-9109966/v1_covered_16eade76-caf6-42e8-be8b-db685ed10cc0.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Near-Quantitative Electrocatalytic Oxidation of HMF to FDCA over a NiMoCu Heterojunction Catalyst","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"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":"catalysis-letters","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":"Learn more about [Catalysis Letters](https://link.springer.com/journal/10562)","snPcode":"10562","submissionUrl":"https://submission.springernature.com/new-submission/10562/3","title":"Catalysis Letters","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"5-Hydroxymethylfurfural (HMF), Electrocatalytic oxidation, NiMoCu ternary catalyst, Heterojunction, 2,5-Furandicarboxylic acid (FDCA)","lastPublishedDoi":"10.21203/rs.3.rs-9109966/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-9109966/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe conversion of 5-hydroxymethylfurfural (HMF) into the high-value-added product 2,5-furandicarboxylic acid (FDCA) requires efficient and stable electrocatalysts. A three-dimensional porous nanosheet -structured nickel-molybdenum-copper (NiMoCu) ternary catalyst was fabricated on nickel foam via a two-step electrodeposition strategy followed by alkaline heat treatment.Multiple heterointerfaces (MoO₃-CuO/NiOOH) were confirmed to form through the homogeneous integration of Ni, Mo, and Cu elements at the nanoscale, as evidenced by comprehensive characterization (XRD, Raman, TEM, and XPS). Simultaneously, the incorporation of Cu refined the grain size of MoO₃ to 8.2 nm and facilitated the in situ formation of amorphous NiOOH (containing Ni\u0026sup3;⁺ species). Moreover, the interfacial electron transfer effect optimized the charge transport pathway, thereby promoting efficient 5-hydroxymethylfurfural oxidation reaction (HMFOR).At1.47 V vs. RHE, the catalyst demonstrated record-breaking performance for HMF electric oxidation, achieving 99% HMF conversion, nearly 100% FDCA selectivity, 98% FDCA yield, and a Faradaic efficiency of 98%. Notably, it retained over 90% of its initial FDCA yield after four consecutive reaction cycles, corresponding to a minimal activity decay of less than 10%.The superior catalytic performance of the NiMoCu ternary catalyst originates from the effective synergy of its three metallic components. Specifically, Ni\u0026sup3;⁺ species serve as dynamicactive sites that efficiently drive the reaction, while Mo⁶⁺ species stabilize the Ni\u0026sup3;⁺ valence state and accelerate charge migration. Concurrently, the incorporation of Cu selectively suppresses the competing oxygen evolution reaction (OER contribution\u0026thinsp;\u0026lt;\u0026thinsp;2%). This work presents an effective strategy for designing highly efficient and stable catalysts dedicated to the electrocatalytic conversion of the key biomass platform compound, HMF.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e","manuscriptTitle":"Near-Quantitative Electrocatalytic Oxidation of HMF to FDCA over a NiMoCu Heterojunction Catalyst","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2026-03-24 11:19:36","doi":"10.21203/rs.3.rs-9109966/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2026-04-13T14:26:21+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-03-25T08:38:44+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"4941475938151205457733934162159766786","date":"2026-03-23T01:24:46+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"299987771980276082576539680954558459993","date":"2026-03-21T11:53:53+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2026-03-20T07:32:09+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"216730663799641721412642652662228549703","date":"2026-03-20T05:51:36+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2026-03-19T16:38:52+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2026-03-16T02:58:16+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2026-03-16T02:57:54+00:00","index":"","fulltext":""},{"type":"submitted","content":"Catalysis Letters","date":"2026-03-13T03:56:03+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"catalysis-letters","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":"Learn more about [Catalysis Letters](https://link.springer.com/journal/10562)","snPcode":"10562","submissionUrl":"https://submission.springernature.com/new-submission/10562/3","title":"Catalysis Letters","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"bc99fcb6-9a62-4e9a-a4b5-d26233495ac7","owner":[],"postedDate":"March 24th, 2026","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2026-05-01T15:09:23+00:00","versionOfRecord":[],"versionCreatedAt":"2026-03-24 11:19:36","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-9109966","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-9109966","identity":"rs-9109966","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}