Influence of Composition, Layer Thickness, and 2D Layer Coupling on Electrochemical Manufacturing

Influence of Composition, Layer Thickness, and 2D Layer Coupling on Electrochemical Manufacturing | 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 Article Influence of Composition, Layer Thickness, and 2D Layer Coupling on Electrochemical Manufacturing Bright Ngozichukwu, Eugenie Pranada, Ray Yoo, Niels Kubitza, Christina S. Birkel, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-8207533/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 24 Mar, 2026 Read the published version in npj 2D Materials and Applications → Version 1 posted 11 You are reading this latest preprint version Abstract The electrochemical reduction of CO 2 to hydrocarbon and oxygenate products has been demonstrated over metal-based catalysts such as Cu, but achieving high Faradaic efficiency (FE) has been a bottleneck. Here, we address this challenge by investigating how metal and C-N composition, layer thickness, and 2D heterostructure coupling influence CO 2 activation and product selectivity in emerging 2D materials. A suite of MXenes and related 2D heterostructures, Ti 2 NT x , Ti 4 N 3 T x , Ti 3 CNT x , V 2 NT x , V 2 CT x , MoS 2 /Ti 2 NTₓ and MoS 2 /Ti 4 N 3 T x were synthesized via a top-down etching method and evaluated for CO₂RR alongside the competing hydrogen evolution reaction (HER). Ti-based nitrides exhibited minimal CO 2 RR activity and strongly favored HER, with layer thickness and MoS₂ coupling showing little effect. Introducing both C and N into Ti 3 CNT x improved performance, yielding FE(CO) ~ 25–30% and FE(HCOOH) ~ 8–10%. A more substantial enhancement arose from changing the metal center: V-based MXenes shifted the reaction pathway toward CO 2 RR, with V 2 NT x achieving FE(CO) ~ 50% and FE(HCOOH) ~ 18%, outperforming V 2 CT x and suppressing HER at moderate current densities. V-based materials also displayed stability over hours with no loss in CO selectivity. Across all catalysts, CO and HCOOH were the only carbon-based products, indicating high intrinsic selectivity. Overall, this study elucidates the fundamental roles of composition, stoichiometry, and 2D structural coupling in governing CO 2 RR behavior, providing insights for designing next-generation catalysts for interfacial electrochemical reactions. Physical sciences/Chemistry Physical sciences/Energy science and technology Physical sciences/Materials science Electrochemical manufacturing 2D materials MXene CO2RR HER heterostructure materials sustainable catalysis carbon neutrality Full Text Additional Declarations No competing interests reported. Supplementary Files SupportingInformationFINAL.docx Cite Share Download PDF Status: Published Journal Publication published 24 Mar, 2026 Read the published version in npj 2D Materials and Applications → Version 1 posted Editorial decision: Revision requested 26 Dec, 2025 Reviews received at journal 22 Dec, 2025 Reviews received at journal 22 Dec, 2025 Reviews received at journal 14 Dec, 2025 Reviewers agreed at journal 13 Dec, 2025 Reviewers agreed at journal 11 Dec, 2025 Reviewers agreed at journal 11 Dec, 2025 Reviewers invited by journal 11 Dec, 2025 Editor assigned by journal 10 Dec, 2025 Submission checks completed at journal 06 Dec, 2025 First submitted to journal 25 Nov, 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. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. 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-8207533","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":560242495,"identity":"eb2aba84-9f35-4c24-8dfe-b64a77299b2f","order_by":0,"name":"Bright Ngozichukwu","email":"","orcid":"","institution":"Texas A\u0026M University","correspondingAuthor":false,"prefix":"","firstName":"Bright","middleName":"","lastName":"Ngozichukwu","suffix":""},{"id":560242496,"identity":"4b7485cb-f3ab-4174-835b-1b52c884699c","order_by":1,"name":"Eugenie Pranada","email":"","orcid":"","institution":"Texas A\u0026M University","correspondingAuthor":false,"prefix":"","firstName":"Eugenie","middleName":"","lastName":"Pranada","suffix":""},{"id":560242497,"identity":"78f742a9-a842-435f-a7b7-2afabf9eb548","order_by":2,"name":"Ray Yoo","email":"","orcid":"","institution":"Texas A\u0026M University","correspondingAuthor":false,"prefix":"","firstName":"Ray","middleName":"","lastName":"Yoo","suffix":""},{"id":560242498,"identity":"4d540608-5388-4945-a279-a487f3c5d2f4","order_by":3,"name":"Niels Kubitza","email":"","orcid":"","institution":"Technische Universitat Darmstadt","correspondingAuthor":false,"prefix":"","firstName":"Niels","middleName":"","lastName":"Kubitza","suffix":""},{"id":560242499,"identity":"a2c17490-ec5f-4bc0-8de1-b648d0ae5674","order_by":4,"name":"Christina S. 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Manufacturing","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":"npj-2d-materials-and-applications","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"npj2dmaterials","sideBox":"Learn more about [npj 2D Materials and Applications](http://www.nature.com/npj2dmaterials/)","snPcode":"41699","submissionUrl":"https://submission.springernature.com/new-submission/41699/3","title":"npj 2D Materials and Applications","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"NPJ","inReviewEnabled":true,"inReviewRevisionsEnabled":true},"keywords":"Electrochemical manufacturing, 2D materials, MXene, CO2RR, HER, heterostructure materials, sustainable catalysis, carbon neutrality","lastPublishedDoi":"10.21203/rs.3.rs-8207533/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-8207533/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe electrochemical reduction of CO\u003csub\u003e2\u003c/sub\u003e to hydrocarbon and oxygenate products has been demonstrated over metal-based catalysts such as Cu, but achieving high Faradaic efficiency (FE) has been a bottleneck. Here, we address this challenge by investigating how metal and C-N composition, layer thickness, and 2D heterostructure coupling influence CO\u003csub\u003e2\u003c/sub\u003e activation and product selectivity in emerging 2D materials. A suite of MXenes and related 2D heterostructures, Ti\u003csub\u003e2\u003c/sub\u003eNT\u003csub\u003ex\u003c/sub\u003e, Ti\u003csub\u003e4\u003c/sub\u003eN\u003csub\u003e3\u003c/sub\u003eT\u003csub\u003ex\u003c/sub\u003e, Ti\u003csub\u003e3\u003c/sub\u003eCNT\u003csub\u003ex\u003c/sub\u003e, V\u003csub\u003e2\u003c/sub\u003eNT\u003csub\u003ex\u003c/sub\u003e, V\u003csub\u003e2\u003c/sub\u003eCT\u003csub\u003ex\u003c/sub\u003e, MoS\u003csub\u003e2\u003c/sub\u003e/Ti\u003csub\u003e2\u003c/sub\u003eNTₓ and MoS\u003csub\u003e2\u003c/sub\u003e/Ti\u003csub\u003e4\u003c/sub\u003eN\u003csub\u003e3\u003c/sub\u003eT\u003csub\u003ex\u003c/sub\u003e were synthesized via a top-down etching method and evaluated for CO₂RR alongside the competing hydrogen evolution reaction (HER). Ti-based nitrides exhibited minimal CO\u003csub\u003e2\u003c/sub\u003eRR activity and strongly favored HER, with layer thickness and MoS₂ coupling showing little effect. Introducing both C and N into Ti\u003csub\u003e3\u003c/sub\u003eCNT\u003csub\u003ex\u003c/sub\u003e improved performance, yielding FE(CO)\u0026thinsp;~\u0026thinsp;25\u0026ndash;30% and FE(HCOOH)\u0026thinsp;~\u0026thinsp;8\u0026ndash;10%. A more substantial enhancement arose from changing the metal center: V-based MXenes shifted the reaction pathway toward CO\u003csub\u003e2\u003c/sub\u003eRR, with V\u003csub\u003e2\u003c/sub\u003eNT\u003csub\u003ex\u003c/sub\u003e achieving FE(CO)\u0026thinsp;~\u0026thinsp;50% and FE(HCOOH)\u0026thinsp;~\u0026thinsp;18%, outperforming V\u003csub\u003e2\u003c/sub\u003eCT\u003csub\u003ex\u003c/sub\u003e and suppressing HER at moderate current densities. V-based materials also displayed stability over hours with no loss in CO selectivity. Across all catalysts, CO and HCOOH were the only carbon-based products, indicating high intrinsic selectivity. Overall, this study elucidates the fundamental roles of composition, stoichiometry, and 2D structural coupling in governing CO\u003csub\u003e2\u003c/sub\u003eRR behavior, providing insights for designing next-generation catalysts for interfacial electrochemical reactions.\u003c/p\u003e","manuscriptTitle":"Influence of Composition, Layer Thickness, and 2D Layer Coupling on Electrochemical Manufacturing","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-12-16 12:57:39","doi":"10.21203/rs.3.rs-8207533/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-12-26T11:14:36+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-12-23T01:47:12+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-12-22T18:00:38+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-12-15T02:59:42+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"25945466770489150740059109893668853002","date":"2025-12-14T00:08:57+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"121340257800980744425944844313530028349","date":"2025-12-12T03:41:31+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"99997197662933635243091727283079701926","date":"2025-12-11T11:19:47+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-12-11T08:58:48+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-12-10T17:03:43+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-12-06T05:41:58+00:00","index":"","fulltext":""},{"type":"submitted","content":"npj 2D Materials and Applications","date":"2025-11-26T01:46:18+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"npj-2d-materials-and-applications","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"npj2dmaterials","sideBox":"Learn more about [npj 2D Materials and Applications](http://www.nature.com/npj2dmaterials/)","snPcode":"41699","submissionUrl":"https://submission.springernature.com/new-submission/41699/3","title":"npj 2D Materials and Applications","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"NPJ","inReviewEnabled":true,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"91266b4b-1ff6-46fc-bd15-4a3915270ddb","owner":[],"postedDate":"December 16th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[{"id":59634461,"name":"Physical sciences/Chemistry"},{"id":59634462,"name":"Physical sciences/Energy science and technology"},{"id":59634463,"name":"Physical sciences/Materials science"}],"tags":[],"updatedAt":"2026-03-30T16:32:20+00:00","versionOfRecord":{"articleIdentity":"rs-8207533","link":"https://doi.org/10.1038/s41699-026-00685-2","journal":{"identity":"npj-2d-materials-and-applications","isVorOnly":false,"title":"npj 2D Materials and Applications"},"publishedOn":"2026-03-24 16:10:08","publishedOnDateReadable":"March 24th, 2026"},"versionCreatedAt":"2025-12-16 12:57:39","video":"","vorDoi":"10.1038/s41699-026-00685-2","vorDoiUrl":"https://doi.org/10.1038/s41699-026-00685-2","workflowStages":[]},"version":"v1","identity":"rs-8207533","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-8207533","identity":"rs-8207533","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}