Effect of Ammonium Hexafluorophosphate (NH₄PF₆) and Mixed Ammonium Hexafluorophosphate/tetrabutylammonium Hexafluorophosphate (NH₄PF₆/NBu₄PF₆) on the Morphological and Structural Evolution of TiO₂ Nanocatalyst

Effect of Ammonium Hexafluorophosphate (NH₄PF₆) and Mixed Ammonium Hexafluorophosphate/tetrabutylammonium Hexafluorophosphate (NH₄PF₆/NBu₄PF₆) on the Morphological and Structural Evolution of TiO₂ Nanocatalyst | 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 Effect of Ammonium Hexafluorophosphate (NH₄PF₆) and Mixed Ammonium Hexafluorophosphate/tetrabutylammonium Hexafluorophosphate (NH₄PF₆/NBu₄PF₆) on the Morphological and Structural Evolution of TiO₂ Nanocatalyst Faridah Abu Bakar, Noor Kamalia Abd Hamed, Mohd Khairul Ahmad This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7617651/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 Titanium dioxide (TiO₂) nanocatalyst has received significant attention due to its superior photo-induced electron transfer properties, particularly in the metastable anatase phase, which underpins its application in advanced oxidation processes (AOPs). However, anatase TiO₂ crystals are predominantly dominated by the thermodynamically stable {101} facet, representing over 94% of the surface, whereas the highly reactive {001} facet diminishes rapidly under equilibrium growth, limiting photocatalytic efficiency. To address this limitation, this study evaluates the morphological and structural evolution of TiO₂ nanocatalysts synthesized via thermal decomposition of peroxotitanic acid in the presence of ammonium hexafluorophosphate (NH₄PF₆) and a mixed ammonium/tetrabutylammonium hexafluorophosphate system (NH₄PF₆/NBu₄PF₆). Field emission scanning electron microscopy (FE-SEM) revealed that fluorine incorporation effectively promoted anisotropic growth, producing rice grain-like nanocrystals with improved dispersion. X-ray diffraction (XRD) analysis demonstrated enhanced anatase phase stability in the co-doped NH₄PF₆/NBu₄PF₆–TiO₂ sample (85.81%) compared with NH₄PF₆–TiO₂ (59.68%) and undoped Peroxo–TiO₂ (57.12%), while Raman spectroscopy confirmed increased crystallinity and coherent lattice vibrations. Surface facet analysis indicated that {001} facet exposure was slightly higher in NH₄PF₆–TiO₂ (6.54%) than in the co-doped system (5.65%), reflecting the effect of dual-cation fluorination on crystal growth. Overall, the dual-cation strategy effectively suppresses anatase-to-rutile transformation, stabilizes the anatase phase, and regulates facet development, yielding TiO₂ nanocatalysts with improved structural integrity, controlled morphology, and tailored high-energy surfaces. These engineered materials present considerable potential for enhanced photocatalytic performance in sustainable energy conversion and environmental remediation applications. Full Text Additional Declarations No competing interests reported. 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. 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-7617651","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":515120972,"identity":"ac68455f-ceb3-4033-8663-fe25db65f146","order_by":0,"name":"Faridah Abu Bakar","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA4klEQVRIiWNgGAWjYBAC9gYGhgM8DAcS+BkY2EACjA2EtPAcgGqRbGAmQQsDSIvBAaK1sJ99eOBNzZ084xv5xx7dYLCR3XCAO00CrxaedIODc449Kza7kcxunMOQZrzhAO82vFrsGdIYDvOwHU7cdiOZTTqH4XAiQS08/M+AWv4dTtw8A6zlPxFaJIC28LYBDZcAazlAjJZnDAfn9h0uljjz2Ew6xyDZeOZh3s0W+B2WxvzhzbfDefztic+kcyrsZPuO9268gU8LGjAAYmYGFrwOwwqYP5CsZRSMglEwCoYzAACTO0+83+gkhAAAAABJRU5ErkJggg==","orcid":"","institution":"Universiti Tun Hussein Onn Malaysia","correspondingAuthor":true,"prefix":"","firstName":"Faridah","middleName":"Abu","lastName":"Bakar","suffix":""},{"id":515120973,"identity":"83b22be2-3da2-4ae8-b757-973a5dc7960b","order_by":1,"name":"Noor Kamalia Abd Hamed","email":"","orcid":"","institution":"Universiti Tun Hussein Onn Malaysia","correspondingAuthor":false,"prefix":"","firstName":"Noor","middleName":"Kamalia Abd","lastName":"Hamed","suffix":""},{"id":515120974,"identity":"72b7eb2b-8447-4e90-97ee-177f3030242f","order_by":2,"name":"Mohd Khairul Ahmad","email":"","orcid":"","institution":"Universiti Tun Hussein Onn Malaysia","correspondingAuthor":false,"prefix":"","firstName":"Mohd","middleName":"Khairul","lastName":"Ahmad","suffix":""}],"badges":[],"createdAt":"2025-09-15 07:53:13","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-7617651/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-7617651/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":91873774,"identity":"397e59bf-d581-437e-a581-1dbc4f564eb6","added_by":"auto","created_at":"2025-09-22 14:10:28","extension":"pdf","order_by":1,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1043971,"visible":true,"origin":"","legend":"","description":"","filename":"ManuscriptMDRGrant.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7617651/v1_covered_53a82e47-a161-43ab-a96d-780d01911dfa.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"\u003cp\u003eEffect of Ammonium Hexafluorophosphate (NH₄PF₆) and Mixed Ammonium Hexafluorophosphate/tetrabutylammonium Hexafluorophosphate (NH₄PF₆/NBu₄PF₆) on the Morphological and Structural Evolution of TiO₂ Nanocatalyst\u003c/p\u003e","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":true,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":true,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","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":"","lastPublishedDoi":"10.21203/rs.3.rs-7617651/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7617651/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eTitanium dioxide (TiO₂) nanocatalyst has received significant attention due to its superior photo-induced electron transfer properties, particularly in the metastable anatase phase, which underpins its application in advanced oxidation processes (AOPs). However, anatase TiO₂ crystals are predominantly dominated by the thermodynamically stable {101} facet, representing over 94% of the surface, whereas the highly reactive {001} facet diminishes rapidly under equilibrium growth, limiting photocatalytic efficiency. To address this limitation, this study evaluates the morphological and structural evolution of TiO₂ nanocatalysts synthesized via thermal decomposition of peroxotitanic acid in the presence of ammonium hexafluorophosphate (NH₄PF₆) and a mixed ammonium/tetrabutylammonium hexafluorophosphate system (NH₄PF₆/NBu₄PF₆). Field emission scanning electron microscopy (FE-SEM) revealed that fluorine incorporation effectively promoted anisotropic growth, producing rice grain-like nanocrystals with improved dispersion. X-ray diffraction (XRD) analysis demonstrated enhanced anatase phase stability in the co-doped NH₄PF₆/NBu₄PF₆\u0026ndash;TiO₂ sample (85.81%) compared with NH₄PF₆\u0026ndash;TiO₂ (59.68%) and undoped Peroxo\u0026ndash;TiO₂ (57.12%), while Raman spectroscopy confirmed increased crystallinity and coherent lattice vibrations. Surface facet analysis indicated that {001} facet exposure was slightly higher in NH₄PF₆\u0026ndash;TiO₂ (6.54%) than in the co-doped system (5.65%), reflecting the effect of dual-cation fluorination on crystal growth. Overall, the dual-cation strategy effectively suppresses anatase-to-rutile transformation, stabilizes the anatase phase, and regulates facet development, yielding TiO₂ nanocatalysts with improved structural integrity, controlled morphology, and tailored high-energy surfaces. 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