Tailoring Dielectric Properties and Crystallinity in Poly(Vinylidene Fluoride-Co-Hexafluoropropylene) Nanocomposites via Iron (III) Chloride Hexahydrate Incorporation

Tailoring Dielectric Properties and Crystallinity in Poly(Vinylidene Fluoride-Co-Hexafluoropropylene) Nanocomposites via Iron (III) Chloride Hexahydrate Incorporation | 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 Tailoring Dielectric Properties and Crystallinity in Poly(Vinylidene Fluoride-Co-Hexafluoropropylene) Nanocomposites via Iron (III) Chloride Hexahydrate Incorporation Jureeporn Yuennan, Nantakan Muensit, Nikruesong Tohluebaji, Wichain Chailad, and 4 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6141766/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 22 May, 2025 Read the published version in Scientific Reports → Version 1 posted 8 You are reading this latest preprint version Abstract This study investigates the impact of iron (III) chloride hexahydrate (FeCl 3 ·6H 2 O) incorporation on the structural, thermal, and dielectric properties of poly(vinylidene fluoride-co-hexafluoropropylene) [P(VDF-HFP)] nanocomposites, which were prepared using a solution casting method with varying filler concentrations (1–4 wt%). Scanning electron microscopy (SEM) revealed a systematic increase in porosity—from 0.72% in pure P(VDF-HFP) to 27.5% at 4 wt% FeCl 3 ·6H 2 O—along with increased pore size and surface heterogeneity. Atomic force microscopy (AFM) confirmed enhanced surface roughness correlating with increased filler content. Fourier-transform infrared (FTIR) spectroscopy demonstrated a significant α-to-β phase transformation, indicating the formation of the polar β-phase with increasing FeCl 3 ·6H 2 O content. X-ray diffraction (XRD) analysis corroborated these findings, revealing a notable increase in crystallinity and β-phase content, with 4 wt% FeCl 3 ·6H 2 O achieving the highest β-phase fraction (88.99%). Thermogravimetric analysis (TGA) confirmed thermal stability up to approximately 500°C, with a gradual shift in degradation onset attributed to FeCl 3 ·6H 2 O interactions. Dielectric measurements at 10 Hz showed a remarkable enhancement in dielectric constant—from 5.62 in pure P(VDF-HFP) to 19.16 at 4 wt% FeCl 3 ·6H 2 O—while maintaining a low dielectric loss (< 0.30). These improvements are attributed to the synergistic effects of FeCl 3 ·6H 2 O on porosity, phase transformation, crystallinity, thermal stability, and dielectric properties. The superior performance of these nanocomposites makes them promising candidates for flexible electronics, energy storage systems, and advanced sensors. Physical sciences/Materials science Physical sciences/Materials science/Structural materials P(VDF-HFP) composites FeCl3·6H2O doping Hydrogen bonding interactions Thermal stability Dielectric properties Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Full Text Additional Declarations No competing interests reported. Cite Share Download PDF Status: Published Journal Publication published 22 May, 2025 Read the published version in Scientific Reports → Version 1 posted Editorial decision: Accepted 16 May, 2025 Reviews received at journal 30 Apr, 2025 Reviewers agreed at journal 09 Apr, 2025 Reviews received at journal 08 Apr, 2025 Reviewers agreed at journal 08 Apr, 2025 Reviewers invited by journal 07 Apr, 2025 Submission checks completed at journal 05 Apr, 2025 First submitted to journal 01 Apr, 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. 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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-6141766","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":440714976,"identity":"3215d92e-f65f-4868-bc5c-890f75b498b4","order_by":0,"name":"Jureeporn Yuennan","email":"","orcid":"","institution":"Nakhon Si Thammarat Rajabhat University","correspondingAuthor":false,"prefix":"","firstName":"Jureeporn","middleName":"","lastName":"Yuennan","suffix":""},{"id":440714978,"identity":"322f53f5-060c-49f7-b5d6-b40708ae30d1","order_by":1,"name":"Nantakan Muensit","email":"","orcid":"","institution":"Prince of Songkla 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01:38:12","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6141766/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6141766/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1038/s41598-025-02895-y","type":"published","date":"2025-05-22T15:57:10+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":80273938,"identity":"f50728a1-9a52-4959-9e9d-3d1f807df53e","added_by":"auto","created_at":"2025-04-10 04:25:26","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":170070,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic representation of the preparation process for FeCl₃·6H₂O/P(VDF-HFP) nanocomposite films using the solution casting method.\u003c/p\u003e","description":"","filename":"image1.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/740508e7a08b7b0bb1c1c9e9.png"},{"id":80273937,"identity":"441e8378-d6cc-4fdd-97fc-f7179b859c90","added_by":"auto","created_at":"2025-04-10 04:25:26","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":1057444,"visible":true,"origin":"","legend":"\u003cp\u003e(a) SEM images, (b) porosity and (c) pore size analyses by ImageJ of pure P(VDF-HFP) and FeCl₃·6H₂O/P(VDF-HFP) nanocomposites.\u003c/p\u003e","description":"","filename":"image2.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/829fba07da8576ebba1eb4be.png"},{"id":80273417,"identity":"37b8a121-ca33-45e0-a226-19d3fdbf2c25","added_by":"auto","created_at":"2025-04-10 04:17:26","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":198982,"visible":true,"origin":"","legend":"\u003cp\u003ePorosity and pore size values analyzed by ImageJ of pure P(VDF-HFP) and FeCl₃·6H₂O/P(VDF-HFP) nanocomposites.\u003c/p\u003e","description":"","filename":"image3.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/41bb819ca4dc6365a206f109.png"},{"id":80273412,"identity":"cf59f734-27be-4b1e-bc2a-a531d6ff78fb","added_by":"auto","created_at":"2025-04-10 04:17:26","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":1121101,"visible":true,"origin":"","legend":"\u003cp\u003eAFM images of pure P(VDF-HFP) and FeCl₃·6H₂O/P(VDF-HFP) nanocomposites.\u003c/p\u003e","description":"","filename":"image4.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/b455b92f813eeb6ab85f0ecd.png"},{"id":80274186,"identity":"0804db14-8187-4605-b11f-75433f212848","added_by":"auto","created_at":"2025-04-10 04:33:26","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":287786,"visible":true,"origin":"","legend":"\u003cp\u003eATR-FTIR spectra of pure P(VDF-HFP) and FeCl\u003csub\u003e3\u003c/sub\u003e·6H\u003csub\u003e2\u003c/sub\u003eO/P(VDF-HFP) nanocomposites with different filler concentrations (1–4 wt%). Peaks corresponding to α-, β-, and γ-phases are marked. Increasing FeCl\u003csub\u003e3\u003c/sub\u003e·6H\u003csub\u003e2\u003c/sub\u003eO content enhances the β-phase (840 cm⁻¹) while reducing α-phase signals, indicating phase transformation. The inset highlights these spectral changes for improved clarity.\u003c/p\u003e","description":"","filename":"image5.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/fcef36cfa5f2d50210aedbf7.png"},{"id":80273941,"identity":"187f9a6b-b97e-42b2-ae8c-e4dbaccd99ee","added_by":"auto","created_at":"2025-04-10 04:25:26","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":354195,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic representation of hydrogen bonding interaction for (a) pure P(VDF-HFP) and (b) FeCl₃·6H₂O/P(VDF-HFP) nanocomposites.\u003c/p\u003e","description":"","filename":"image6.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/d92a3c888f7a9a38fda34b9b.png"},{"id":80273942,"identity":"6aa55ccc-7936-4e35-ad02-43f2bac33aff","added_by":"auto","created_at":"2025-04-10 04:25:26","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":281126,"visible":true,"origin":"","legend":"\u003cp\u003eXRD patterns of pure P(VDF-HFP) and FeCl\u003csub\u003e3\u003c/sub\u003e·6H\u003csub\u003e2\u003c/sub\u003eO /P(VDF-HFP) nanocomposites with varying FeCl\u003csub\u003e3\u003c/sub\u003e·6H\u003csub\u003e2\u003c/sub\u003eO concentrations (1–4 wt%). Characteristic diffraction peaks corresponding to the α-phase (2θ ≈ 18.6°, 19.7°) and β-phase (2θ ≈ 20.6°) are indicated. The inset provides a magnified view of the 2θ range from 15° to 25°, highlighting the subtle increase in the β-phase peak intensity at 20.6° with increasing FeCl\u003csub\u003e3\u003c/sub\u003e·6H\u003csub\u003e2\u003c/sub\u003eO content.\u003c/p\u003e","description":"","filename":"image7.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/210a74f58d03db4e8dfbc287.png"},{"id":80273944,"identity":"82c18e84-ec86-4332-9a7f-dcdf8ee89df7","added_by":"auto","created_at":"2025-04-10 04:25:26","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":145205,"visible":true,"origin":"","legend":"\u003cp\u003eTGA and DTG (inset) curves of pure P(VDF-HFP) and FeCl₃·6H₂O/P(VDF-HFP) nanocomposites.\u003c/p\u003e","description":"","filename":"image8.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/5f3bd730da67419032975217.png"},{"id":80273439,"identity":"98fed2e4-d9f6-4394-ab43-e04a5338d2b8","added_by":"auto","created_at":"2025-04-10 04:17:27","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":411405,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Dielectric constant, (b) dielectric loss and (c) conductivity of pure P(VDF-HFP) and FeCl₃·6H₂O/P(VDF-HFP) nanocomposites.\u003c/p\u003e","description":"","filename":"image9.png","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1/ce4a8d4fd65c95e4e16d3807.png"},{"id":83460066,"identity":"f1d080ed-c9e7-4bf7-89df-6338006817b7","added_by":"auto","created_at":"2025-05-26 16:09:47","extension":"pdf","order_by":1,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":4569210,"visible":true,"origin":"","legend":"","description":"","filename":"manuscriptonlyTEXTTableRevised1APRILClean.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6141766/v1_covered_8c67afe5-7c7e-4ece-987b-090c74198753.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Tailoring Dielectric Properties and Crystallinity in Poly(Vinylidene Fluoride-Co-Hexafluoropropylene) Nanocomposites via Iron (III) Chloride Hexahydrate Incorporation","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":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true},"keywords":"P(VDF-HFP) composites, FeCl3·6H2O doping, Hydrogen bonding interactions, Thermal stability, Dielectric properties","lastPublishedDoi":"10.21203/rs.3.rs-6141766/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6141766/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThis study investigates the impact of iron (III) chloride hexahydrate (FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO) incorporation on the structural, thermal, and dielectric properties of poly(vinylidene fluoride-co-hexafluoropropylene) [P(VDF-HFP)] nanocomposites, which were prepared using a solution casting method with varying filler concentrations (1\u0026ndash;4 wt%). Scanning electron microscopy (SEM) revealed a systematic increase in porosity\u0026mdash;from 0.72% in pure P(VDF-HFP) to 27.5% at 4 wt% FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO\u0026mdash;along with increased pore size and surface heterogeneity. Atomic force microscopy (AFM) confirmed enhanced surface roughness correlating with increased filler content. Fourier-transform infrared (FTIR) spectroscopy demonstrated a significant α-to-β phase transformation, indicating the formation of the polar β-phase with increasing FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO content. X-ray diffraction (XRD) analysis corroborated these findings, revealing a notable increase in crystallinity and β-phase content, with 4 wt% FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO achieving the highest β-phase fraction (88.99%). Thermogravimetric analysis (TGA) confirmed thermal stability up to approximately 500\u0026deg;C, with a gradual shift in degradation onset attributed to FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO interactions. Dielectric measurements at 10 Hz showed a remarkable enhancement in dielectric constant\u0026mdash;from 5.62 in pure P(VDF-HFP) to 19.16 at 4 wt% FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO\u0026mdash;while maintaining a low dielectric loss (\u0026lt;\u0026thinsp;0.30). These improvements are attributed to the synergistic effects of FeCl\u003csub\u003e3\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO on porosity, phase transformation, crystallinity, thermal stability, and dielectric properties. The superior performance of these nanocomposites makes them promising candidates for flexible electronics, energy storage systems, and advanced sensors.\u003c/p\u003e","manuscriptTitle":"Tailoring Dielectric Properties and Crystallinity in Poly(Vinylidene Fluoride-Co-Hexafluoropropylene) Nanocomposites via Iron (III) Chloride Hexahydrate Incorporation","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-04-10 04:17:21","doi":"10.21203/rs.3.rs-6141766/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Accepted","date":"2025-05-16T06:48:22+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-04-30T16:44:55+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"330719279895765255789302560611837384276","date":"2025-04-09T14:59:43+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-04-09T03:59:36+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"294774802216781343320262024616501382812","date":"2025-04-09T01:38:02+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-04-07T14:28:41+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-04-05T15:25:57+00:00","index":"","fulltext":""},{"type":"submitted","content":"Scientific Reports","date":"2025-04-01T08:49:22+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"scientific-reports","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"scirep","sideBox":"Learn more about [Scientific Reports](http://www.nature.com/srep/)","snPcode":"","submissionUrl":"","title":"Scientific Reports","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Scientific Reports","inReviewEnabled":true,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"cff8b856-e71d-4464-afbf-8fb45e0b8674","owner":[],"postedDate":"April 10th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[{"id":46923221,"name":"Physical sciences/Materials science"},{"id":46923222,"name":"Physical sciences/Materials science/Structural materials"}],"tags":[],"updatedAt":"2025-05-26T16:03:02+00:00","versionOfRecord":{"articleIdentity":"rs-6141766","link":"https://doi.org/10.1038/s41598-025-02895-y","journal":{"identity":"scientific-reports","isVorOnly":false,"title":"Scientific Reports"},"publishedOn":"2025-05-22 15:57:10","publishedOnDateReadable":"May 22nd, 2025"},"versionCreatedAt":"2025-04-10 04:17:21","video":"","vorDoi":"10.1038/s41598-025-02895-y","vorDoiUrl":"https://doi.org/10.1038/s41598-025-02895-y","workflowStages":[]},"version":"v1","identity":"rs-6141766","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6141766","identity":"rs-6141766","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}