Polymer Nanoparticles: Preparation Methods and Structural Characterization

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This preprint studied how alkaline hydrolysis conditions affect the synthesis and structure of silk fibroin micro- and nanoparticles, using an alkaline modulus of 1:6 at 180°C for 120–150 minutes. Particle morphology, size distribution, and crystallinity were assessed with dynamic light scattering (DLS), atomic force microscopy (AFM), and X-ray diffraction (XRD), with reported findings that the products were white, odorless, ultra-spherical fine powders that were almost insoluble in water. At 120 minutes the size distribution was dominated by ~16.54 nm particles (70.6%) with some larger fraction (~240 µm, 29.4%), while at 150 minutes it shifted largely to ~82.07 nm (96.5%) with only a small ~100 µm fraction (3.5%); AFM showed needle-like to spherical morphology changes with longer hydrolysis and XRD indicated increased crystallinity, though excessive acid reduced ordering. The work is limited by being a non-peer-reviewed preprint and provides no biomedical testing. The paper does not explicitly discuss endometriosis or adenomyosis; it was included in the corpus via a keyword match in the upstream search index.

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Abstract

Abstract The synthesis of functional nanoscale particles and their composites is of increasing interest for biomedical and materials science applications. Silk fibroin, a biocompatible and surface-active polymer, offers tunable properties for such purposes. Silk fibroin micro- and nanoparticles were synthesized via hydrolysis at an alkaline modulus of 1:6, temperatures of 180°C, and durations of 120–150 min. Particle morphology, size distribution, and crystallinity were characterized by dynamic light scattering (DLS), atomic force microscopy (AFM), and X-ray diffraction (XRD). The particles obtained were white, odorless, ultra-spherical fine powders, almost insoluble in water, with a bulk density of 650–750 kg/m³. At 120 min, size distribution was 70.6% at 16.54 nm and 29.4% at 240 µm. At 150 min, it shifted to 96.5% at 82.07 nm and 3.5% at 100 µm. AFM revealed morphological changes from needle-like to spherical shapes with prolonged hydrolysis, while XRD indicated increased crystallinity with reaction time, though excessive acid concentration reduced order. Hydrolysis time strongly affects silk fibroin nanoparticle size distribution and morphology. The optimized conditions-180°C for 150 min at 1:6 alkaline modulus-yield predominantly spherical nanoparticles with controlled crystallinity. These findings provide a basis for tailoring fibroin-based materials for targeted applications in nanotechnology and biomedicine.
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Polymer Nanoparticles: Preparation Methods and Structural Characterization | 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 Polymer Nanoparticles: Preparation Methods and Structural Characterization Jakhongir Khakkulov This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7913532/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 The synthesis of functional nanoscale particles and their composites is of increasing interest for biomedical and materials science applications. Silk fibroin, a biocompatible and surface-active polymer, offers tunable properties for such purposes. Silk fibroin micro- and nanoparticles were synthesized via hydrolysis at an alkaline modulus of 1:6, temperatures of 180°C, and durations of 120–150 min. Particle morphology, size distribution, and crystallinity were characterized by dynamic light scattering (DLS), atomic force microscopy (AFM), and X-ray diffraction (XRD). The particles obtained were white, odorless, ultra-spherical fine powders, almost insoluble in water, with a bulk density of 650–750 kg/m³. At 120 min, size distribution was 70.6% at 16.54 nm and 29.4% at 240 µm. At 150 min, it shifted to 96.5% at 82.07 nm and 3.5% at 100 µm. AFM revealed morphological changes from needle-like to spherical shapes with prolonged hydrolysis, while XRD indicated increased crystallinity with reaction time, though excessive acid concentration reduced order. Hydrolysis time strongly affects silk fibroin nanoparticle size distribution and morphology. The optimized conditions-180°C for 150 min at 1:6 alkaline modulus-yield predominantly spherical nanoparticles with controlled crystallinity. These findings provide a basis for tailoring fibroin-based materials for targeted applications in nanotechnology and biomedicine. Polymer Science silk fibroin nanoparticles hydrolysis dynamic light scattering (DLS) Atomic force microscopy (AFM) X-ray diffraction (XRD) particle size distribution bio compatible materials Full Text Additional Declarations The authors declare no competing interests. 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. 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Characterization\u003c/strong\u003e\u003c/p\u003e","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":true,"highlight":"","institution":"National University of Uzbekistan","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":"silk fibroin, nanoparticles, 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Silk fibroin, a biocompatible and surface-active polymer, offers tunable properties for such purposes. Silk fibroin micro- and nanoparticles were synthesized via hydrolysis at an alkaline modulus of 1:6, temperatures of 180\u0026deg;C, and durations of 120\u0026ndash;150 min. Particle morphology, size distribution, and crystallinity were characterized by dynamic light scattering (DLS), atomic force microscopy (AFM), and X-ray diffraction (XRD). The particles obtained were white, odorless, ultra-spherical fine powders, almost insoluble in water, with a bulk density of 650\u0026ndash;750 kg/m\u0026sup3;. At 120 min, size distribution was 70.6% at 16.54 nm and 29.4% at 240 \u0026micro;m. At 150 min, it shifted to 96.5% at 82.07 nm and 3.5% at 100 \u0026micro;m. AFM revealed morphological changes from needle-like to spherical shapes with prolonged hydrolysis, while XRD indicated increased crystallinity with reaction time, though excessive acid concentration reduced order. Hydrolysis time strongly affects silk fibroin nanoparticle size distribution and morphology. The optimized conditions-180\u0026deg;C for 150 min at 1:6 alkaline modulus-yield predominantly spherical nanoparticles with controlled crystallinity. These findings provide a basis for tailoring fibroin-based materials for targeted applications in nanotechnology and biomedicine.\u003c/p\u003e","manuscriptTitle":"Polymer Nanoparticles: Preparation Methods and Structural Characterization","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-10-22 07:15:53","doi":"10.21203/rs.3.rs-7913532/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","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}}],"origin":"","ownerIdentity":"0412c5e8-4e18-4031-99ba-b5382b3133ad","owner":[],"postedDate":"October 22nd, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[{"id":56681280,"name":"Polymer Science"}],"tags":[],"updatedAt":"2025-10-22T07:15:53+00:00","versionOfRecord":[],"versionCreatedAt":"2025-10-22 07:15:53","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-7913532","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7913532","identity":"rs-7913532","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}

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