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Structure design and determination of curing kinetics for epoxy based functional hybrid materials

dc.contributor.advisorJovičić, Mirjana
dc.contributor.otherBera, Oskar
dc.contributor.otherPavličević, Jelena
dc.contributor.otherJovičić, Mirjana
dc.contributor.otherBaloš, Sebastian
dc.creatorTeofilović, Vesna
dc.date.accessioned2019-10-10T14:25:11Z
dc.date.available2019-10-10T14:25:11Z
dc.date.available2020-07-03T13:56:52Z
dc.date.issued2019-09-30
dc.identifier.urihttps://www.cris.uns.ac.rs/DownloadFileServlet/Disertacija156456192673042.pdf?controlNumber=(BISIS)111006&fileName=156456192673042.pdf&id=13278&source=NaRDuS&language=srsr
dc.identifier.urihttps://nardus.mpn.gov.rs/handle/123456789/11401
dc.identifier.urihttps://www.cris.uns.ac.rs/record.jsf?recordId=111006&source=NaRDuS&language=srsr
dc.identifier.urihttps://www.cris.uns.ac.rs/DownloadFileServlet/IzvestajKomisije156456194052160.pdf?controlNumber=(BISIS)111006&fileName=156456194052160.pdf&id=13279&source=NaRDuS&language=srsr
dc.description.abstractU ovoj doktorskoj disertaciji je ispitan uticaj montmorilonita i termoplastičnih segmentiranih poliuretana na kinetiku reakcija umrežavanja, strukturu i svojstva funkcionalnih hibridnih materijala na osnovu epoksidnih smola. Pripremljene su dve serije uzoraka hibridnih materijala: prva na osnovu epoksidne smole sa različitim sadržajem organski modifikovanog montmorilonita (0, 1, 3, 5 i 10 mas.%) umrežene sa umreživačem Jeffamine D-230; druga serija je sintetisana na osnovu epoksidne smole, sa različitim sadržajem (10, 15 i 20 mas.%) termoplastičnog poliuretanskog elastomera sa različitim sadržajem tvrdih segmenata (20, 25 i 30 mas.%) sintetisanih na osnovu alifatičnog polikarbonatnog diola i heksametilendiizocijanata i produživača lanca butandiola, kao i katalizatora dibutiltin dilaurata; kao i bez dodatog elastomera umrežene sa diaminom Jeffamine D-2000. Umrežavanje reaktivnih sistema sa projektovanim sirovinskim sastavom je praćeno diferencijalnom skenirajućom kalorimetrijom (DSC). Modeli izokonverzije primenjeni su da se ustanovi da li dodatak punila utiče na reakciju umrežavanja hibridnih materijala. Sintetisani materijali su analizirani dinamičkomehaničkom analizom (DMA), mikroskopijom atomskih sila (AFM), kao i TG-DSC i TG-MS metodama i određena su mehanička svojstva (zatezna čvrstoća, prekidno izduženje i tvrdoća po Šoru A). Epoksidni materijal sa 10 mas.% organski modifikovanog montmorilonita ima značajno niže vrednosti energija aktivacije za definisane stepene reagovanja, čime je potvrđen katalitički efekat gline sa slojevitom strukturom kada je prisutna u reakcionoj smeši u dovoljnoj količini. Uticaj otežane difuzije pri kraju reakcije je izraženiji u prisustvu montmorilonita, čime je pokazano da njegovo prisustvo utiče na ceo mehanizam umrežavanja. Utvrđeno je da na vrednosti G', pored udela montmorilonita, utiče i stepen dispergovanja čestica unutar polimerne matrice. Zaključeno je da dodatak punila do 3 mas. % utiče povoljno na ispitana mehanička svojstva, dok pri sadržaju od 5 i 10 mas. % dolazi do aglomeracije čestica punila, što negativno utiče na ispitana svojstva, osim tvrdoće, koja se povećava linearno sa dodatkom punila montmorilonita. Na osnovu rezultata TG analize zaključeno je da je sa porastom udela montmorilonita u epoksidnoj matrici termička stabilnost uzoraka ispitivanih u atmosferi vazduha neznatno poboljšana, dok u inertnoj atmosferi nema uticaja na termičku stabilnost, niti na mehanizam raspada hibridnih materijala na osnovu epoksidnih smola sa različitim udelima montmorilonita. Kod sistema kod kojih je dodavan termoplastični poliuretanski elastomer, zaključeno je da pri većem sadržaju segmentiranih poliuretana u epoksidnoj matrici (10 i 15 mas.%) proces umrežavanja započinje na nižim temperaturama i maksimalna brzina se ostvaruje na nižim temperaturama, a najveća vrednost promena ukupne entalpije reakcije umrežavanja je određena za hibridni materijal sa poliuretanom koji u svojoj strukturi ima 30 mas.% tvrdih segmenata. Zatezna čvrstoća hibridnih materijala raste sa porastom udela tvrdih segmenata u strukturi poliuretana, kao i sa porastom masenog udela poliuretanskog elastomera u epoksidnoj matrici. Dodatkom termoplastičnih segmentiranih poliuretana značajno je povećano prekidno izduženje epoksidnih smola. Sa porastom udela tvrdih segmenata kod poliuretana dodatih u istom masenom procentu u epoksidnu matricu, tvrdoća raste. Ustanovljeno je da na konačna svojstva hibridnih materijala utiče izbor polaznih komponenti, način umešavanja punila u matricu i uslovi pri kojima se vrši umrežavanje. Zaključeno je da je dobro poznavanje kinetičkih parametara reakcije umrežavanja važno za pravilan odabir optimalnih uslova za proizvodnju i preradu hibridnih materijala u industrijskim uslovima.sr
dc.description.abstractIn this thesis the influence of clay fillers and thermoplastic segmented polyurethanes on the curing kinetics, structure and properties of functional hybrid materials based on epoxy resins was assessed. Two sets of hybrid material samples were prepared. First type of samples was based on epoxy resin with a different content of organically modified montmorillonite (0, 1, 3, 5 and 10 wt. %) and crosslinking with hardener Jeffamine D-230. Second type of samples was based on epoxy resin, having different content (10, 15 and 20 wt. %) of thermoplastic segmented polyurethane with different content of hard segments (20, 25 and 30 wt. %) based on aliphatic polycarbonate macrodiols and hexamethylene diisocyanate, with chain extender 1,4-butanediol and the catalyst, dibutyltin dilaurate, and also a sample without added elastomeric polyurethane and crosslinking with hardener Jeffamine D- 2000. The curing of the hybrid materials based on epoxy resins systems were investigated by non-isothermal differential scanning calorimetry (DSC). The kinetic study by isoconversion models has been carried out using data from DSC. The synthesized materials were analyzed by dynamicmechanical analysis (DMA), atomic force microscopy (AFM) as well as TG-DSC and TG-MS methods and mechanical properties (tensile strength, elongation and hardness at Shore A) were determined. Epoxy based hybrid material with 10 wt. % of the organically modified montmorillonite has significantly lower activation energy values for the defined reaction rates, thereby confirming the catalytic effect of the clay with the layered structure when present in the reaction mixture in sufficient quantity. The diffusion effects at the end of the reaction are more pronounced in the presence of montmorillonite, which indicates that its presence affects the entire curing mechanism. It was found that G', along with montmorillonite content, is affected by the degree of particle dispersion inside the polymer matrix. It was concluded that the addition of montmorillonite up to 3 wt. % improves investigated mechanical properties, while the samples with 5 and 10 wt. % of montmorillonite resulted in agglomeration of the filler particles, which negatively influenced the investigated properties, except for the hardness which increases linearly with the addition of montmorillonite. TG analysis shows that the increase of montmorillonite content in the epoxy matrix slightly improves the thermal stability in the air, while in the inert atmosphere there is no influence on the thermal stability nor on the mechanism of the decomposition of epoxy based hybrid materials. In the system with a thermoplastic polyurethane filler, it was concluded that hybrid materials with a higher content of segmented polyurethane (10 and 15 wt. %), curing process starts at lower temperatures and the maximum speed is achieved at lower temperatures and the highest value of changes in total enthalpy of the crosslinking reaction is determined for the epoxy hybrid material with polyurethanes containing 30 wt. % of hard segments. Tensile strength of hybrid materials increases with the increase of hard segments content in the polyurethane elastomer as well as with the increase of polyurethane content in the epoxy matrix. The addition of thermoplastic segmented polyurethanes significantly increased the elongation at break of prepared epoxy resins hybrid materials. The increase of the hard segments content in polyurethane, in the same ratio, improves hardness of epoxy based hybrid material. It was concluded that the final properties of hybrid materials are influenced by the selection of initial compounds, methods of processing and the curing conditions. It was concluded, as well that knowing the kinetic parameters of curing reaction is important for the proper selection of optimal parameters for production and processing of hybrid materials in industrial conditions.en
dc.languagesr (latin script)
dc.publisherУниверзитет у Новом Саду, Технолошки факултетsr
dc.relationinfo:eu-repo/grantAgreement/MESTD/Integrated and Interdisciplinary Research (IIR or III)/45022/RS//
dc.rightsopenAccessen
dc.rights.urihttps://creativecommons.org/licenses/by-nc-nd/4.0/
dc.sourceУниверзитет у Новом Садуsr
dc.subjectEpoksidne smolesr
dc.subjectEpoxy resinsen
dc.subjecthibridni materijalisr
dc.subjectmontmorilonitsr
dc.subjecttermoplastični poliuretanisr
dc.subjectkinetika reakcije umrežavanjasr
dc.subjecthybrid materialsen
dc.subjectmontmorilloniteen
dc.subjectthermoplastic polyurethanesen
dc.subjectcuring kineticsen
dc.titleStrukturiranje i određivanje kinetike reakcija nastajanja funkcionalnih hibridnih materijala na osnovu epoksidnih smolasr
dc.title.alternativeStructure design and determination of curing kinetics for epoxy based functional hybrid materialsen
dc.typedoctoralThesisen
dc.rights.licenseBY-NC-ND
dc.identifier.fulltexthttp://nardus.mpn.gov.rs/bitstream/id/41036/IzvestajKomisije.pdf
dc.identifier.fulltexthttps://nardus.mpn.gov.rs/bitstream/id/41035/Disertacija.pdf
dc.identifier.fulltexthttps://nardus.mpn.gov.rs/bitstream/id/41036/IzvestajKomisije.pdf
dc.identifier.fulltexthttp://nardus.mpn.gov.rs/bitstream/id/41035/Disertacija.pdf
dc.identifier.rcubhttps://hdl.handle.net/21.15107/rcub_nardus_11401


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