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Optimization and characterization of dimethacrylate-based resin
Baradzina, Lizaveta ; Petruš, Josef (referee) ; Poláček, Petr (advisor)
This diploma thesis was focused on the optimization and characterization of resins based on dimethacrylate monomers. The polymerization process was also monitored depending on the type and molar ratio of monomers used, on the content of barium glass filler and the presence of glass fibers. Changes in the viscoelastic properties of materials during polymerization were also investigated. The following methods were used to characterize the prepared dimethacrylate resins and composite materials based on them: viscosimetry, differential scanning photocalorimetry (DPC), photoreology, dynamic mechanical analysis (DMA) and thermogravimetric analysis (TGA). The dynamic viscosity of the prepared dimethacrylate matrices was determined by viscometry. Based on the results of DPC analysis of the tested resins, the dependences of heat flow on time, conversion on time and polymerization rate on conversion were created. With photoreology, the course of curing, the onset of the gelation point and changes in the viscoelastic properties of the systems were monitored. The viscoelastic properties of the cured composite materials were then determined by DMA in the three-point arrangement. TGA was performed to accurately determine the composition of the tested samples
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Photopolymerization study of composites
Baradzina, Lizaveta ; Petruš, Josef (referee) ; Poláček, Petr (advisor)
This bachelor thesis investigated the influence of ceramic nanofibers and particle filler on the curing kinetics of composite materials with dimethacrylate matrix. Changes in viscoelastic properties of materials during polymerization were also monitored. Within this work, four types of materials were prepared: particle composite, fiber composite, hybrid composite and pure matrix. Composite systems of different compositions were characterized by photorheology, differential photocalorimetry (DPC), and dynamic-mechanical analysis (DMA). The effect of light intensity and irradiation time on changes in the rheological properties of materials that occur during photopolymerization were investigated using photorheology. Based on the results of DPC analysis of the tested samples the dependencies of conversion on time and polymerization rate on conversion were created. The viscoelastic properties of the cured composites were determined by DMA analysis in a three-point arrangement.
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Photosensitive thin polymeric layers
Rudická, Andrea ; Klusoň, Petr (referee) ; Veselý, Michal (advisor)
This bachelor thesis deals with photosensitive thin polymeric layers. The experimental part deals with the composition preparation and layers coating. The prepared layers were exposed and studied in detail for their color response to the light. The aim was to prepare a dosimeter, to achieve significant color change between individual doses, to improve the mechanical resistence of the layers and to adjust the sensitivity of the compositions to UVB radiation.
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Crosslinking of thermosensitive functionalized copolymers by blue light
Křivánková, Nikola ; Michlovská, Lenka (referee) ; Vojtová, Lucy (advisor)
Cílem mé bakalářské práce byla příprava hydrogelu s hybridní sítí pouze z jednoho typu biodegradovatelného kopolymeru. Nový degradabilní hydrogel, obsahující jak fyzikální interakce (vznikající při fyziologické teplotě 37 °C), tak i chemické vazby iniciované modrým světlem by mohl být využit jako resorbovatelný kryt ran nebo jako injektovatelný nosič s postupným a velice dobře řízeným uvolňováním léčiv. Termocitlivý PLGA–PEG–PLGA kopolymer syntetizovaný živou polymerací za otevření kruhu byl následně funkcionalizován anhydridem kyseliny itakonové za vzniku ITA/PLGA–PEG–PLGA/ITA makromonomeru citlivého jak na světlo, tak i na změnu teploty. Při teplotě 37 °C tvoří kopolymer díky hydrofobním interakcím micelární síť. Dvojné vazby kyseliny itakonové, která je navázaná na koncích kopolymerního řetězce, umožňují fotochemické zesítění micel a zvýšení tak hydrolytické stability hydrogelu. Syntetizované kopolymery byly charakterizované metodami GPC a 1H NMR. Vznik fyzikální sítě při fyziologické teplotě byl potvrzen reologickou analýzou. Fyzikálně zesítěný ITA/PLGA–PEG–PLGA/ITA hydrogel byl následně, v přítomnosti hydrofilního fotoiniciátoru LiTPO, ozářen modrým světlem (o vlnové délce 430–490 nm) a chemicky charakterizován pomocí ATR-FTIR. Vzniklý hydrogel byl transparentní, ohebný, absorboval až 1176 % vody a ve fyziologickém roztoku při 37 °C byl stabilní 20 dní. ITA/PLGA–PEG–PLGA/ITA hydrogel s hybridní sítí byl rovněž připraven v přítomnosti síťovadla, které výrazně snížilo dobu potřebnou na zesítění hydrogelu, nicméně další analýzy jsou potřeba k podrobnějšímu pochopení principů nových typů hydrogelů.
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Effect of preparation conditions on the structure and properties of hybrid light curing composites
Škriniarová, Nina ; Ing. Vladimír Pavelka. Ph.D. (referee) ; Jančář, Josef (advisor)
The purpose of this thesis was to implement and evaluate series of experiments focused on the impact of mixing conditions and component dispensing on the structure and properties of hybrid polymer composite materials for resistant dental fillings. There were suggested some preparation methods and subsequently some mechanical properties of prepared samples were measured. Short non-formable polymer fibers in combination with filler particles of various particle sizes were added into the matrix. As matrix a polymer, light curable monomer mixture based on urethandimethacrylate and dodecandioldimethacrylate was used. Tensile deformation curves of prepared samples were measured. Morphology of prepared composites was observed by surface fractography using scanning electron microscopy (SEM). Samples were evaluated by comparing of tensile curves and morphology observed on SEM slides. The best way of component mixing and dispensing was evaluated based on comparison of experiment results and properties predicted by existed models.
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Two-photon photopolymerization with multiple laser beams
Skalický, Jiří ; Pilát,, Zdeněk (referee) ; Jákl,, Petr (advisor)
Photopolymerization is a technique used to create surface structures or microobjects from a photoresist. This process is started by illuminating the sample with a light of proper wavelength absorbed by the resist. After exposure, the sample is processed according to the type of the photoresist – be it heating, treating with developer or just washing the unaffected monomer with some reagent. Focused femtosecond laser beam with double wavelength can be used in the process. Short pulse length with high photon density starts two-photon absorption localized in the vicinity of focal point. The method resolution is thus increased and details with 1/10 micrometer size can be created. Moreover, very short laser pulse decreases the heat affected zone and the risk of thermal initiation is minimized. Manufacturing of larger structures composed of tiny details with two-photon photopolymerization is time-demanding process. Therefore, we have complemented the optical setup with spatial light modulator (SLM), which splits the incoming laser beam into several beams with holograms dynamically generated by a computer. Polymerization can be thus performed by multiple foci simultaneously which can be used to create separated microparticles or periodical surface structures. Additional speed improvement of the process can be substitution of static configuration, requiring sample replacement after each exposition, with continuous setup using microfluidic channel steadily supplied with photoresist transported to the active region of the sample.
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Photopolymerization kinetics of dimethacrylate dental resin
Vaněk, Martin ; Bystřický, Zdeněk (referee) ; Poláček, Petr (advisor)
Aim of magister´s thesis was to study reaction kinetics of dental materials. Thesis was focused on dimethacrylate dental polymers, which are for example used for dental restoration, tooth repair and creating now teeth. First part of the thesis concentrates on influence of molar ratio on reation kinetics by addition of other monomer to polymer resin. Second part concentrates on influence of addition of additive silica on reaction kinetics of polymerization. Essential variables know as a polymerization ratio, conversion, gel point, glass transition temperature and storage modulus were studied. Firstly, polymerization ratio and conversion were observed by differential scanning calorimetry (DSC). Secondly rheology was observed by photoreometr. Finally, glass transition temperature and storage modulus were observed by dynamic mechanical analysis (DMA). Behaviour changes caused by addion of monomer or filler point out decrease of polymeration ratio and converstion. Same behaviour was observed by short exposure. In order to established network formation, values of gel point increased by higher concentration of monomer or filler. Glass transition temperature and storage modulus measured by DMA were evaluated. Those valuables had variable tendency due to monomer acting like filler at higher concentration. Also contradictory impact of different material conversion and filler concetration was discussed.
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Thermal Stability/Degradation of High Viscosity Dental Resins
Bystřický, Zdeněk ; Trautmann, Radoslav (referee) ; Poláček, Petr (advisor)
This diploma thesis deals with the influence of long term thermal load on the stability of high-viscous resins used for dental composites matrix. The process of polymerization was also investigated in connection with type and ratio of monomer units, mass content of the initiator system and the presence of nanosilica filler. Prepared resins were characterized by differential compensation photocalorimetry (DPC) and dynamic mechanical analysis (DMA). The dependence of the heat flow on time was measured by DPC. Based on the experimental data, the dependence of conversion on time and the dependence of polymerization rate on conversion were determined. Viscoelastic properties of the cured resins were determined by DMA. Experimentally measured data implies that by the influence of elevated temperature both the degree of conversion and the polymerization rate decreased. With a higher content of the initiator system incorporated in resin the decrease was more significant. Therefore, we can conclude that when the resin was exposed to the elevated temperature one of the components of the initiator system was inactivated. For the photopolymerized resins presence of two glass transition temperatures is typical due to the inhomogenous morphology of the cured resin. There are two types of domains with varying relative composition. However, after the degradation only one glass transition temperature was detected. That was caused by reducing the resin viscosity due to the increased temperature. Higher mobility of the initiator system molecules and monomers itself resulted in more homogenous structure of the cured resin. In case of elevated temperature exposed resins more significant decrease of the elastic modulus was observed. The curing process is considerably influenced by the type and ratio of the monomer units and by the presence of filler.
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Preparation of methacrylated hydroxybutyrates monomers and polymers
Liška, Marek ; Mgr. Petra Zbořilová, Ph.D (referee) ; Figalla, Silvestr (advisor)
The aim of this work is the study, design, and preparation of methacrylated derivatives of poly(3-hydroxybutyrate) and the subsequent preparation of polymers from the prepared precursors. A total of six compounds were prepared. The prepared compounds include methyl-3-hydroxybutyrate and ethyl-3-hydroxybutyrate prepared by alcoholytic depolymerization with monofunctional alcohol and their methacrylated derivatives. The preparation of ethylene glycol terminated oligomer of 3-hydroxybutyrate prepared via depolymerization using ethylene glycol in two ways is also an essential part of the work. The first way involves depolymerization using conventional heating and the second one explores the preparation of a series of oligomers with different molecular weights using microwave heating. Methacrylated derivatives of the prepared oligomers were also prepared. The prepared compounds and their actual preparation are characterized using multiple analytical methods including VPO, NMR, GPC, FT-IR, LC-MS, and DSC. A series of polymers were obtained from the prepared compounds by radical polymerization using purple light (with wavelength 405 nm) as the energy source. The prepared polymer networks were characterized by DSC and their tensile strengths were tested.
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Crosslinking of thermosensitive functionalized copolymers by blue light
Křivánková, Nikola ; Michlovská, Lenka (referee) ; Vojtová, Lucy (advisor)
Cílem mé bakalářské práce byla příprava hydrogelu s hybridní sítí pouze z jednoho typu biodegradovatelného kopolymeru. Nový degradabilní hydrogel, obsahující jak fyzikální interakce (vznikající při fyziologické teplotě 37 °C), tak i chemické vazby iniciované modrým světlem by mohl být využit jako resorbovatelný kryt ran nebo jako injektovatelný nosič s postupným a velice dobře řízeným uvolňováním léčiv. Termocitlivý PLGA–PEG–PLGA kopolymer syntetizovaný živou polymerací za otevření kruhu byl následně funkcionalizován anhydridem kyseliny itakonové za vzniku ITA/PLGA–PEG–PLGA/ITA makromonomeru citlivého jak na světlo, tak i na změnu teploty. Při teplotě 37 °C tvoří kopolymer díky hydrofobním interakcím micelární síť. Dvojné vazby kyseliny itakonové, která je navázaná na koncích kopolymerního řetězce, umožňují fotochemické zesítění micel a zvýšení tak hydrolytické stability hydrogelu. Syntetizované kopolymery byly charakterizované metodami GPC a 1H NMR. Vznik fyzikální sítě při fyziologické teplotě byl potvrzen reologickou analýzou. Fyzikálně zesítěný ITA/PLGA–PEG–PLGA/ITA hydrogel byl následně, v přítomnosti hydrofilního fotoiniciátoru LiTPO, ozářen modrým světlem (o vlnové délce 430–490 nm) a chemicky charakterizován pomocí ATR-FTIR. Vzniklý hydrogel byl transparentní, ohebný, absorboval až 1176 % vody a ve fyziologickém roztoku při 37 °C byl stabilní 20 dní. ITA/PLGA–PEG–PLGA/ITA hydrogel s hybridní sítí byl rovněž připraven v přítomnosti síťovadla, které výrazně snížilo dobu potřebnou na zesítění hydrogelu, nicméně další analýzy jsou potřeba k podrobnějšímu pochopení principů nových typů hydrogelů.
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