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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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Manufacturing of micro-structures by two-photon polymerization
Skalický, Jiří ; Petrůj, Jaroslav (referee) ; Richtera, Lukáš (advisor)
Utilization of focused laser beam for photo-polymerization represents an elegant and fast method how to manufacture microstructures in dimensions from hundreds of nanometres to tens of micrometres. Two-photon photo-polymerization is used with advantage to manufacture microstructures with sub-micrometre details. In this case the laser wavelength is about two times longer comparing to the spectral region of the highest photoresist sensitivity and the two-photon photo-polymerization is initiated only in the positions of sufficient optical intensity. Precise and controlled positioning of the photoresist with respect to the laser focus ensures only illumination of areas of future microstructure and initialization of photo-polymerization here. Fine details of manufactured microstructures depends, except the laser beam focusing, also on the chosen photoresist and quenching of polymerization in non-illuminated areas.
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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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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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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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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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