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Effect of body fluids on setting, structure and mechanical properties of phosphate bone cements
Bednaříková, Vendula ; Michlovská, Lenka (oponent) ; Vojtová, Lucy (vedoucí práce)
Presented diploma thesis describes the preparation and characterization of composite calcium-phosphate bone cements (CPCs). In the literature review properties and structure of tricalcium phosphates (TCPs) are described, including their interaction with body environment. In the experimental work, first of all, sample preparation technique was determined by experiments with setting reactions provided in ultrapure water environment. Optimal technique of setting CPC samples included memory foam setting mold, ending setting reactions by absolute cold ethanol and vacuum drying procedures. Consequently, the work describes the sample preparation and process of TCP bone cement setting in both natural (pig blood) and simulated body fluids (physiological, Hank´s and Ringer´s solutions). Morphology study by Scanning Electron Microscopy (SEM) was performed for samples set for 1 day, 1 week, 2 weeks and 1 month, due to the significant change in crystalline structure proving as well by X-ray diffraction (XRD) analysis by determining -TCP conversion to calcium-deficient hydroxyapatite (CDHA). Porosity investigated by X-ray computed microtomography (-CT) was slightly higher at sample set in natural blood. Mechanical properties of CPC samples measured by mechanical compression tests showed stable cement strength set in physiological solution already after 1 day while cements set in blood has shown still increasing strength even at 1 month. On contrary, strength of cement samples rapidly decreased after 2 weeks of setting in both Hank´s and Ringer´s solutions probably due to its slightly acidic pH accelerating CPC disintegration. As a result, setting environment has significant effect on resulting CPC properties and natural blood in comparison to simulated plasma had shown better CPC properties while more closely imitating the in vivo conditions.
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The effect of polymer microfibers on rheological and mechanical properties of calcium phosphate bone cements
Dzurov, Matej ; Montufar Jimenez, Edgar Benjamin (oponent) ; Vojtová, Lucy (vedoucí práce)
Proposed master’s thesis focuses on mechanical and rheological properties of biodegradable polymer-calcium phosphate bone cement composite reinforced with PCL (poly(-caprolactone)) and PCL-Pluronic polymer microfibers. The theoretical part describes bone structure, evolution of bone cements and structural additives. In the experimental part, synthesis and characterization of PLGA-PEG-PLGA thermosensitive copolymer and -tricalcium phosphate powder is depicted as well as microfibers preparation technique. Copolymer aqueous solution was used to counteract the paste limited injectability, where liquid to powder (L/P) ratio of 0.5 ml/g was used for all of the samples. The two different mixing techniques were used in cement preparation to modulate the sample’s porosity. PCL and PCL-Pluronic fibers used to reinforce the cement were added in the amount of 1, 3 and 5 wt. % to the total mass of cement paste. Prepared pastes were studied at the laboratory (23 °C) and under physiological conditions (37 °C) using dynamical rheological analysis, with the aim to establish workability and setting of the paste. Samples for the rest of the analyses were enabled to set at physiological conditions for the duration of 10 days. Afterward, mechanical parameters like compressive strength, elastic modulus and diametric tensile strength of dried and in some cases hydrated samples were tested. Porosity was established using micro-computed tomography. Scanning electron microscopy was used to study microstructure and fiber incorporation into a ceramic matrix. Presence of fibers was semi-quantitatively studied using Fourier transformed infrared spectroscopy. X-ray diffraction provided data about powder phase transformation and mineralogical aspects of cement. Individual sample performances were evaluated and compared. As a result, addition of either hydrophobic PCL or amphiphilic PCL-Pluronic fibers into polymer-phosphate cement slightly increased compressive strength where PCL-Pluronic modified fibers performed better. Therefore was concluded, that polymer-phosphate bone cement reinforced with microfibers is promising candidate for surgical practice.
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The effect of polymer microfibers on rheological and mechanical properties of calcium phosphate bone cements
Dzurov, Matej ; Montufar Jimenez, Edgar Benjamin (oponent) ; Vojtová, Lucy (vedoucí práce)
Proposed master’s thesis focuses on mechanical and rheological properties of biodegradable polymer-calcium phosphate bone cement composite reinforced with PCL (poly(-caprolactone)) and PCL-Pluronic polymer microfibers. The theoretical part describes bone structure, evolution of bone cements and structural additives. In the experimental part, synthesis and characterization of PLGA-PEG-PLGA thermosensitive copolymer and -tricalcium phosphate powder is depicted as well as microfibers preparation technique. Copolymer aqueous solution was used to counteract the paste limited injectability, where liquid to powder (L/P) ratio of 0.5 ml/g was used for all of the samples. The two different mixing techniques were used in cement preparation to modulate the sample’s porosity. PCL and PCL-Pluronic fibers used to reinforce the cement were added in the amount of 1, 3 and 5 wt. % to the total mass of cement paste. Prepared pastes were studied at the laboratory (23 °C) and under physiological conditions (37 °C) using dynamical rheological analysis, with the aim to establish workability and setting of the paste. Samples for the rest of the analyses were enabled to set at physiological conditions for the duration of 10 days. Afterward, mechanical parameters like compressive strength, elastic modulus and diametric tensile strength of dried and in some cases hydrated samples were tested. Porosity was established using micro-computed tomography. Scanning electron microscopy was used to study microstructure and fiber incorporation into a ceramic matrix. Presence of fibers was semi-quantitatively studied using Fourier transformed infrared spectroscopy. X-ray diffraction provided data about powder phase transformation and mineralogical aspects of cement. Individual sample performances were evaluated and compared. As a result, addition of either hydrophobic PCL or amphiphilic PCL-Pluronic fibers into polymer-phosphate cement slightly increased compressive strength where PCL-Pluronic modified fibers performed better. Therefore was concluded, that polymer-phosphate bone cement reinforced with microfibers is promising candidate for surgical practice.
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Effect of body fluids on setting, structure and mechanical properties of phosphate bone cements
Bednaříková, Vendula ; Michlovská, Lenka (oponent) ; Vojtová, Lucy (vedoucí práce)
Presented diploma thesis describes the preparation and characterization of composite calcium-phosphate bone cements (CPCs). In the literature review properties and structure of tricalcium phosphates (TCPs) are described, including their interaction with body environment. In the experimental work, first of all, sample preparation technique was determined by experiments with setting reactions provided in ultrapure water environment. Optimal technique of setting CPC samples included memory foam setting mold, ending setting reactions by absolute cold ethanol and vacuum drying procedures. Consequently, the work describes the sample preparation and process of TCP bone cement setting in both natural (pig blood) and simulated body fluids (physiological, Hank´s and Ringer´s solutions). Morphology study by Scanning Electron Microscopy (SEM) was performed for samples set for 1 day, 1 week, 2 weeks and 1 month, due to the significant change in crystalline structure proving as well by X-ray diffraction (XRD) analysis by determining -TCP conversion to calcium-deficient hydroxyapatite (CDHA). Porosity investigated by X-ray computed microtomography (-CT) was slightly higher at sample set in natural blood. Mechanical properties of CPC samples measured by mechanical compression tests showed stable cement strength set in physiological solution already after 1 day while cements set in blood has shown still increasing strength even at 1 month. On contrary, strength of cement samples rapidly decreased after 2 weeks of setting in both Hank´s and Ringer´s solutions probably due to its slightly acidic pH accelerating CPC disintegration. As a result, setting environment has significant effect on resulting CPC properties and natural blood in comparison to simulated plasma had shown better CPC properties while more closely imitating the in vivo conditions.
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