O objetivo deste estudo foi produzir por electrospinning fibras de zircônia, caracterizá-las e avaliar sua influência, como agente de carga, nas propriedades de compósitos tendo como matriz uma resina à base de metacrilatos de uso odontológico. O óxido de zircônio foi utilizado como precursor das fibras obtidas, as quais foram caracterizadas por microscopia eletrônica de varredura (MEV) e analisadas por termogravimetria (ATG). Após tratamento térmico, a morfologia das fibras foi analisada por MEV, a cristalinidade, por difração de raios X e a área superficial específica e a porosidade foram calculadas pelos métodos BET e BJH, respectivamente. Os compósitos odontológicos foram formulados a partir da adição das fibras de zircônia obtidas por electrospinning (grupo Híbrido N+F) e comparados com os formados com as partículas originais de zircônia nanométrica (grupo Nano N), e com a própria matriz sem carga (grupo Matriz). O grau de conversão (GC) foi analisado usando espectroscopia no infravermelho por transformada de Fourier (FT-IR). Os compósitos e a matriz foram submetidos ao ensaio de resistência à flexão, que também permitiu determinar o módulo de elasticidade. Os compósitos odontológicos foram submetidos ao ensaio de microdureza Vickers e tenacidade à fratura em deformação plana. Os compósitos estudados não formaram trincas radiais porque a matriz polimérica absorveu e dissipou a tensão gerada no material e por esse motivo não foi possível determinar a tenacidade à fratura. Observou-se que o GC dos compósitos odontológicos não apresentou diferença estatisticamente significativa entre os grupos N+F e N, sendo 54,2% e 55,1%, respectivamente. O GC da matriz polimérica foi de 68,1% (±0,6)%, sendo estatisticamente superior ao dos compósitos experimentais. Para os ensaios de resistência à flexão, módulo de elasticidade e microdureza Vickers não houve diferença estatisticamente significativa entre os grupos dos compósitos, sendo que o grupo matriz apresentou resultado estatisticamente inferior para a dureza e módulo de elasticidade. / This study aimed to produce zirconia ultrafine fibers through electrospinning method, characterize them and evaluate their influence as reinforcing element on properties for composites having as matrix methacrylate-based resin for dental use. Zirconium oxide was used as precursor of the fibers obtained which were characterized by scanning electron microscopy (SEM) and analyzed by thermogravimetry (TGA). After heat treatment fibers morphology was analyzed by SEM, crystallinity by X-ray diffraction and porosity and specific surface area were calculated by BET and BJH methods, respectively. The dental composites were formulated from the addition of zirconia fibers obtained by electrospinning (Hybrid group N+F) and compared with those formed with the original nanometric zirconia particles (Nano group N), and with matrix without reinforcing element (group Matriz). The degree of conversion (DC) was analyzed by Fourier transform infrared spectroscopy (FT-IR). The composites and matrix groups were submitted to flexural strength test, which also allowed determining elastic modulus. The dental composites were tested on Vickers microhardness and fracture toughness in flat deformation. The studied composites studied didn’t form radial cracks because polymer matrix absorbed and dissipated generated tension in material and for this reason it wasn’t possible to determine the fracture toughness. It was observed that dental composites DC showed no statistically significant difference between groups N+F and N, being 54.2% and 55.1%, respectively. The polymer matrix DC was 68.1% being statistically higher than experimental composites. Flexural strength, elastic modulus and Vickers microhardness showed no statistically significant difference between composite groups, and matrix group results were statistically lower for microhardness and elastic modulus.

O objetivo deste estudo foi produzir por electrospinning fibras de zircônia, caracterizá-las e avaliar sua influência, como agente de carga, nas propriedades de compósitos tendo como matriz uma resina à base de metacrilatos de uso odontológico. O óxido de zircônio foi utilizado como precursor das fibras obtidas, as quais foram caracterizadas por microscopia eletrônica de varredura (MEV) e analisadas por termogravimetria (ATG). Após tratamento térmico, a morfologia das fibras foi analisada por MEV, a cristalinidade, por difração de raios X e a área superficial específica e a porosidade foram calculadas pelos métodos BET e BJH, respectivamente. Os compósitos odontológicos foram formulados a partir da adição das fibras de zircônia obtidas por electrospinning (grupo Híbrido N+F) e comparados com os formados com as partículas originais de zircônia nanométrica (grupo Nano N), e com a própria matriz sem carga (grupo Matriz). O grau de conversão (GC) foi analisado usando espectroscopia no infravermelho por transformada de Fourier (FT-IR). Os compósitos e a matriz foram submetidos ao ensaio de resistência à flexão, que também permitiu determinar o módulo de elasticidade. Os compósitos odontológicos foram submetidos ao ensaio de microdureza Vickers e tenacidade à fratura em deformação plana. Os compósitos estudados não formaram trincas radiais porque a matriz polimérica absorveu e dissipou a tensão gerada no material e por esse motivo não foi possível determinar a tenacidade à fratura. Observou-se que o GC dos compósitos odontológicos não apresentou diferença estatisticamente significativa entre os grupos N+F e N, sendo 54,2% e 55,1%, respectivamente. O GC da matriz polimérica foi de 68,1% (±0,6)%, sendo estatisticamente superior ao dos compósitos experimentais. Para os ensaios de resistência à flexão, módulo de elasticidade e microdureza Vickers não houve diferença estatisticamente significativa entre os grupos dos compósitos, sendo que o grupo matriz apresentou resultado estatisticamente inferior para a dureza e módulo de elasticidade. / This study aimed to produce zirconia ultrafine fibers through electrospinning method, characterize them and evaluate their influence as reinforcing element on properties for composites having as matrix methacrylate-based resin for dental use. Zirconium oxide was used as precursor of the fibers obtained which were characterized by scanning electron microscopy (SEM) and analyzed by thermogravimetry (TGA). After heat treatment fibers morphology was analyzed by SEM, crystallinity by X-ray diffraction and porosity and specific surface area were calculated by BET and BJH methods, respectively. The dental composites were formulated from the addition of zirconia fibers obtained by electrospinning (Hybrid group N+F) and compared with those formed with the original nanometric zirconia particles (Nano group N), and with matrix without reinforcing element (group Matriz). The degree of conversion (DC) was analyzed by Fourier transform infrared spectroscopy (FT-IR). The composites and matrix groups were submitted to flexural strength test, which also allowed determining elastic modulus. The dental composites were tested on Vickers microhardness and fracture toughness in flat deformation. The studied composites studied didn’t form radial cracks because polymer matrix absorbed and dissipated generated tension in material and for this reason it wasn’t possible to determine the fracture toughness. It was observed that dental composites DC showed no statistically significant difference between groups N+F and N, being 54.2% and 55.1%, respectively. The polymer matrix DC was 68.1% being statistically higher than experimental composites. Flexural strength, elastic modulus and Vickers microhardness showed no statistically significant difference between composite groups, and matrix group results were statistically lower for microhardness and elastic modulus.

Kyoto University (京都大学) / 0048 / 新制・課程博士 / 博士(工学) / 甲第16510号 / 工博第3503号 / 新制||工||1530(附属図書館) / 29167 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 落合 庄治郎, 教授 田中 功 / 学位規則第4条第1項該当

Kyoto University (京都大学) / 0048 / 新制・論文博士 / 博士(工学) / 乙第12650号 / 論工博第4078号 / 新制||工||1547(附属図書館) / 29728 / (主査)教授 辻 伸泰, 教授 落合 庄治郎, 教授 乾 晴行 / 学位規則第4条第2項該当

The microstructures of the near-surface layers on AA3104 aluminium alloys and their evolution through rolling and deep drawing processes have been investigated. The effect of the near-surface layers on the optical property of AA3104 aluminium alloy has also been assessed. It was revealed that two types of near-surface deformed layers, both with different microstructures different from the underlying bulk alloy, were generated on the surface of AA3104 aluminium alloy during rolling. Both of them are characterized by ultrafine, equiaxed grains, with diameters <100 nm for type A near-surface deformed layer and <200 nm for type B near-surface deformed layer. A high population density of nano-sized, oxygen-rich particles is present along grain boundaries within type A deformed layer. But type B deformed layer is free of oxygen-rich particles. Type A deformed layer was generated through two mechanisms, i.e. geometric dynamic recrystallization and mechanical alloying. Rolling introduced plastic strain in the surface/near-surface region of aluminium sheet was of sufficient magnitude to cause geometric dynamic recrystallization and thus microstructure refinement. In addition, the incorporation of oxides into the near-surface region was also involved in the formation of type A deformed layer. However, the formation of type B deformed layer was only attributed to severe strain induced geometric dynamic recrystallization. Type A deformed layer was mainly formed at the early stages of hot rolling. The subsequent rolling and deep drawing reduced the thickness of type A deformed layer by distributing it over a larger surface area. During cold rolling, type A deformed layer broke into patches with the extension of alloy surface. Type B deformed layer may be generated on the nascent surface if the strain is sufficiently severe to cause geometric dynamic recrystallization. For the hot rolled alloy sheets, the surface/near-surface region is mainly covered by type A deformed layer. However, for the alloys after cold rolling, only limited area is covered with type A deformed layer. The thicknesses of the near-surface deformed layers are not uniform across the surface of AA3104 aluminium alloy. The maximum thickness of type A deformed layer on transfer slab is approximately 4 µm, while that on re-roll gauge sheet is ~1 µm, and ~0.8 µm on the final gauge sheet, ~400 nm on formed cup and ~100 nm on formed can. Type A deformed layer is randomly distributed as patches on the cold rolled aluminium sheet. The reflectivity of oxygen-rich particles is lower compared with the reflectivity of aluminium. As a result, the type A deformed layer patches absorb more incident light than the area without type A deformed layer. Further, there are plenty of micro-scale mini-cracks present on type A deformed layer, their opening sizes are in the equivalent scale of the wavelength of visible light. The incident light may not able to be reflected out if they go into these mini-cracks. It is more prone to happen for short wavelength light since it is easier for them to go into the mini-cracks than long wavelength light. As a result, less short wavelength visible light is reflected from the type A deformed layer patches. Thus, such patches exhibit a yellow appearance while the surrounding area appears the original silver white aluminium appearance. The aluminium sheet with a high coverage of type A deformed layer exhibits a low total reflectance. Further, its total reflectance is with a significant “red shift”. Neither the macro-scale surface roughness nor the ultrafine grain size affects the total reflectance of aluminium alloys. The total reflectance of aluminium alloys is primarily dependent on the presence of type A deformed layer.

O objetivo deste estudo foi produzir por electrospinning fibras de zircônia, caracterizá-las e avaliar sua influência, como agente de carga, nas propriedades de compósitos tendo como matriz uma resina à base de metacrilatos de uso odontológico. O óxido de zircônio foi utilizado como precursor das fibras obtidas, as quais foram caracterizadas por microscopia eletrônica de varredura (MEV) e analisadas por termogravimetria (ATG). Após tratamento térmico, a morfologia das fibras foi analisada por MEV, a cristalinidade, por difração de raios X e a área superficial específica e a porosidade foram calculadas pelos métodos BET e BJH, respectivamente. Os compósitos odontológicos foram formulados a partir da adição das fibras de zircônia obtidas por electrospinning (grupo Híbrido N+F) e comparados com os formados com as partículas originais de zircônia nanométrica (grupo Nano N), e com a própria matriz sem carga (grupo Matriz). O grau de conversão (GC) foi analisado usando espectroscopia no infravermelho por transformada de Fourier (FT-IR). Os compósitos e a matriz foram submetidos ao ensaio de resistência à flexão, que também permitiu determinar o módulo de elasticidade. Os compósitos odontológicos foram submetidos ao ensaio de microdureza Vickers e tenacidade à fratura em deformação plana. Os compósitos estudados não formaram trincas radiais porque a matriz polimérica absorveu e dissipou a tensão gerada no material e por esse motivo não foi possível determinar a tenacidade à fratura. Observou-se que o GC dos compósitos odontológicos não apresentou diferença estatisticamente significativa entre os grupos N+F e N, sendo 54,2% e 55,1%, respectivamente. O GC da matriz polimérica foi de 68,1% (±0,6)%, sendo estatisticamente superior ao dos compósitos experimentais. Para os ensaios de resistência à flexão, módulo de elasticidade e microdureza Vickers não houve diferença estatisticamente significativa entre os grupos dos compósitos, sendo que o grupo matriz apresentou resultado estatisticamente inferior para a dureza e módulo de elasticidade. / This study aimed to produce zirconia ultrafine fibers through electrospinning method, characterize them and evaluate their influence as reinforcing element on properties for composites having as matrix methacrylate-based resin for dental use. Zirconium oxide was used as precursor of the fibers obtained which were characterized by scanning electron microscopy (SEM) and analyzed by thermogravimetry (TGA). After heat treatment fibers morphology was analyzed by SEM, crystallinity by X-ray diffraction and porosity and specific surface area were calculated by BET and BJH methods, respectively. The dental composites were formulated from the addition of zirconia fibers obtained by electrospinning (Hybrid group N+F) and compared with those formed with the original nanometric zirconia particles (Nano group N), and with matrix without reinforcing element (group Matriz). The degree of conversion (DC) was analyzed by Fourier transform infrared spectroscopy (FT-IR). The composites and matrix groups were submitted to flexural strength test, which also allowed determining elastic modulus. The dental composites were tested on Vickers microhardness and fracture toughness in flat deformation. The studied composites studied didn’t form radial cracks because polymer matrix absorbed and dissipated generated tension in material and for this reason it wasn’t possible to determine the fracture toughness. It was observed that dental composites DC showed no statistically significant difference between groups N+F and N, being 54.2% and 55.1%, respectively. The polymer matrix DC was 68.1% being statistically higher than experimental composites. Flexural strength, elastic modulus and Vickers microhardness showed no statistically significant difference between composite groups, and matrix group results were statistically lower for microhardness and elastic modulus.

Titanium is thanks to its high corrosion resistance and biocompatibility widely used in medicine. Ti alloys are used due to their superior mechanical properties instead of pure Ti for load carrying components. Ti alloys are often alloyed with elements which are toxic for human body and further increase cost of Ti products. Main focus of current development is to create pure Ti with better mechanical properties. It can be done by reducing grain size by processes based on severe plastic deformation. The aim of this work is to evaluate fatigue properties as well as fatigue crack initiation and propagation mechanism of Ti grade 2 with the ultrafine grained structure. After microstructure analysis, fatigue tests with symmetrical loading were executed. Fracture surfaces of ultrafine grained Ti grade 2 were observed after fatigue tests for identification of failure mechanism. Results were compared with those for course-grained Ti grade 2.

This work deals with the study of limestone and corundum dry milling using attritor-type stirred mill in a batch mode. There were stearin and polyethylene glycol used as surfactants and spherical shaped steel grinding elements used for the experimental part of the work. The main idea was to examine behavior of the selected grinding stock type within a long-term grinding forces exposure in selected conditions of ultrafine dry milling leading up to the submicron area. Characterization of samples was performed by laser granulometry, X-ray powder diffraction analysis, flame atomic absorption spectroscopy, objective color determination and electrokinetic potential measurement. Experimetaly measured data implies that in all cases there was a re-agglomeration of the grinding stock particles occurring, although in different stages of the disintegration process and in mutually various degree. The analysis results denote that a larger erosion of the crystal structures with the associated increase of the amorphous phase in the submicron particle size took place in the grinding stock.

Title: Study of ultrafine-grained materials prepared with different methods of severe plastic deformation Author: RNDr. Tomáš Krajňák Department: Department of Physics of Materials, Faculty of Mathematics and Physics, Charles University in Prague Supervisor: Doc. RNDr. Kristián Máthis, PhD., Department of Physics of Materials, Faculty of Mathematics and Physics, Charles University in Prague Abstract: Interstitial free steel with ultrafine-grained (UFG) structure was prepared by high-pressure torsion (HPT). The development of the microstructure as a function of the number of HPT turns was studied at the centre, half-radius and periphery of the HPT-processed disks by X-ray line profile analysis (XLPA), positron annihilation spectroscopy (PAS) and electron microscopy. The dislocation densities and the dislocation cell sizes determined by XLPA were found to be in good agreement with those obtained by PAS. The evolution of the dislocation density, the dislocation cell and grain sizes, the vacancy cluster size, as well as the high-angle grain boundary (HAGB) fraction was determined as a function of the equivalent strain. It was found that first the dislocation density saturated, then the dislocation cell size reached its minimum value and finally the grain size got saturated. For very high strains after the...

Estimating infiltration of quasi-ultrafine black carbon particles by an absorbance method: air quality in Pavla Stehlíková Abstract This diploma thesis focused on the estimating quasi-ultrafine particles amount in school gyms continue previous study researched air quality in schools. The size-segregated mass concentration of particulate matter was measured in three elementary school gyms in central part of Prague, on periphery of Prague and in a small settlement Černošice during twenty campaigns, from 2005 to 2009. The mass concentration of particulate matter were measured by 5-staged Sioutas impactor. For this thesis we have selected samples on filters with particle size <0,25µm. To evaluate carbonaceous particles amount we used reflectance. Reflectance was transformed into an absorption coefficient (m- 1 .10-5 ). The average levels of absorptions coeficients were higher outdoors (14,66 ± 8,93 m- 1 .10-5 ) than indoors (13,64 ± 8,08 m-1 .10-5 ). The correlations between absorption coeffitients outdoors and indoors were significant for all schools (Spearman's correlation coefficient at intervals 0,834-0,957, regression slope 0,759-1,007), suggesting a high outdoor-to-indoor penetration rate. The weak correlation between absorption coefficients and number of exercising pupils (correlation coefficient 0,059)...