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Made available in DSpace on 2014-06-11T19:35:08Z (GMT). No. of bitstreams: 0 Previous issue date: 2001-07-19Bitstream added on 2014-06-13T20:06:32Z : No. of bitstreams: 1 sigoli_fa_dr_araiq.pdf: 3331714 bytes, checksum: f15f140dd71661951c9acd489ff18e44 (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Neste trabalho, obteve-se uma matriz porosa com alto teor de sílica a partir de vidros Pyrex® utilizando-se o tratamento hidrotérmico. A matriz porosa é formada principalmente por dois processos: (i) reação da água no estado supercrítico com a rede vítrea e, (ii) separação e lixiviação de fases. A matriz apresenta-se macroporosa, possuindo também baixa percentagem de micro e mesoporos. Através de técnicas espectroscópicas verifica-se que a matriz apresenta grupos silanóis de superfície, os quais foram utilizados em reações de funcionalização. A espectroscopia de ressonância magnética nuclear de 29Si, MAS RMN, indica a presença de grupos ordenados, (SiO)4Si, no interior da matriz e do grupo (SiO)3Si(OAl). Os espectros de 29Si, CPMAS RMN, indicam que a matriz porosa é constituída de átomos de silício localizados em dois ambientes químicos diferentes, (SiO)3Si(OH), e (SiO)4Si. Pelo espectro de 27Al MAS RMN confirma-se a presença do grupo Al-O-Si, o qual é responsável pela formação de sítios ácidos de Brönsted. Pela análise dilatométrica verifica-se que a contração máxima da matriz foi de 6% em 1365oC, aumentando a densidade do material, o tamanho médio dos poros, devido a consolidação de micro e mesoporos, diminuindo assim a área superficial. A matriz cristaliza-se em 950oC como α-cristobalita pertencente ao grupo espacial P41212. A matriz obtida foi então utilizada como suporte para complexos luminescentes. O complexo diaquatris(tenoiltrifluoroacetonato)európio(III), [Eu(tta)3(H2O)2], impregnado ou ancorado na matriz, apresenta emissões com alargamento não-homogêneo indicando que há interações entre o complexo e a superfície da matriz... / In the present work, porous silica matrix has been obtained from Pyrex glass by hydrothermal treatment under saturated steam condition. The formation process was principally investigated using scanning and transmission electron microscopies and Raman spectroscopy. The results indicate that the process of phase separation takes place on edge of vitreous sample at lower temperature than of glass-transition temperature at room atmosphere. This process occurs due to the glass hydration by hydrothermal treatment that diminishes both viscosity and glass transition temperature. The segregated orthoborate phase was leached out by water in supercritical condition. The formation and leaching of this phase together with essential reactions between water and silica at supercritical condition contribute to obtain a porous silica matrix. The matrix has a high percentage of porosity, an interconnected macroporous structure, a low percentage of micro and mesopores and also a good thermal stability. It is non-crystalline and after thermal treatment it presented X-ray pattern characteristic of cristobalite and a low contraction of volume. The chemical analysis shows a high concentration of silicon and low concentrations of aluminum and boron. The chemical environments of silicon and aluminum atoms into the porous silica matrix were investigated by solid state NMR spectroscopy. The 29Si MAS NMR spectrum exhibits a broad signal at -110 ppm, typical of an ordered silica phase. The chemical nature of surface was better understood with application of the 1H - 29Si CPMAS NMR technique. This technique leaded to a strong and selective... (Complete abstract, click electronic access below)

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Resumo: Neste trabalho, obteve-se uma matriz porosa com alto teor de sílica a partir de vidros Pyrex® utilizando-se o tratamento hidrotérmico. A matriz porosa é formada principalmente por dois processos: (i) reação da água no estado supercrítico com a rede vítrea e, (ii) separação e lixiviação de fases. A matriz apresenta-se macroporosa, possuindo também baixa percentagem de micro e mesoporos. Através de técnicas espectroscópicas verifica-se que a matriz apresenta grupos silanóis de superfície, os quais foram utilizados em reações de funcionalização. A espectroscopia de ressonância magnética nuclear de 29Si, MAS RMN, indica a presença de grupos ordenados, (SiO)4Si, no interior da matriz e do grupo (SiO)3Si(OAl). Os espectros de 29Si, CPMAS RMN, indicam que a matriz porosa é constituída de átomos de silício localizados em dois ambientes químicos diferentes, (SiO)3Si(OH), e (SiO)4Si. Pelo espectro de 27Al MAS RMN confirma-se a presença do grupo Al-O-Si, o qual é responsável pela formação de sítios ácidos de Brönsted. Pela análise dilatométrica verifica-se que a contração máxima da matriz foi de 6% em 1365oC, aumentando a densidade do material, o tamanho médio dos poros, devido a consolidação de micro e mesoporos, diminuindo assim a área superficial. A matriz cristaliza-se em 950oC como α-cristobalita pertencente ao grupo espacial P41212. A matriz obtida foi então utilizada como suporte para complexos luminescentes. O complexo diaquatris(tenoiltrifluoroacetonato)európio(III), [Eu(tta)3(H2O)2], impregnado ou ancorado na matriz, apresenta emissões com alargamento não-homogêneo indicando que há interações entre o complexo e a superfície da matriz...(Resumo completo, clicar acesso eletrônico abaixo) / Abstract: In the present work, porous silica matrix has been obtained from Pyrex glass by hydrothermal treatment under saturated steam condition. The formation process was principally investigated using scanning and transmission electron microscopies and Raman spectroscopy. The results indicate that the process of phase separation takes place on edge of vitreous sample at lower temperature than of glass-transition temperature at room atmosphere. This process occurs due to the glass hydration by hydrothermal treatment that diminishes both viscosity and glass transition temperature. The segregated orthoborate phase was leached out by water in supercritical condition. The formation and leaching of this phase together with essential reactions between water and silica at supercritical condition contribute to obtain a porous silica matrix. The matrix has a high percentage of porosity, an interconnected macroporous structure, a low percentage of micro and mesopores and also a good thermal stability. It is non-crystalline and after thermal treatment it presented X-ray pattern characteristic of cristobalite and a low contraction of volume. The chemical analysis shows a high concentration of silicon and low concentrations of aluminum and boron. The chemical environments of silicon and aluminum atoms into the porous silica matrix were investigated by solid state NMR spectroscopy. The 29Si MAS NMR spectrum exhibits a broad signal at -110 ppm, typical of an ordered silica phase. The chemical nature of surface was better understood with application of the 1H - 29Si CPMAS NMR technique. This technique leaded to a strong and selective... (Complete abstract, click electronic access below) / Orientador: Marian Rosaly Davolos / Coorientador: Miguel Jafelicci Junior / Banca: Aldo José Gorgatti Zarbin / Banca: Hermi Felinto de Brito / Banca: Henrique Eisi Toma / Banca: Sandra Helena Pulcinelli / Doutor

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Recently there has been an increased focus on the use of microfluidics for the synthesis of different products. One of the products proposed for synthesis is quantum dots. Microfluidics often uses Polydimethylsiloxane for structure in microfluidic chips, but quantum dots use octadecene in several synthesis steps. The purpose of this work was to create a lab setup capable of anodically bonding 4” diameter wafers, and to characterize the bond formed using the Plaza test chip so that microfluidic devices using glass and silicon as substrates could be created. Two stainless steel electrodes placed on top of a hot plate were attached to a high power voltage supply to perform anodic bonding. A Plaza test mask was created and used to pattern P type silicon wafers. The channels etched were between 300 and 500nm deep and ranged between 1000µm and 50µm. These wafers were then anodically bonded to Corning 7740 glass wafers. Bonding stopped once the entire surface of the wafer was bonded, determined by visual inspection. All bonds were formed at 400°C and the bond strength and toughness between wafers bonded at 400V and 700V was compared. A beam model was used to predict the interfacial fracture toughness, and the stress at the bond was calculated with a parallel spring model. By measuring the crack length of the test structures under a light microscope the load conditions of the beam could be found. It was concluded that the electrostatic forces between the wafers give the best indication of what the bond quality will be. This was seen by the large difference in crack length between samples that were bonded using a thick glass wafer (1 mm) and a thin glass wafer (500µm). The observed crack lengths for the thick glass wafers were between 40 and 60µm. Thin glass wafers had a crack length between 20 and 40µm. The fracture toughness was calculated using the beam model approximation. Fracture toughness of the thin glass wafers was 7MPa m1/2, and of the thick glass wafers was 30 MPa m1/2. The fracture toughness of the thick glass wafers agreed with results found through the use of the double cantilever beam samples in literature. The maximum observed interfacial stress was 70 MPa. Finally, to measure the change in the size of the sodium depletion zone formed during bonding, samples were placed under a scanning electron microscope (SEM). Depletion zones were found to be between 1.1 and 1.4µm for thin glass samples that were bonded at 400 and 700 volts. This difference was not found to have a significant effect on the strength or fracture toughness observed. Thicker glass samples could not have their depletion zone measured due to SEM chuck size.

The fabrication characteristic of focused ion beam (FIB) for Pyrex glass was investigated. FIB has several advantages such as high sensitivity, high material removal rates, low forward scattering, and direct fabrication in selective area without any etching mask, etc. In this study, FIB etched Pyrex glass was used for fast fabrication of 3-D submicron structures. A high-aspect-ratio (HRA) glass structure of 5 (1.97µm depth/0.39µm width) was fabricated. The experimental results in terms of limiting beam size, ion dose¡]ion/cm2¡^, beam current, etc was discussed. Xenon difluoride (XeF2) was applied to enhance the FIB process. Its influence on glass fabrication is studied and characterized.

Focused Ion Beam (FIB) has several advantages such as high sensitivity, high material removal rates, low forward scattering and directing fabrication. Without any etched mask, processing time can be reduced. Pyrex glass etched by FIB is used for fast fabrication of 3-D submicron structure mold. In this study, glass is used as substrate. The UV-cured resin that spin-coated onto a mold has 3-D structure patterns. 3-D structure patterns are transferred on the plate to investigate the effects of parameters of UV cured, pressure and exposure time on the occurrence of defects. The relationship of these processing parameters for the imprinting process is also realized. Besides, the material property of UV-cured resin is investigated. UV-Cured resin is investigated by thermogravimetric Analysis (TGA) to measure the degradation temperature (Td). The hardness and modulus of UV-Cured resin was measured by nanoindentation to realize deformed ability of material for the imprinting process. Moreover, the contact angle of Pyrex glass is measured to investigate its surface quality for the imprint process.

Polarized Raman spectroscopy has been used to measure the deuterium isotope effect, (delta)pK = pKD2O – pKH2O, for the second ionization constant of sulfuric acid in the temperature range of 25 °C to 200 °C at saturation pressure. Results for pK in light water agree with the literature within ± 0.034 pK units at alltemperatures under study, confirming the reliability of the method. The ionization constant of deuterated bisulfate, DSO4-, differs significantly from previous literature results at elevated temperatures. This results in an almost constant (delta)pK ≈ 0.425 ± 0.076 over the temperature range under study. Differences in (delta)pK values between the literature and current results can be attributed to the effect of dissolved silica from cell components. The new results are consistent with (delta)pK models that treat the temperature dependence of (delta)pK by considering differences in the zero-point energy of hydrogen bonds in the hydrated product and reactant species. The phosphate hydrolysis equilibrium was measured between the temperatures of 5 °C and 80 °C and the borate/boric acid equilibrium between the temperatures of 25 °C and 200 °C. The high alkalinity and temperatures experienced by these two systems had a significant impact on the glass dissolution and equilibrium. / Raman spectroscopy was used to measure the small differences in ionization constants for weak acids/bases as a function of temperature. / University of Guelph, Atomic Energy of Canada Limited (AECL), Bruce Power, University Network of Excellence in Nuclear Engineering (UNENE), National Sciences and Engineering Research Council of Canada (NSERC), Natural Resources Canada, Ontario Power Generation (OPG), Canada Foundation for Innovation

Thesis (M.F.A.)--University of Wyoming, 2009. / Title from PDF title page (viewed on Apr. 12, 2010).