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Adetola, Opeyemi. "Immobilization of Heteropolyacids in Silica Gel." Digital Commons @ East Tennessee State University, 2016. https://dc.etsu.edu/etd/3050.
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Silica gels containing incorporated heteropolyacids (HPAs) were synthesized in acidic media by co-condensation of tetraethoxysilane (TEOS) with phosphotungstic or phosphomolybdic acids using sol-gel technique. Effect of the synthesis conditions on their structure and morphology was studied. Yields of modified materials were some lower as compared to non-modified silica gels. All materials were mesoporous but contained micropores in their structures. Presence of bands of Keggin’s structures in FT-IR spectra along with absence of XRD patterns of crystalline HPAs confirmed their fine incorporation into silica network. Particle sizes of modified materials were 800-1100 nm excepting for W-containing sample obtained with trimethylstearylammonium chloride. This unusual effect was attributed to stabilization of primary silica nanoparticles by interaction between surfactant and HPA. High ratio HPA/TEOS resulted in partial loss of porosity. Obtained results might be used for optimization of synthesis of effective catalysts and adsorbents containing HPAs in mesoporous structure.
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Selwyn, Rebecca. "Improved adsorption calorimeter : studies of loose grained silica gel and silica gel-based selective water sorbent (SWS-1L)." Thesis, University of Bristol, 2015. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.702188.
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This thesis aimed to develop a new version of an adsorption calorimeter originally proposed by Ahamat and Tierney. A more rigorous approach was taken in terms of mechanical components, vacuum equipment, calibration of thermoelectric modules, and length of tests. Novel contributions include the new temperature control algorithm, new adsorbent configuration, new adsorbent, and consideration of the effect of residual air on the kinetics of adsorption. Improved design of the hardware reduced the air ingress from 1mbar/hour to
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Kapusuz, Derya. "Sol-gel Synthesis Of Dna Encapsulated Silica." Master's thesis, METU, 2009. http://etd.lib.metu.edu.tr/upload/2/12610627/index.pdf.
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Sol-gel processing routes for encapsulation of double stranded DNA in solid porous silica hosts have been established. The encapsulation was carried out in two steps: hydrolysis of a silica-forming alkoxide-based sol was followed by condensation/gelation to a solid form upon addition of a buffer solution containing DNA molecules. The effects of gelation chemistry and DNA amount on chemical and microstructural properties of resultant silica matrices and on DNA encapsulation efficiency were investigated. The analytical characterization was performed by UV-vis spectroscopy, 29Si nuclear magnetic resonance spectroscopy and by nitrogen adsorption studies. It was demonstrated that DNA incorporation had a pH-dependent catalytic effect on gelation kinetics and promoted silica network completion. In addition, the scale of porosity and the average pore size of the resultant silica increased with gelation pH and also with DNA-buffer solution in the starting sol-gel formulation. The chemistry-derived pore size variation controls the DNA encapsulation efficiency in the silica matrices and the DNA holding capacity strongly depends on the scale of the porosity attained.
The selective adsorption of ethidium bromide- a DNA-intercalative reagent molecule- on DNA-silica gels confirmed that the DNA molecules remained entrapped within the silica host in their native state without any deterioration. Besides pure silica, amine-functionalized hybrid silica hosts were also formed by sol-gel. The hybrid gels were found not to be suitable for DNA encapsulation, as these matrices dissolve in aqueous environment due to incomplete silica network formation. The DNA-doped silica hosts may provide promising matrices for development of biosensors, bioreactors and bioassay platforms.
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Tan, Bing. "Controlled synthesis and functionalization of nanoporous sol-gel silica particles and gels." Lexington, Ky. : [University of Kentucky Libraries], 2005. http://lib.uky.edu/ETD/ukychen2005d00329/etd.pdf.
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Thesis (Ph. D.)--University of Kentucky, 2005.Title from document title page (viewed on November 2, 2005). Document formatted into pages; contains xix, 336 p. : ill. Includes abstract and vita. Includes bibliographical references (p. 331-334).
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Spencer, Laura Marie. "Evaluation of sand treated with colloidal silica gel." Diss., Georgia Institute of Technology, 2010. http://hdl.handle.net/1853/37131.
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Liquefiable soils are common at ports due to the use of hydraulic fills for construction of waterfront facilities. Liquefaction-induced ground failure can result in permanent ground deformations that can cause loss of foundation support and structural damage. This can lead to substantial repair and/or replacement costs and business interruption losses that can have an adverse effect on the port and the surrounding community. Although numerous soil improvement methods exist for remediating a liquefaction-prone site, many of these methods are poorly suited for developed sites because they could damage existing infrastructure and disrupt port operations. An alternative is to use a passive remediation technique. Treating liquefiable soils with colloidal silica gel via permeation grouting has been shown to resist cyclic deformations and is a candidate to be used as a soil stabilizer in passive mitigation.
The small-strain dynamic properties are essential to determine the response to seismic loading. The small-to-intermediate strain shear modulus and damping ratio of loose sand treated with colloidal silica gel was investigated and the influence of colloidal silica concentration was determined. The effect of introducing colloidal silica gel into the pore space in the initial phase of treatment results in a 10% to 12% increase in the small-strain shear modulus, depending on colloidal silica concentration. The modulus reduction curve indicates that treatment does not affect the linear threshold shear strain, however the treated samples reduce at a greater rate than the untreated samples in the intermediate-strain range above 0.01% cyclic shear strain. It was observed that the treated sand has slightly higher damping ratio in the small-strain range; however, at cyclic shear strains around 0.003% the trend reverses and the untreated sand begins to have higher damping ratio.
Due to the nature of the colloidal silica gelation process, chemical bonds continue to form with time, thus the effect of aging on the dynamic properties is important. A parametric study was performed to investigate the influence of gel time on the increase in small-strain shear modulus. The effect of aging increases the small-strain shear modulus after gelling by 200 to 300% for the 40-minute-gel time samples with a distance from gelation (time after gelation normalized by gel time) of 1000 to 2000; 700% for the 2-hour-gel time sample with a distance from gelation of 1000; and 200 to 400% for the 20-hour-gel time samples with a distance from gelation of 40 to 100.
The treatment of all potentially liquefiable soil at port facilities with colloidal silica would be cost prohibitive. Identifying treatment zones that would reduce the lateral pressure and resulting pile bending moments and displacements caused by liquefaction-induced lateral spreading to prevent foundation damage is an economic alternative. Colloidal silica gel treatment zones of varying size and location were evaluated by subjecting a 3-by-3 pile group in gently sloping liquefiable ground to 1-g shaking table tests. The results are compared to an untreated sample. The use of a colloidal silica treatment zone upslope of the pile group results in reduced maximum bending moments and pile displacements in the downslope row of piles when compared to an untreated sample; the presence of the treatment zone had minimal effect on the other rows of piles within the group.
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Williams, Sian Lowri. "Photochemistry and photophysics of anthracenes on silica gel." Thesis, Loughborough University, 1996. https://dspace.lboro.ac.uk/2134/19426.
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Studies have been carried out investigating the photochemical and photophysical properties of anthracene adsorbed on silica gel. The photochemistry and photo physics of anthracene in solution are well reported and known, hence its choice as a probe for the silica gel surface. UV -visible absorption and fluorescence spectra of anthracene adsorbed on silica gel reveal aggregate formation at very low loadings (1 % of a monolayer) indicating preferential adsorption occurs at some surface sites. Laser flash photolysis at 355 nm produces both the triplet and radical cation of anthracene, their production was found to be mono- and multi-photonic respectively. The decays of both these transients were complex and the rates increased with increasing loading. Analysis of the triplet state decay has been carried out by studying the delayed fluorescence which arises from triplet triplet annihilation. Fractal and twodimensional models have been used to describe this bimolecular decay. The coadsorption of anthracene and an electron donor having an oxidation potential below 1.09 V on silica gel causes electron transfer to occur from the electron donor to the anthracene radical cation produced following laser flash photolysis at 355 nm. Studies using a selection of electron donors with varying reduction potentials were carried out. The electron donor transfers an electron to the anthracene radical cation, thus greatly accelerating its rate of decay; for electron donors such as triphenylamine, N,N-dimethylaniline and N,N,N',N'tetramethyl- l,4-phenylenediamine the rise of the donor radical cation is observed as the anthracene cation decays. These systems were studied using fluorescence measurements and laser flash photolysis to study any fluorescence quenching and the rate of decay of both the anthracene triplet and radical cation. A selection of anthracene derivatives adsorbed onto silica gel were also briefly studied to see the effect of substituent group and its position. Symmetrically substituted dialkoxyanthracenes and 9-cyanoanthracene were used. The transient absorption spectra of the 2,3- and 2,6-dialkoxyderivatives and 9-cyanoanthracene revealed spectral similarities with that of unsubstituted anthracene. The spectra of9,10- and I,S-didecyloxyanthracene showed significant differences in the radical cation spectra to those obtained for unsubstituted anthracene.
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Adeogun, Michael J. "Silica sol-gel hybrids based on ionene polymers." Thesis, University of Surrey, 1998. http://epubs.surrey.ac.uk/843746/.
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By use of the Menshutkin reaction a variety of polyviologens has been synthesised containing bromide, tosylate or mesylate counter-ions and varying methylene units. Owing to the ionic character of these main-chain polymers, these polyviologens are also known as ionene polymers. Additionally, this ionic character conveys a wide range of properties including the ability to undergo redox reactions and display liquid crystalline behaviour. The redox behaviour of these polymers can be followed easily by a colour change in the polyviologen. It was this reasoning, and the susceptibility of polyviologens to atmospheric water, that first led to the introduction of these polymers into a silica sol-gel network to produce 'durable' sol-gel redox sensors. The sol-gel process was found to be a convenient and versatile route to produce inorganic networks using the acid-catalysed hydrolysis and condensation of silicon alkoxide precursors. Synthetic methods were developed to optimise the incorporation of various polyviologens into a silica network. A variety of analytical techniques was employed to characterise the polyviologens and the corresponding sol-gel hybrids. Results from SAXS, IR and surface analysis provide strong evidence that the polyviologens have an effect on the structure of the inorganic component. Rare surface fractal behaviour was observed and the pore geometry was found to go from smooth and cylindrical to ink-bottle in shape for some of the hybrid systems. An hypothesis is forwarded suggesting that the presence and concentration of polyviologen, electrostatic interactions between N+ and silanol groups, and hydrophobic hydration may all play an important role in determining the structure of the silica network.
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Steinthal, Michael Gregory 1964. "Laser densification of sol-gel-derived silica coatings." Thesis, The University of Arizona, 1989. http://hdl.handle.net/10150/277183.
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Sol-gel derived silica coatings were deposited on soda-lime-silica by dip-coating. An absorbing metallic layer was sputtered onto the surface of the gel to couple near-infrared radiation from a Nd:YAG laser into the transparent coating. Laser energy was utilized to heat the ceramic coating on a substrate which has a lower glass transition temperature than the coating. Scanning the sample across the beam's path resulted in the formation of a 50 mum wide channel. The characteristics of a channel were altered by varying laser power, sol-gel coating thickness, and scanning speeds. Profilometry and SEM analysis verified that the coating can be heated to high temperatures without damaging the substrate.
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Silva, Junior José da. "Obtenção de xerogel de sílica a partir das cascas de arroz em uma aproximação bottom-up para produção de materiais em eletrônica." Florianópolis, SC, 2009. http://repositorio.ufsc.br/xmlui/handle/123456789/93406.
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Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro Tecnológico, Programa de Pós-Graduação em Engenharia Elétrica, Florianópolis, 2009.Made available in DSpace on 2012-10-24T21:43:06Z (GMT). No. of bitstreams: 1 266490.pdf: 3362494 bytes, checksum: 6f0e40dce0871c4b18b495a44d1a3e28 (MD5)
O presente trabalho tem por objetivo desenvolver uma rota de obtenção de dióxido de silício a partir das cascas de arroz, realizando um pré-tratamento com água régia, solução piranha e pirólise em mufla a 600°C por 4 horas. Com estes procedimentos buscou-se um grau de pureza acima dos 99%, adequado ao uso do material na síntese de uma matriz microporosa que servirá ao desenvolvimento de dispositivos eletrônicos futuramente. Realizou-se, em cada etapa de separação da sílica, análise termogravimétrica, calorimetria diferencial de varredura, espectroscopia de infravermelho com transformada de Fourier, fluorescência e difração de raios X, com o objetivo de conhecer as etapas de separação da matéria orgânica e as mudanças de composição e estrutura ocorridas no pré-tratamento e na pirólise final em mufla. Com o dióxido de silício obtido a partir das cascas de arroz foram sintetizados géis dentro do processo Sol-Gel, com a solubilização alcalina, a precipitação ácida, a moldagem, a gelificação, o crescimento do gel e a secagem para obter o xerogel. Foi verificado que os xerogéis produzidos, ao secarem, apresentaram fraturas causadas por pressões capilares geradas na microporosidade que impossibilitou a preservação do volume inicial, elemento fundamental no projeto de dispositivos eletrônicos. É apresentada uma via para evitar a degradação do volume das amostras, através da secagem supercrítica, utilizando dióxido de carbono na substituição da fase líquida. Isto atenuaria as pressões capilares no ato de remoção dos solventes dispersos, eliminando as correntes de fuga e permitindo a construção dos dispositivos.
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Forero, Duenas Carlos Antonio. "Characterisation of a silica-gel as a geotechnical cement." Thesis, Imperial College London, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.301001.
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Crossley, Jill E. "Photoinduced electron transfer on the surface of silica gel." Thesis, Loughborough University, 2000. https://dspace.lboro.ac.uk/2134/35558.
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The kinetics of electron transfer between the radical cations of a series of anthracene derivatives and a variety of amine electron donors were studied on the surface of silica gel. The anthracene derivatives were excited with 355 nm radiation and formed radical cations by multi-photon ionisation. The radical cation absorption decay was measured by diffuse reflectance laser flash photolysis at wavelengths between 680 and 780 nm, depending upon the identity of the substituent of the anthracene. The decay kinetics of the radical cations were complex and non-exponential. The addition to the surface of a co-adsorbed electron donor, with an oxidation potential below that of the anthracene derivative resulted in an increase in the rate of the radical cation decay because of the electron transfer from the donor species. The kinetics of electron transfer were fitted with using the dispersive model of Albery.
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Seaton, Kenneth Marshall III. "Functionalized Silica Gel for Adsorption of Cesium from Solution." Digital Commons @ East Tennessee State University, 2017. https://dc.etsu.edu/etd/3215.
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Mesoporous silica gel containing embedded phosphotungstic acid (PTA) was synthesized by sol-gel co-condensation of tetraethyl orthosilicate with PTA in acidic media. The obtained material had high Brunauer-Emmett-Teller Theory (BET) surface area and pore volume. A characteristic band of the Keggin structure of PTA was present in its FT-IR spectrum while its X-ray diffraction patterns were absent. This proved the embedding of PTA on a sub-molecular level and not as a second phase. Acidic sites were determined by neutralization with base in aprotic solvent, followed by titration of the remaining base with an acid. The material demonstrated high adsorption capacity of Cs. Kinetic studies showed that the adsorption data correlates strongly with the pseudo-second order model. At higher temperatures, the nature of adsorption fit the Langmuir model extremely well. The obtained results can be used in the development of an effective adsorbent for clean-up of water contaminated by radioactive 137Cs.
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Toyama, Dominique Yukie. "Efeito da bioinspiração e infiltração de zircônia por sílica nas propriedades mecânicas de bicamadas cerâmicas /." São José dos Campos, 2017. http://hdl.handle.net/11449/149755.
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Orientador: Renata Marques de Melo MarinhoCoorientador: Tiago Moreira Bastos Campos
Banca: Rubens Nisie Tango
Banca: Getulio de Vasconcelos
Resumo: Neste trabalho avaliou-se o comportamento mecânico e a homogeneidade estrutural de bilaminados cerâmicos com configuração convencional (compressão da zircônia) e bioinspirada (tração da zircônia) com e sem infiltração de sílica. Além disso, determinou-se a distribuição de tensões utilizando a análise de elementos finitos, e avaliou-se o modo de falha e o mecanismo de adesão da interface porcelana/zircônia. Amostras bilaminadas foram confeccionadas com Y-TZP e cerâmica injetável e divididos em 4 grupos (n=30): zircônia sob compressão (T), zircônia infiltrada sob compressão (I), zircônia sob tração (B) e zircônia infiltrada sob tração (BI); para teste da resistência à flexão biaxial. A infiltração por sílica ocorreu pelo método sol-gel. Os dados (MPa) do ensaio mecânico foram avaliados com análise de Weibull (IC 95 %). Análise de elementos finitos utilizou o critério de tensão máxima principal para avaliar a distribuição de tensões nos modelos e seus resultados foram apresentados em forma de figuras e gráficos da tensão máxima principal (TMP). A camada de infiltração foi caracterizada usando DRX e microscopia (MEV, MEV-FEG e EDS). O comportamento da interface foi analisado usando resistência ao risco e dureza. O grupo mais homogêneo estruturalmente foi o BI (m= 9,59). A concentração de tensão na cerâmica feldspática foi menor nos grupos bioinspirados. Houve formação de silicato de zircônia na superfície dos discos de zircônia infiltrados e preenchimento de defeitos superficiais... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: This study analyzed the mechanical behavior of bilayers using conventional arrangement (leucite ceramic under traction) and a bioinspired arrangement (zirconia under traction) with or without sol-gel silica infiltration, analyze stress distribution using FEA, characterize infiltration layer and observe interfacial behavior. 120 bilayered specimens were produced for biaxial flexural strength testing using Y-TZP and pressed ceramic and divided into 4 groups (n=30): zirconia under compression (T), infiltrated zirconia under compression (I), zirconia under traction (B) and infiltrated zirconia under traction (BI). The zirconia was infiltrated using sol-gel method. The results for the biaxial flexural strength (MPa) were analyzed using Weibull analysis (CI 95 %). Stress distribution within the models were examined using maximum principal stress and the results were presented as graphs and figures. The infiltration layer was characterized using XRD and microscopy (SEM, FEG-SEM and EDS). The interfacial behavior was analyzed using scratch test and micro-hardness indentation. The BI group was the most reliable (m=9.59). The stress distribution in the feldspar ceramic was better for the bioinspired groups. The infiltrated zirconia discs presented zirconia silicate formation on the surface and plugged internal flaws. The traditional zirconia had a better scratch performance compared to the infiltrated zirconia. The interfacial indentation showed that the weakest link of the set is the ... (Complete abstract click electronic access below)
Mestre
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McGiveron, James Kevin. "Aspects of sol-gel chemistry : the adsorption properties of silica sol-gel monoliths and the preparation of indium(III) oxide and indium(III)/tin(IV) oxide thin films by the inorganic sol-gel process." Thesis, Brunel University, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.294504.
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Torikai, Delson. "Preparação e caracterização da silica vitrea de alta pureza por Verneuil, : a partir da silica sol-gel." [s.n.], 1994. http://repositorio.unicamp.br/jspui/handle/REPOSIP/264999.
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Orientadores: Carlos Kenichi Suzuki, Antonio Celso de Fonseca ArrudaTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica
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Resumo: A sílica vítrea é um do" únicos materiais que cobinam excelentes propriedades térmicas, ópticas, dielétricas, mecânicas, assim como alta durabilidade química com o alto grau dc pureza. Tradicionalmente, o quartzo brasileiro na forma de lascas tem sido um insumo básico de grande importância na fabricação da sílica vítrea. A seleção de jazidas com quartzo da melhor qualidade em termos dc impurezas, e processos industriais dc purificação tornam-no um material com concentração total da ordem de 10 ppm de impurezas metálicas. Entretanto, nestes últimos anos, um novo insumo (pó de sílica) tem sido desenvolvido por processo sol-gel chegando a um grau de pureza extrema (< 0.1 ppm DD total de impurezas metálicas); e o mais importante, a sua produção independe da matéria-prima quartzo natural. Na presente pesquisa, utilizamos esses novos insumos de elevada pureza, obtidos por processo sol-gel, na preparação da sílica vítrea por fusão em chama (técnica de Verneuil), que resultou num produto inédito em termos das propriedades pureza e resistência mecânica. Contamos, para isso, com a participação de duas empresas, a Nitto Chemical e a Mitsubishi Rasei, para o fornecimento desses novos insumos, ainda em fase de desenvolvimento, através do canal de cooperação técnica entre a UNICAMP e o NIRiN. Realizamos um estudo sobre a influência das principais características das pós de sílica e do processo de fusão nas propriedades da sílica fundida como a transmitância no infra-vermelho e ultra-violeta, e em particular na viscosidade do material. 0 processo Verneuil de fusão utilizado neste trabalho, mostrou ser um processo limpo, não apresentando contaminações metálicas acima da ordem de 0.1 ppm, A agregação de radicais OH mostrou ser reduzida dependendo do tipo de chama (redutora), como por exemplo pela utilização da chama do gás liquefeito de petróleo (GLP), com contaminação da ordem de 100 ppm em comparação com a contaminação de 200 - 250 ppm verificado para a chama de hidrogênio. A viscosidade da sílica vítrea mostrou ser mais vulnerável à presença de alcalinos nas sílicas livres de Alumínio, tendo sua viscosidade reduzida em uma ordem de grandeza para concentrações de sódio de apenas alguns ppm. A sílica vítrea obtida pela fusão em chama à partir do pó de sílica sol-gel, apresenta conteúdos de impurezas metálicas equivalentes à da sílica vítrea comercial obtida pelo processo sintético de deposição química no estado vapor (CVD) por chama de Hz. Apresenta a vantagem de possuir concentrações de OH 5 vezes inferior, e valores dc viscosidade uma ordem de grandeza superior, além do menor custo do processo de fusão por chama em relação ao processo CVD.
Abstract: Not informed.
Doutorado
Doutor em Engenharia Mecânica
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Silveira, Tayla Fernanda Serantoni da [UNESP]. "Potencialidade analítica de um silsesquioxano e uma sílica organofuncionalizados com imidazol." Universidade Estadual Paulista (UNESP), 2012. http://hdl.handle.net/11449/97898.
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No presente trabalho, a 3-cloropropil sílica gel (SG) e o octa-(3-cloropropil)silsesquioxano (SS) foram preparados e organofuncionalizados com grupos imidazol e os materiais obtidos da funcionalização foram descritos como SGI e SSI, respectivamente. Os materiais funcionalizados foram preliminarmente caracterizados por técnicas tais como: espectroscopia na região do infravermelho (FTIR), difração de raios-X (DRX), microscopia eletrônica de varredura (MEV), além de análise de área superficial e porosidade para o precursor SG e o produto SGI. Foram realizados estudos de adsorção de íons metálicos (Cu2+ e Cd2+) para o SGI e SSI em diferentes meios, tais como: aquoso, etanol 42% e etanol 99%. Determinou-se o tempo de equilíbrio de adsorção para todos os meios e posteriormente, determinou-se a capacidade de adsorção (Nf) através de isotermas com diferentes concentrações molares dos íons metálicos, onde se observou que o SSI possui uma capacidade adsorvente maior que o SGI e ambos os adsorventes tem uma capacidade de adsorção maior para íons Cu2+ do que para os íons Cd2+. Os valores de Nf aumentaram de acordo com a seguinte ordem de solventes: água < etanol 42% < etanol 99%. Em uma segunda etapa do trabalho, após a adsorção dos íons metálicos (Cd2+ e Cu2+) pelo SGI e pelo SSI, reagiu-se os mesmos com ferricianeto de potássio (hexacianoferrato de potássio - HCF) formando-se assim os materiais CdHSGI, CuHSGI, CdHSSI e CuHSSI, respectivamente. Estes materiais foram caracterizados por espectroscopia na região do infravermelho (FTIR), difração de raios-X (DRX), espectroscopia na região do UV-visível (Reflectância difusa) e voltametria cíclica, além de serem testados na determinação eletrocatalítica de substâncias de interesse biológico. Foram realizados estudos voltamétricos da oxidação...
In the present work, 3-chloropropyl silica gel (SG) and octa-(3-chloropropyl)silsesquioxane (SS) were organofunctionalized with imidazole groups and the materials obtained of the functionalization were described as SGI and SSI, respectively. The functionalized materials were preliminarily characterized by very techniques such as: infrared spectroscopy (FTIR), X- ray diffraction (XRD), scanning electron microscopy (SEM), and also analysis of surface area and porosity for the precursor SG and the product SGI. Studies of adsorption were carried for metal ions (Cu2+ and Cd2+) for SGI and SSI in different media, such as: aqueous, ethanol 42% and ethanol 99%. It was determined the adsorption equilibrium time for all media and posteriorly, it was determined adsorption capacity (Nf) through isotherms with different molar concentrations of metal ions, where it was observed that SSI has an adsorption capacity greater than the SGI and both adsorbents have a superior adsorption capacity for ions Cu 2+ than ions Cd2+. The values of Nf increased according the following order of solvents: water < ethanol 42% < ethanol 99 %. After adsorption of metal ions (Cd2+ and Cu2+) by SGI and SSI, it was reacted with potassium ferricyanide (potassium hexacyanoferrate – HCF) thus forming the materials CdHSGI, CuHSGI, CdHSSI and CuHSSI, respectively. These materials were characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), spectroscopy in the UV-visible (diffuse reflectance) and cyclic voltammetry and tested in the electrocatalytic determination of biologically important substances. Voltammetric studies of the electrocatalytic oxidation of ascorbic acid were carried out using CdHSGI and CdHSSI modified carbon paste electrodes, respectively. The CdHSGI modified electrode was sensitive to... (Complete abstract click electronic access below)
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Santos, Daniele Cristina Almeida Hummel Pimenta. "Obtenção e caracterização de materiais dopados SiO2-CdSe a partir de sonogeis de silica." [s.n.], 1994. http://repositorio.unicamp.br/jspui/handle/REPOSIP/265224.
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Orientador: Iris Concepcion Linares de TorrianiTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica
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Resumo: O processo de obtenção de materiais pela via sol-gel tem-se mostrado muito interessante na obtenção de novos materiais como atesta o grande número de trabalhos desenvolvidos na última década. A possibilidade de obter materiais sólidos monolíticos assim como pós, filmes e fibras a partir de uma mistura no estado líquido à temperatura ambiente através de reações de agregação e polimerização é particularmente interessante. A fácil manipulação da composição química precursora permite criar materiais compósitos com propriedades ópticas, eletrônicas, químicas, mecânicas especiais para aplicações em alta tecnologia. Em particular, os materiais compostos de uma matriz vítrea com inclusão de nanocristais semicondutores apresentam propriedades ópticas não-lineares e são considerados de grande importância tecnológica em aplicações estratégicas, como comunicação e processamento de informações. Neste trabalho apresentamos os resultados da obtenção de materiais compostos por partículas semicondutoras imersas numa matriz ele sílica gel. As matrizes hospedeiras foram preparadas por hidrólise do tetraetilortosilicato (TEOS) com adição de nitrato de cádmio. Como agente controlador da cinética ele secagem (drying control chemical additive -DCCA) foram usadas a formamida e a N-N-dimetilformamida. O processo de preparação incluiu a aplicação de doses pré-determinadas de ultrasom de alta potência. As matrizes foram caracterizadas através de técnicas de análise térmica (ADT e ATG), adsorção de gases (BET), picnometria de mercúrio, microscopia eletrônica de varredura (SEM) e espalhamento de raios X a baixos ângulos (SAXS). A impregnação do "sonogel" seco com uma solução de KSeCN realizada em condições de vácuo, permitiu a formação de nanocristais de seleneto de cádmio (CdSe) e melhorou as propriedades mecânicas da matriz. Xerogéis vermelhos e transparentes foram obtidos e caracterizados por espectroscopia óptica de absorção, microscopia eletrônica por transmissão (TEM) e SAXS. Os resultados desses estudos levam a propor um modelo estrutural para estes materiais consistente em uma matriz porosa contendo nanocristais de seleneto de cádmio, apresentando uma distribuição de tamanhos bimodal que depende da concentração de selênio na solução usada para a difusão líquida. O deslocamento das bandas de absorção óptica para grandes energias ("blue shift") revela o confinamento quântico nos nanocristais de seleneto de cádmio
Abstract: The sol-gel process has proved to be extremely interesting in the production of new materiaIs. This is clearly indicated by the great number of publications in this area in the last decade. The possibility of obtaining monolithic solid materials and also powders, films and fibers from a liquid mixture of components at room temperature via aggregation and polymerization reactions is particularly interesting. The easy way in which chemical composition can be modified allows the preparation of composite materiais with specific optical, electronic, chemicalor mechanical properties designed for special applications in modern tecnology. In particular, materiaIs consisting in a vitreous matrix with embedded nanocrystals of semiconductor compounds are known to present non-linear optical properties wich makes them very important in strategic technological applications, such as communications and data processing. In this work we present the results of the preparation of materials consisting of semiconducting nanoparticles embedded in a silica gel matrix. The host matrices were prepared by hydrolysis of tretaethylortosilicate (TEOS) with the addition of cadmium nitrate. Two different additives were used as a drying control agent (DCCA) : formamide and N-Ndimethylformamide. The preparation process included the use of pre-determined doses of high power ultrasound. The matrices were characterized by thermal analyses (TGA and DTA), gas adsorption techniques (BET), mercury picnometry, scanning electron microscopy (SEM) and small angle X ray scattering (SAXS). The impregnation of the dry "sonogels" using a KSeCN solution under vacuum, led to the formation of CdSe nanocrystals and improved the mechanical properties of the matrix. Typically red, transparent xerogels were obtained and characterized by optical absorption spectroscopy, transmission electron microscopy (TEM), and SAXS. The results of this study lead to propose a structural model for these materials, consisting of a porous matrix containing CdSe nanocrystals with a bimodal size distribution that depends on the selenium content in the solution used for the liquid diffusion. The shift in the optical absorption band towards higher energies (blue shift) revcals the quantum confinement in the nanosized particles of cadmium selenide
Doutorado
Doutor em Engenharia Mecânica
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Silveira, Tayla Fernanda Serantoni da. "Potencialidade analítica de um silsesquioxano e uma sílica organofuncionalizados com imidazol /." Ilha Solteira:, 2012. http://hdl.handle.net/11449/97898.
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Orientador: Devaney Ribeiro do CarmoBanca: Urquisa de Oliveira Bicalho
Banca: Everaldo Carlos Venancio
Resumo: No presente trabalho, a 3-cloropropil sílica gel (SG) e o octa-(3-cloropropil)silsesquioxano (SS) foram preparados e organofuncionalizados com grupos imidazol e os materiais obtidos da funcionalização foram descritos como SGI e SSI, respectivamente. Os materiais funcionalizados foram preliminarmente caracterizados por técnicas tais como: espectroscopia na região do infravermelho (FTIR), difração de raios-X (DRX), microscopia eletrônica de varredura (MEV), além de análise de área superficial e porosidade para o precursor SG e o produto SGI. Foram realizados estudos de adsorção de íons metálicos (Cu2+ e Cd2+) para o SGI e SSI em diferentes meios, tais como: aquoso, etanol 42% e etanol 99%. Determinou-se o tempo de equilíbrio de adsorção para todos os meios e posteriormente, determinou-se a capacidade de adsorção (Nf) através de isotermas com diferentes concentrações molares dos íons metálicos, onde se observou que o SSI possui uma capacidade adsorvente maior que o SGI e ambos os adsorventes tem uma capacidade de adsorção maior para íons Cu2+ do que para os íons Cd2+. Os valores de Nf aumentaram de acordo com a seguinte ordem de solventes: água < etanol 42% < etanol 99%. Em uma segunda etapa do trabalho, após a adsorção dos íons metálicos (Cd2+ e Cu2+) pelo SGI e pelo SSI, reagiu-se os mesmos com ferricianeto de potássio (hexacianoferrato de potássio - HCF) formando-se assim os materiais CdHSGI, CuHSGI, CdHSSI e CuHSSI, respectivamente. Estes materiais foram caracterizados por espectroscopia na região do infravermelho (FTIR), difração de raios-X (DRX), espectroscopia na região do UV-visível (Reflectância difusa) e voltametria cíclica, além de serem testados na determinação eletrocatalítica de substâncias de interesse biológico. Foram realizados estudos voltamétricos da oxidação... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: In the present work, 3-chloropropyl silica gel (SG) and octa-(3-chloropropyl)silsesquioxane (SS) were organofunctionalized with imidazole groups and the materials obtained of the functionalization were described as SGI and SSI, respectively. The functionalized materials were preliminarily characterized by very techniques such as: infrared spectroscopy (FTIR), X- ray diffraction (XRD), scanning electron microscopy (SEM), and also analysis of surface area and porosity for the precursor SG and the product SGI. Studies of adsorption were carried for metal ions (Cu2+ and Cd2+) for SGI and SSI in different media, such as: aqueous, ethanol 42% and ethanol 99%. It was determined the adsorption equilibrium time for all media and posteriorly, it was determined adsorption capacity (Nf) through isotherms with different molar concentrations of metal ions, where it was observed that SSI has an adsorption capacity greater than the SGI and both adsorbents have a superior adsorption capacity for ions Cu 2+ than ions Cd2+. The values of Nf increased according the following order of solvents: water < ethanol 42% < ethanol 99 %. After adsorption of metal ions (Cd2+ and Cu2+) by SGI and SSI, it was reacted with potassium ferricyanide (potassium hexacyanoferrate - HCF) thus forming the materials CdHSGI, CuHSGI, CdHSSI and CuHSSI, respectively. These materials were characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), spectroscopy in the UV-visible (diffuse reflectance) and cyclic voltammetry and tested in the electrocatalytic determination of biologically important substances. Voltammetric studies of the electrocatalytic oxidation of ascorbic acid were carried out using CdHSGI and CdHSSI modified carbon paste electrodes, respectively. The CdHSGI modified electrode was sensitive to... (Complete abstract click electronic access below)
Mestre
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Faria, Cristiano Gomes de. "Adsorção de cations metalicos sobre silica organofuncionalizada." [s.n.], 1996. http://repositorio.unicamp.br/jspui/handle/REPOSIP/250626.
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Orientador: Jose de Alencar SimoniDissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica
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Mestrado
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Ling, Dee Ann. "Primary structural evolution in acid-catalyzed silica polysol-gel processes." Diss., Georgia Institute of Technology, 1992. http://hdl.handle.net/1853/11873.
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Arnoldsson, Joel. "Adsorption Chillers : uptake of Ethanol on Type RD Silica gel." Thesis, Linköpings universitet, Energisystem, 2012. http://urn.kb.se/resolve?urn=urn:nbn:se:liu:diva-80930.
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The adsorption cooling technology has the potential to replace all vapor compression based chillers in the future. So, in all over the world immense researches are going on in this field. The purpose of this report is to experimentally investigate whether ethanol could serve as a refrigerant in the technology. Compared to water it has freezing point below 0 °C (-114.1 °C) and can therefore in theory be used in refrigeration applications. The report begins with the theory regarding the adsorption cooling process, describing the cycle and parameters that affect the Coefficient of Performance (COP).In the actual experiment, adsorption between the silica gel and the ethanol vapor is studied at various pressures by maintaining isothermal conditions. An experimental apparatus (Constant Volume Variable Pressure apparatus - CVVP) was fabricated, assembled and tested for this project. After the assembly and testing, volume calibration for the apparatus was carried out as it is essential to know in further experimental calculation. All the data related with the fabrication, assembly and testing of the apparatus and the volume calibrations are presented later in this report in detail.Adsorption experiments are conducted at 301.15K, 311.15K, 321.15K and 331.15K with varying inlet pressure condition to the system and then the uptake data is calculated for each and every experiments using ideal gas equation. Subsequently, the validations of the experimental data with the standard adsorption isotherms are done. Dubinin-Astakhov is found to be the most ideal isotherm to simulate the theoretical data. Its RMSE (Root Mean Square Error) value is found to be 0.506%. It is concluded that ethanol valid option for refrigeration, but further research is needed and recommended.
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Noble, Kate. "Preparation of organically modified mesoporous materials via sol-gel processing." Thesis, University of Sheffield, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.340139.
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Brambilla, Rodrigo. "Sílicas funcionalizadas com octadecilsilano pelos métodos sol-gel e grafting." reponame:Biblioteca Digital de Teses e Dissertações da UFRGS, 2007. http://hdl.handle.net/10183/10993.
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No presente estudo, sílicas funcionalizadas com grupos octadecilsilano (ODS) foram obtidas pelas rotas de grafting e sol-gel. Na rota grafting foram variadas as temperaturas de pré-tratamento da sílica comercial na faixa de 100-450 °C. Na rota sol-gel, foram variadas as razões molares ODS: TEOS, o instante de adição do ODS e a velocidade de agitação da reação. As sílicas foram caracterizadas em termos do teor de carbono, da natureza das espécies imobilizadas, da textura e morfologia pelas técnicas complementares de Análise Elementar (CHN), Espectroscopia Fotoeletrônica de Raios-X (XPS), Espectroscopia molecular no Infravermelho com Transformada de Fourier (FTIR), Espectroscopia de Ressonância Magnética Nuclear de 29Si e 13C (NMR de 29Si e 13C), Adsorção de nitrogênio, Análise Termogravimétrica (TGA), Espalhamento de Laser (LLS), Espectroscopia de Espalhamento de Raios-X em Baixo Ângulo (SAXS), Microscopia de Força Atômica (AFM) e Microscopia Eletrônica de Varredura com Espectroscopia de Emissão de Raios-X por Dispersão de Energia (SEM-EDX).As sílicas funcionalizadas por grafting apresentaram teores de carbono determinados por CHN na faixa de 1,2-3,5 %, morfologia irregular e conformação de grupos ODS próxima ao estado líquido. Já as sílicas funcionalizadas por sol-gel, apresentaram teores de carbono na faixa de 5,0-53 %, combinação de morfologia esférica com lamelar e conformação de grupos ODS próximas ao estado cristalino. A potencialidade das sílicas funcionalizadas como adsorventes de compostos aromáticos em amostras ambientais de água e ar foi avaliada.In the present study, octadecylsilane-modified silicas were obtained by the grafting and the sol-gel methods. In the grafting route, silica pretreatment temperature was varied between 100 and 450 °C. In the sol-gel one, the following variables were evaluated: ODS:TEOS molar ratio, ODS addition time and stirring speed. The resulting silicas were characterized in terms of carbon content, nature of the surface species, texture and morphology by a set of complementary techniques, namely: elemental analysis (CHN), X-ray photoelectron spectroscopy (XPS), infrared spectroscopy with Fourier Transform (FTIR), 29Si e 13C nuclear magnetic resonance (29Si e 13C NMR), nitrogen adsorption, thermogravimetric analysis (TGA), laser-light scattering (LLS), small angle X-ray scattering (SAXS), atomic force microscopy (AFM) and electron scanning microscopy combined with energy dispersive X-ray analysis (SEM-EDX). Chemically-modified silica by grafting presented low carbon content in the range of 1.2 – 3.5 wt.%, irregular morphology and ODS conformation groups close to the liquid state. Hybrid silica prepared by the sol-gel method showed carbon contents between 5.0 and 53.0 wt.%, combining spherical and lamellar morphology, and ODS groups conformation close to the crystalline state. The potentiality of the chemically-modified silicas as sorbents for aromatic compounds was evaluated in environmental water and air matrices.
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Jackson, Dominic. "Organic functionalisation of hexagonal mesoporous silica." Thesis, University of York, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.341112.
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Zhang, Zhengping. "Hydrophobic, fluorinated silica xerogel for low-k applications." Thesis, University of North Texas, 2004. https://digital.library.unt.edu/ark:/67531/metadc4472/.
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A new hydrophobic hybrid silica film was synthesized by introducing one silicon precursor (as modifiers) into another precursor (network former). Hybrid films have improved properties. Hydrolysis and condensation of dimethyldiethoxysilane (DMDES) (solvent (EtOH) to DMDES molar ratio R = 4, water to DMDES molar ratio r = 4, 0.01 N HCl catalyst) was analyzed using high-resolution liquid 29Si NMR. It was found that after several hours, DMDES hydrolyzed and condensed into linear and cyclic species. Films from triethoxyfluorosilane (TEFS) have been shown to be promising interlayer dielectric materials for future integrated circuit applications due to their low dielectric constant and high mechanical properties (i.e., Young's modulus (E) and hardness (H)). Co-condensing with TEFS, linear structures from DMDES hydrolysis and condensation reactions rendered hybrid films hydrophobic, and cyclic structures induced the formation of pores. Hydrophobicity characterized by contact angle, thermal stability by thermogravimetric analysis (TGA), Fourier transform Infrared spectroscopy (FTIR), contact angle, and dynamic secondary ion mass spectroscopy (DSIMS), dielectric constant determined by impedance measurement, and mechanical properties (E and H) determined by nanoindentation of TEFS and TEFS + DMDES films were compared to study the effect of DMDES on the TEFS structure. Hybrid films were more hydrophobic and thermally stable. DMDES incorporation affected the dielectric constant, but showed little enhancement of mechanical properties.
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Roux, Richard. "Synthèse de phase stationnaires monolithiques de silice hybrides pour les techniques séparatives miniaturisées." Thesis, Lyon 1, 2009. http://www.theses.fr/2009LYO10208.
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Ce manuscrit est consacré à la synthèse par procédé sol-gel et à la caractérisation de matériaux monolithiques de silice hybrides pour les techniques séparatives miniaturisées : nano-chromatographie en phase liquide (nano-CPL), électrochromatographie capillaire (ECC) et microsystèmes séparatifs. La partie bibliographique situe les axes de développement récents des techniques séparatives : l’augmentation de l’efficacité par unité de temps, l’augmentation de la capacité de pics et la miniaturisation de ces techniques. Après un descriptif détaillé de l’évolution des techniques séparatives lors de ces dernières années, une attention particulière est portée sur les phases stationnaires monolithiques à base de silice. Enfin, une étude approfondie des différentes fonctionnalisations de ces monolithes de silice met en évidence l’intérêt porté aux monolithes de silice hybrides en termes de simplification du protocole de synthèse. La partie expérimentale est ainsi axée sur le développement et la caractérisation de ces monolithes de silice hybrides dédiés à la chromatographie à polarités de phases inversée. Dans un premier temps, la synthèse de monolithes de silice hybrides C3 illustre la possibilité de synthétiser par voie sol-gel (100% aqueux) un monolithe de silice fonctionnalisé et performant en une seule étape (« one pot »). Dans un second temps, ce type de procédé est employé et optimisé afin de synthétiser des capillaires monolithiques de silice hybrides C8 présentant des performances équivalentes à leurs homologues C8 préparés en deux étapes (synthèse puis greffage) et comparables à des colonnes particulaires (d particules 5 μm)This manuscript is dedicated to the synthesis (via sol-gel process) and caracterization of hybrid monolithic silica for miniaturized separation techniques : nano-liquid chromatography (nano-LC), capillary electrochromatography (CEC) and microchips. The bibliography part deals with the recent axis of development of these separatives techniques : increase of efficiency per time unit, increase of peak capacity and miniaturisation of these techniques. After an overview of this evolution, the manuscript is focused on the silica monolithic stationnary phases. Finally, a detailed study on the different kinds of protocol fonctionnalization of these silica monoliths highlights the advantage of simplifying the synthesis using a single step protocol (« one pot »). The experimental part is also focused on this kind of single step protocol so as to synthesize hybrid silica monoliths dedicated to the reversed phase mode in chromatography. First, the synthesis of hybrid C3 silica monoliths shows the ability to synthesize a functionnalized silica monolith via a single step sol gel process (« one pot »). Then, this kind of process is used and optimized in order to synthesize a hybrid C8 silica monolithic into capillaries. These stationary phases allowed reaching performances similar to those synthesized in two steps (sol-gel process and grafting) and to the particulate columns (5 μm)
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Denofre, Silvia. "Propriedades do oxido de miobio (V) enxertado sobre a superficie da silica gel." [s.n.], 1991. http://repositorio.unicamp.br/jspui/handle/REPOSIP/249844.
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Orientador :Yoshitaka GushikemDissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica
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Mestrado
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Awano, Carlos Miranda [UNESP]. "Preparação e caracterização de sílicas mesoporosas." Universidade Estadual Paulista (UNESP), 2012. http://hdl.handle.net/11449/91874.
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awano_cm_me_rcla.pdf: 1416595 bytes, checksum: b05e63e15fc2c41a54e30a327a12dfff (MD5)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
O presente trabalho tem como um dos objetivos estudar as características estruturais de sílicas mesoporosas ordenadas, funcionalizadas com vários grupos orgânicos (-amino, -epoxi, -fenil, -vinil, -nitrila, -amina) incorporados diretamente no processo de preparação. As sílicas funcionalizadas foram preparadas por precipitação a partir da hidrólise de misturas de tetraetilortosilicato (TEOS) e trialcóxidos de silício, com os específicos grupos funcionais, utilizando o surfactante tri-block poly(etileno óxido)-poly(propileno óxido)-poly(etileno óxido) (Pluronic P123) como direcionador de estrutura. Outro objetivo do trabalho foi preparar géis de sílica a partir da hidrólise ácida do tetraetilortosilicato (TEOS) com adições de diferentes quantidades de P123 e estudamos suas características estruturais em estágios que vão desde o saturado (gel úmido) até os estados secos do gel (aerogel e xerogel). Os aerogéis foram obtidos por secagem à pressão ambiente (APD) (depois de sililação em fase úmida) e por secagem supercrítica (SCD). Os xerogéis foram obtidos por evaporação depois de envelhecimento em solução de NH4OH 0,1 M. As amostras foram caracterizadas principalmente por adsorção de nitrogênio e espalhamento de raios-X a baixo ângulo (SAXS). As sílicas mesoporosas funcionalizadas apresentam estrutura ordenada hexagonal de poros cilíndricos, com diâmetro de poro de cerca de 8 nm e parâmetro de rede da base hexagonal da estrutura de cerca de 11 nm, valores aproximadamente independentes do grupo de funcionalização. A superfície específica (SBET), o volume (Vp) e o tamanho médio (lp) de poros aumentam, enquanto o tamanho médio das partículas (ls) de sílica diminui com as adições dos trialcóxidos, com relação aos valores da sílica ordenada derivada do TEOS puro. Isto significa que além da estrutura...
One of the aims of this work was to study the structural characteristics of ordered mesoporous silicas, functionalized with various organic groups (-amino, -epoxy, -phenyl, -vinyl, -nitrile- and -amine) incorporated directly in the preparation process. The functionalized silicas were prepared by precipitation from the hydrolysis of mixtures of tetraethoxysilane (TEOS) and trialkoxysilanes, with specific functional groups, using the surfactant tri-block poly (ethylene oxide)-poly (propylene oxide)-poly (ethylene oxide) (P123 PLURONIC) as a structure-directing agent. Another objective was to prepare silica gels from acid hydrolysis of tetraethoxysilane (TEOS) with additions of different amounts of P123 and study their structural characteristics in stages ranging from the saturated (wet gel) to the dry stages of the gels (aerogels and xerogels). Aerogels were obtained by ambient pressure drying (APD) (after silylation process) and supercritical drying (SCD). Xerogels were obtained by evaporation after aging in a solution of 0.1 M NH4OH. The samples were characterized by nitrogen adsorption and small angle X-ray scattering (SAXS). The functionalized mesoporous silicas have ordered hexagonal structure with cylindrical pores, with pore diameter of about 8 nm and lattice parameter of the hexagonal structure with about 11 nm; these values being approximately independent of the functionalization group. The specific surface area (SBET), the volume (Vp) and the size (lp) of pores increase, while the silica particle size (ls) decreases with additions of trialkoxysilanes, when compared to values of ordered silica derived from pure TEOS. This means that in addition to that hexagonal pore structure it also arises in the functionalized silicas microscopic pores (by the increase of SBET and decrease of ls) and larger pores than those... (Complete abstract click electronic access below)
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Awano, Carlos Miranda. "Preparação e caracterização de sílicas mesoporosas /." Rio Claro : [s.n.], 2012. http://hdl.handle.net/11449/91874.
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Orientador: Dimas Roberto VolletBanca: Dario Antonio Donatti
Banca: Dermeval José Mazzini Sartori
Resumo: O presente trabalho tem como um dos objetivos estudar as características estruturais de sílicas mesoporosas ordenadas, funcionalizadas com vários grupos orgânicos (-amino, -epoxi, -fenil, -vinil, -nitrila, -amina) incorporados diretamente no processo de preparação. As sílicas funcionalizadas foram preparadas por precipitação a partir da hidrólise de misturas de tetraetilortosilicato (TEOS) e trialcóxidos de silício, com os específicos grupos funcionais, utilizando o surfactante tri-block poly(etileno óxido)-poly(propileno óxido)-poly(etileno óxido) (Pluronic P123) como direcionador de estrutura. Outro objetivo do trabalho foi preparar géis de sílica a partir da hidrólise ácida do tetraetilortosilicato (TEOS) com adições de diferentes quantidades de P123 e estudamos suas características estruturais em estágios que vão desde o saturado (gel úmido) até os estados secos do gel (aerogel e xerogel). Os aerogéis foram obtidos por secagem à pressão ambiente (APD) (depois de sililação em fase úmida) e por secagem supercrítica (SCD). Os xerogéis foram obtidos por evaporação depois de envelhecimento em solução de NH4OH 0,1 M. As amostras foram caracterizadas principalmente por adsorção de nitrogênio e espalhamento de raios-X a baixo ângulo (SAXS). As sílicas mesoporosas funcionalizadas apresentam estrutura ordenada hexagonal de poros cilíndricos, com diâmetro de poro de cerca de 8 nm e parâmetro de rede da base hexagonal da estrutura de cerca de 11 nm, valores aproximadamente independentes do grupo de funcionalização. A superfície específica (SBET), o volume (Vp) e o tamanho médio (lp) de poros aumentam, enquanto o tamanho médio das partículas (ls) de sílica diminui com as adições dos trialcóxidos, com relação aos valores da sílica ordenada derivada do TEOS puro. Isto significa que além da estrutura... (Resumo completo, clicar acesso eletrônico abaixo)
Abstract: One of the aims of this work was to study the structural characteristics of ordered mesoporous silicas, functionalized with various organic groups (-amino, -epoxy, -phenyl, -vinyl, -nitrile- and -amine) incorporated directly in the preparation process. The functionalized silicas were prepared by precipitation from the hydrolysis of mixtures of tetraethoxysilane (TEOS) and trialkoxysilanes, with specific functional groups, using the surfactant tri-block poly (ethylene oxide)-poly (propylene oxide)-poly (ethylene oxide) (P123 PLURONIC) as a structure-directing agent. Another objective was to prepare silica gels from acid hydrolysis of tetraethoxysilane (TEOS) with additions of different amounts of P123 and study their structural characteristics in stages ranging from the saturated (wet gel) to the dry stages of the gels (aerogels and xerogels). Aerogels were obtained by ambient pressure drying (APD) (after silylation process) and supercritical drying (SCD). Xerogels were obtained by evaporation after aging in a solution of 0.1 M NH4OH. The samples were characterized by nitrogen adsorption and small angle X-ray scattering (SAXS). The functionalized mesoporous silicas have ordered hexagonal structure with cylindrical pores, with pore diameter of about 8 nm and lattice parameter of the hexagonal structure with about 11 nm; these values being approximately independent of the functionalization group. The specific surface area (SBET), the volume (Vp) and the size (lp) of pores increase, while the silica particle size (ls) decreases with additions of trialkoxysilanes, when compared to values of ordered silica derived from pure TEOS. This means that in addition to that hexagonal pore structure it also arises in the functionalized silicas microscopic pores (by the increase of SBET and decrease of ls) and larger pores than those... (Complete abstract click electronic access below)
Mestre
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Winkler, Robert. "Developement of an "all-in-one" approach for the synthesis of silica-based hybrid materials." Thesis, Montpellier, 2019. http://www.theses.fr/2019MONTS075.
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Ce travail de thèse porte sur la synthèse de nouveaux précurseurs d'organosilane et leur utilisation dans des matériaux hybrides à base de silice par une approche tout-en-un pour l'extraction de terres rares.Pour atteindre cet objectif, cinq précurseurs d'organosilane ont été synthétisés avec un bon rendement. Premièrement, ces nouveaux précurseurs ont été utilisés pour élaborer des matériaux hybrides à base de silice dense (SHM). La caractérisation de la structure locale par FTIR et de la mésostructure par SAXS du SHM final a permis de mettre en évidence le lien entre les interactions chimiques et physiques entre les groupes fonctionnels des précurseurs et les autres espèces présentes dans le mélange réactionnel qui déterminent la connectivité locale du réseau siloxane et la mésostructure des matériaux obtenus (phases lamellaire et hexagonale 2D). Deuxièmement, afin d'améliorer les propriétés du matériau, une approche innovante en deux étapes a été proposée. La première étape est basée sur la structuration de mélanges binaires alcool/eau afin d’influencer le comportement à l’agrégation des nanoparticules de silice préparé à partir de tétraéthyl orthosilicate. Ainsi, une surface spécifique remarquable de 2000 m² g-1 a pu être obtenue. Dans une seconde étape, les conditions de réaction conduisant aux matériaux ayant la plus grande surface spécifique ont été utilisées avec l’addition d’un précurseur d’organosilane synthétisé ne présentant pas de groupe fonctionnel générant de forte interaction physico-chimique. Les résultats montrent le potentiel de cette approche pour adapter les propriétés des matériaux obtenus. Enfin, les SHM synthétisés à partir de précurseurs d'organosilane purs ont été testés avec succès pour l'extraction sélective et efficace d'éléments tel que des terres rares présents dans un lixiviat modèle d’aimant NdFeB.Ces travaux offrent des perspectives prometteuses pour la synthèse « tout-en-un » de SHM à applications directesIn this work, we investigated the synthesis of new organosilane precursors and their polymerization to silica hybrid materials with REE extracting properties via an all-in-one approach.To reach this goal, five organosilane precursors were synthetized in good yield. First, these new precursors were used to elaborate dense silica hybrid materials (SHM). The characterization of the local structure by FTIR and of the mesostructure by SAXS of the SHMs highlighted the link between the chemical and physical interactions between the headgroups of the precursors and the others species existing in the reaction mixture. These interactions drive the local connectivity of the siloxane network and the mesostructure of the obtained materials (lamellar and 2D hexagonal phases). Second, in order to improve the material properties, an innovative approach in two steps was proposed. The first step was based on the structuring of binary alcohol/water mixtures to influence the aggregation behavior of silica nanoparticles prepared from tetraethyl orthosilicate (TEOS). Here, a remarkable specific surface area of 2000 m2 g-1 was achieved. In a second step, the reaction conditions that lead to materials with the highest specific surface area were used in combination with the synthesized organosilane precursors. The results show the potential of this approach to tailor the properties of the obtained materials. Finally, the SHMs synthesized from the pure organosilane precursors were successfully tested for the selective and efficient extraction of rare earth elements present in a simulated leachate of NdFeB magnets.This work offers promising prospects for the "all-in-one" synthesis of SHMs with direct applications
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Pike, James Stephen. "Sol-gel derived boro-siolicate coatings to impede the devitrification of vitreous silica." Thesis, Georgia Institute of Technology, 1987. http://hdl.handle.net/1853/10006.
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Aubonnet, Severine. "Structural and preparative studies of doped silica glasses." Thesis, Nottingham Trent University, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.297723.
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Göbel, Ronald. "Hybridmaterialien aus mesoporösen Silica und ionischen Flüssigkeiten." Phd thesis, Universität Potsdam, 2011. http://opus.kobv.de/ubp/volltexte/2011/5402/.
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Die vorliegende Arbeit beschäftigt sich mit der Synthese und Charakterisierung mesoporöser monolithischer Silica und deren Hybridmaterialien mit Ionischen Flüssigkeiten (ILs, ionic liquids). Zur Synthese der Silicaproben wurde ein Sol-Gel-Verfahren, ausgehend von einer Präkursorverbindung wie Tetramethylorthosilicat angewendet. Der Katalysator mit der geringsten Basizität führte zum Material mit der kleinsten Porengröße und der größten spezifischen Oberfläche.
Eine Kombination von porösen Silica mit ILs führt zur Materialklasse der Silica-Ionogele. Diese Hybridmaterialien verbinden die Eigenschaften eines porösen Festkörpers mit denen einer IL (Leitfähigkeit, weites elektrochemisches Fenster, gute thermische Stabilität) und bieten vielfältige Einsatzmöglichkeiten z.B. in der Katalyse- Solar- und Sensortechnik. Um diese Materialien für ihren Verwendungszweck zu optimieren, bedarf es deren umfassenden Charakterisierung. Daher wurde in der vorliegenden Arbeit das thermische Verhalten von Silica-Ionogelen unter Verwendung verschiedener 1-Ethyl-3-methylimidazolium [Emim]-basierter ILs untersucht. Interessanterweise zeigen die untersuchten ILs deutliche Änderungen in ihrem thermischen Verhalten, wenn diese in porösen Materialien eingeschlossen werden (Confinement). Während sich die untersuchten reinen ILs durch klar unterscheidbare Phasenübergänge auszeichnen, konnten für die entsprechenden Hybridmaterialien deutlich schwächer ausgeprägte Übergänge beobachtet werden. Einzelne Phasenübergänge wurden unterdrückt (Glas- und Kristallisationsübergänge), während z.B. Schmelzübergänge in verbreiterten Temperaturbereichen, zum Teil als einzeln getrennte Schmelzpeaks beobachtet wurden. Diese Untersuchungen belegen deutliche Eigenschaftsänderungen der ILs in eingeschränkten Geometrien. Über Festkörper-NMR-Spektroskopie konnte außerdem gezeigt werden, daß die ILs in den mesoporösen Silicamaterialien eine unerwartet hohe Mobilität aufweisen. Die ILs können als quasi-flüssig bezeichnet werden und zeigen die nach bestem Wissen höchste Mobilität, die bisher für vergleichbare Hybridmaterialien beobachtet wurde.
Durch Verwendung von funktionalisierten Präkursoren, sowie der Wahl der Reaktionsbedingungen, kann die Oberfläche der Silicamaterialien chemisch funktionalisiert werden und damit die Materialeigenschaften in der gewünschten Weise beeinflußt werden. In der vorliegenden Arbeit wurde der Einfluß der Oberflächenfunktionalität auf das thermische Verhalten hin untersucht. Dazu wurden zwei verschiedene Möglichkeiten der Funktionalisierung angewendet und miteinander verglichen. Bei der in-situ-Funktionalisierung wird die chemische Funktionalität während der Sol-Gel-Synthese über ein entsprechend funktionalisiertes Silan mit in das Silicamaterial einkondensiert. Eine postsynthetische Funktionalisierung erfolgt durch Reaktion der Endgruppen eines Silicamaterials mit geeigneten Reaktionspartnern. Um den Einfluß der physikalischen Eigenschaften der Probe auf die Reaktion zu untersuchen, wurden pulverisierte und monolithische Silicamaterialien miteinander verglichen. Im letzten Teil der Arbeit wurde die Vielfältigkeit, mit der Silicamaterialien postsynthetisch funktionalisiert werden können demonstriert.
Durch die Kenntnis von Struktur-Eigenschaftsbeziehungen können die Eigenschaften von Silica-Ionogelen durch die geeignete Kombination von fester und mobiler Phase in der gewünschten Weise verändert werden. Die vorliegende Arbeit soll einen Beitrag zur Untersuchung dieser Beziehungen leisten, um das Potential dieser interessanten Materialien für Anwendungen nutzen zu können.This work describes the synthesis and characterization of mesoporous monolithic silica and its hybrid materials with ionic liquids (ILs). For synthesis of the silica samples a sol-gel method was used. The catalyst with the weakest basicity leads to the material with the smallest pore size and the largest specific surface area. Combination of porous silica with ILs yields silica-ionogels. These hybrid materials combine the properties of porous solids with the properties of ILs (which is e.g. high conductivity, wide electrochemical stability window, and good thermal stability) and therefore offer a variety of possible applications like catalysis, solar and sensing. To optimize these materials for specific applications there is a need to understand their structure-composition-property relations. For this reason the thermal behavior of silica-ionogels was studied using different 1-ethyl-3-methylimidazolium [Emim]-based ILs. Interestingly the ILs show a clear change in their thermal behavior upon confinement in porous silica. Whereas the pure ILs show distinct phase transitions, the hybrid materials exhibit considerably weaker phase transitions. Phase transitions are suppressed (glass- and crystallization phase transitions); melting transitions show multiple melting peaks. Furthermore solid-state NMR also shows that ILs in mesoporous silica exhibit unusual high mobility. The confined ILs can therefore be classified as quasi-liquid and represents to our best knowledge the highest mobility observed so far in ionogels. By using functionalized silane precursors and different reaction conditions the silica surface was chemically functionalized which further changes the material properties. In a final approach a post-synthetic functionalization was performed by reaction of the selected groups of a silica material with suitable reactants. To study the effect of the physical appearance on the characteristics of the final material, powdered and monolithic samples were studied. In the last part of the work the versatility of post-synthetic silica functionalization was demonstrated. The current work contributes to a better understanding of structure-property correlations, to improve the potential of these interesting materials for possible applications.
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Rodrigues, Filho Ubirajara Pereira. "Sintese e caracterização de complexos de pentacianoferrato (II) na superficie da silica gel organomodificada." [s.n.], 1992. http://repositorio.unicamp.br/jspui/handle/REPOSIP/249712.
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Orientadores : Yoshitaka Gushikem, Eduardo StadlerDissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica
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Santos, Junior Luiz de Souza. "Interação de sitios acidos da silica gel com algumas bases organicas." [s.n.], 1985. http://repositorio.unicamp.br/jspui/handle/REPOSIP/250030.
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Orientador : Claudio AiroldiDissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica
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Abbas, Bassam. "Linear and nonlinear optical phenomena in thin sol-gel organic-inorganic films." Thesis, University of Reading, 1999. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.298744.
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Saravanamuttu, Kalaichelvi. "Photo-induced structural transformation in sol-gel derived silica-methacrylate composites." Thesis, McGill University, 2000. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=38093.
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We describe our investigations into photochemical and micro-structural characteristics of sol-gel derived silica-methacrylate composites (SAC). Upon irradiation with UV light, thin SAC films undergo spatially localised increases of the index of refraction, a macroscopic property that has been used in the photo-lithography of passive integrated optics devices. Our spectroscopic studies indicate that UV initiated free-radical polymerisation of methacrylate substituents trigger further growth and densification of the silica host. This advances our molecular level understanding of photo-reactions in hybrid organo-silica networks.We examine laser-initiated organic chain growth in SAC planar waveguides. Optical modes initiate polymerisation of methacrylate substituents along the propagation path. In turn, the nascent reaction medium presents a non-uniform refractive index profile to the guided laser beam. Spatially localised and intensity-dependent refractive index changes create a lens-like profile in the medium. As a result, the beam self-focuses along its propagation axis without diffraction.
We describe oriented organic chain growth in the nonlinear optical and highly anisotropic reaction field provided by a linearly polarised, self-focusing laser beam. A self-focusing laser beam induces an anisotropy in the refractive index profile of SAC waveguides. We characterise laser-induced birefringence in the hybrid network through polarised waveguide Raman spectroscopy and optical birefringence measurements.
Long-range periodic self-organisation in sol-gel derived silica acrylate composites formed in the absence of external templates was observed for the first time. Significantly, the periodicity associated with this structure is approximately 200 nm, approaching the optical wavelength regime.
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Skipper, Laura. "The atomic scale structure of bioactive calcia : silica sol-gel glasses." Thesis, University of Kent, 2006. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.443757.
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Rezk, Ahmed Rezk Masoud. "Theoretical and experimental investigation of silica gel/water adsorption refrigeration systems." Thesis, University of Birmingham, 2012. http://etheses.bham.ac.uk//id/eprint/3623/.
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This PhD project was set out to improve the performance of silica gel / water adsorption cooling systems using a number of investigation tools. A novel global lumped analytical simulation model has been constructed for a commercialised two-bed silica gel / water 450kW adsorption chiller. It was integrated with a genetic algorithm (GA) optimisation toolbox to determine the optimum operating conditions to obtain the optimum chiller performance. The model was used to investigate the effect of physical and operating on the chiller performance. The model was also used to investigate the effect of various adsorbent bed enhancement techniques that are presented in published literature. An experimental test facility has been designed, constructed and commissioned to study the performance of scaled down adsorbent bed modules. It has been constructed to understand the effect of the operating conditions on adsorbent-bed heat and mass transfer performance. A dynamic vapour sorption (DVS) gravimetric analyser has been used to characterise a new species of adsorbents (MOFs). These adsorbents have strong potential towards water sorption and could replace the currently applied silica gel. MOFs adsorbents have been characterised in terms of adsorption isotherms and kinetics, in addition to its cyclic analysis. It was found that HKUST-1 (copper based MOF) outperforms silica gel with 95.7% increase in the water uptake. Iron based MOF (MIL-100) was found to outperform silica gel for high evaporating temperature application.
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Caggiano, Lorenzo. "Silica gel induced episulfonium ion formation and capture with internal nucleophiles." Thesis, University of Cambridge, 2002. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.620471.
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Rincon, Guillermo J. "Photocatalytic Mineralization of Phenol on Fluidized Titanium Oxide-Coated Silica Gel." ScholarWorks@UNO, 2015. http://scholarworks.uno.edu/td/2009.
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A bench-scale tubular reactor with recirculation was built in order to study the efficiency of the photocatalytic oxidation of phenol on fluidized titanium oxide-coated silica gel beads. A UV-C lamp placed along the central vertical axes of the reactor was used as source of photons. A bed of silica gel beads was fluidized by means of fluid recirculation and forced to follow upward helical flow around the lamp. Anatase was successfully synthetized on silica gel particles of average diameters 224, 357 and 461 µm, as confirmed by scanning electron micrographs, through a sol-gel technique using a titanium (iv)isopropoxide / hydrochloric acid / ethanol precursor.
Data was obtained from multiple 8-hours photocatalytic experiments using a determined mass of beads fluidized in an aqueous solution of known initial phenol concentration. Contaminant degradation with irradiation time was measured as COD. Beads that had been subjected to three consecutive coating procedures produced an 8-h removal efficiency 10% higher than beads with a single coat. 20 g L-1 of silica beads was found to be the optimum load for the experimental reactor configuration regardless of beads size, although efficiency increased with decreasing size of the latter.
Experimental results confirmed that the efficiency of phenol photocatalytic degradation decreases with increasing pollutant concentration. Also, the highest removal was achieved with initial pH 3, and it decreased with increasing pH. When NaCl was added to the solution, COD removal increased with increasing salinity. Additionally, it was found that dissolved oxygen is indispensable for photocatalysis to proceed, and that saturation of the treated mixture with oxygen was effectively achieved by keeping the liquid surface in contact with pure oxygen at 1 atm.
Finally, statistical analysis of the data showed that photocatalytic mineralization of phenol-derived COD under the experimental conditions follows exponential decay. Based on this finding, a correlation model was proposed for the accurate prediction (minimum R2 = 0.9840) of the COD removal efficiency of the reactor for any given initial COD.
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Robertson, Joseph William F. "Fabrication, analysis and patterning of sol-gel based silica ultrathin films." Diss., The University of Arizona, 2004. http://hdl.handle.net/10150/280795.
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A novel approach to sol-gel thin film fabrication has been developed which leads to the production of ultrathin ∼2 nm to 100 nm thick silica and conductively-doped silica films on metal and semiconductor substrates. The research described herein focuses on the development, characterization and potential application of these thin films in current technology. These ultrathin films were fabricated by a sol-gel procedure, which utilized highly diluted silica precursor compounds. The [H₂O]:[Si] ratio ranged from 50 to 1000, far above the typical values (4-10) used in sol-gel film preparation. This dilution leads to highly densified silica when spin-cast onto an appropriately compatible surface. The surface examined included Si(111)/SiO₂; ITO; and 3-(mercaptopropyl)trimethoxysilane (3MPT) modified Au and Ag. These surfaces must act as wetting control agents for the sol-gel precursor, while simultaneously providing adhesion to the nm sized sol-gel aggregates. The 3MPT-Ag monolayer was examined in detail by Tl, Pb and Cd underpotential deposition electrochemistry, to understand the interfacial structure of the molecule. These results show that the 3MPT monolayer is very stable to outside influences (i.e. Tl and Pb reversibly deposit monolayers at the metal surface). The UPD of metal ions is highly size dependent with Tl depositing with fewer kinetic limitations than Pb and Cd not depositing at all. Raman spectral characterization shows that 3MPT undergoes some reversible rearrangement during the UPD process. The electronic properties of the pure silica films were examined in great detail. The results suggested that in solution, a solvated gel layer at the film-solution interface gives rise to an anomalously low capacitance <100 pF/cm², which has no comparison in the current literature. In the dry state, these silica films have a dielectric constant of ε = 3.5, which is close to that of thermally-grown silica on silicon (3.9). These films were doped with 1,1'-bistriethoxysilylferrocene, an electrochemically-active sol-gel material. The results suggest that under the proper precursor solution conditions, thin ( <10 nm), uniform films can be fabricated. By simply adjusting the ratio of the ferrocene moiety in solution, the film composition can be adjusted. XPS verifies that the atom ratio in solution is near to the observed atom ratio in the films, with some indication of surface segregation of the ferrocene moiety. Electrochemical analysis of these films suggests that electron hopping between the ferrocene centers drives the electrochemical response only when there are pinhole defects, to support counterion conduction to the surface. (Abstract shortened by UMI.)
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Dodd, Brandon M. "Experimental Evaluation of Uranyl Transport into Mesoporous Silica Gel using Fluorescence." VCU Scholars Compass, 2018. https://scholarscompass.vcu.edu/etd/5336.
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This research investigated parameters that can affect the use of nanoporous silica gel as a media for accumulating a detectable amount of uranium. The unique fluorescence of the Uranyl (UO22+) ion was used to evaluate the transport kinetics and accumulation within silica gel in a static fluid and under pressure driven flow. The addition of fluid flow decreased the time constant from on the order of an hour to approximately 2s with a very low fluid velocity of 0.36cm/s. The 0.36cm/s fluid velocity was found to be the critical velocity above which there was no gain in time constant. A table top instrument was developed that can detect trace amounts of uranium in solution. The table top instrument was used to investigate how the time constant depends on the uranyl concentration, which led to the development of a new time-based method for quantifying the uranyl concentration. The time-based method of detection uses a preset threshold and, based on the time it takes to reach that threshold, the concentration in the water sample can be determined. The lifetime of uranyl in complex with silica increased to approximately 120us, allowing for gated detection and background discrimination. In addition to the fluorescent contaminants, competing cations were tested to determine how they affect the fluorescence and transport kinetics of the uranyl. The cations tested were Mn2+, Ca2+, Mg2+, Na+, K+, and Li+. The result shows that within the natural concentrations, Mg2+, Na+, and K+ did quench the fluorescent of the uranyl ions by collision quenching. The time constant was also examined in the presence of each cation and showed that Ca2+, Mg2+, Na+, and K+ decreased the adsorption time constant. Future studies in this area should be directed toward the development of a portable version of the instrument.
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Póvoas, Pamela Luiza de Souza Tavares. "Nanopartículas de sílica da família SBAn: síntese, funcionalização, caracterização e efeito da morfologia na adsorção de lipase." CNEN - Centro de Desenvolvimento da Tecnologia Nuclear, Belo Horizonte, 2014. http://www.bdtd.cdtn.br//tde_busca/arquivo.php?codArquivo=314.
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Conselho Nacional de Desenvolvimento Científico e TecnológicoMateriais mesoporosos têm despertado um interesse cada vez maior na comunidade científica, devido à singularidade das suas propriedades, o que os tornam materiais promissores para serem empregados em processos de adsorção, catálise, nanotecnologia e aplicações eletrônicas. Dentre os diversos materiais da série de sílica mesoporosa, destaca-se a família SBAn. Os materiais SBA-16 e SBA-15 se sobressaem em diversos estudos devido às suas diferentes morfologias, tamanho de poros uniformes, elevada área superficial e elevada densidade de grupos silanois na sua superfície. Estas características conferem aos materiais a possibilidade de modificação superficial e imobilização de diversos agentes tais como enzimas para aplicação em biocatálise. O desenvolvimento de técnicas de imobilização de enzimas em nanopartículas de sílica SBAn pode resultar em melhorias do seu desempenho catalítico, reduzir a sua inativação e melhorar a retenção da atividade catalítica por um maior período de tempo. No presente trabalho, diferentes tipos de nanopartículas de sílica SBAn foram sintetizadas e funcionalizadas com 3-amino-propil-triethoxysilane (APTES). As amostras foram caracterizadas por técnicas de Espectroscopia na Região do Infravermelho com Transformada de Fourier (FTIR), Adsorção de Nitrogênio (BET), Microscopia Eletrônica de Varredura (MEV), Microscopia Eletrônica de Transmissão (TEM), Espalhamento de Raios X a Baixos Ângulos (SAXS), Análise Elementar (CHN) e Análise Termogravimétrica (TG). Foi avaliado o processo de imobilização de lipase de pâncreas do porco (PPL) por adsorção nos suportes sólidos das diferentes nanopartículas de SBAn puras e funcionalizadas, através de reação de hidrólise com o substrato caprilato p-nitrofenila determinados através da técnica de UV-Vis. Foram investigados os diferentes tipos de sílica SBAn e a influência da morfologia no processo de imobilização de lipase (PPL). Os resultados mostraram que a enzima (PPL) foi imobilizada com sucesso em canais de SBAn mesoporosos e que amostra tem um grande potencial para aplicações em biotecnologia.
Mesoporous materials have attracted an increasing interest in the scientific community because of the uniqueness of their properties, which make them promising materials to be employed in the process of adsorption, catalysis, nanotechnology, electronics applications. The mesoporous materials may be chemically manipulated by varying the surfactant and some parameters such as temperature and concentration of the synthesis, which influence the morphology and particle size. Many studies have been developed in the creation of stable materials with well-defined arrangements hexagonal, cubic, lamellar and tetragonal. Among the various materials, the series family of mesoporous silica, highlight the SBAn. These materials are very attractive due to its properties, such as high surface areas and a uniform mesopore size with ordered pore size distribution and readily controlled. The SBA-16 and SBA-15 materials stand out due to their different morphologies and wide application. In this study, different types of nano-silica particles SBAn were synthesized and functionalized with 3-amino-propyl-triethoxysilane (APTES). The samples were characterized by techniques of Fourier Transform Infrared (FTIR), nitrogen adsorption (BET), scanning electron microscopy (SEM), Transmission Electron Microscopy (TEM), Small Angle X- Ray Scattering (SAXS), Elemental Analysis (CHN) and Thermogravimetric Analysis (TG). The immobilization process by adsorption on solid support matrices SBAn silica nanoparticles by hydrolysis reaction with the substrate p-nitropheniyl caprylate determined by UV-VIS technique was evaluated. The different types of silica SBAn and its influence on morphology and functionalization in the process of immobilization of PPL were investigated. The results showed that the enzyme porcine pancreatic lipase (PPL) was successfully immobilized on mesoporous SBAn channels.
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Hamderi, Murat Gallagher Patricia M. "Pilot-scale modeling of colloidal silica delivery to liquefiable sands /." Philadelphia, Pa. : Drexel University, 2010. http://hdl.handle.net/1860/3285.
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Long, Theresa A. "Sol-gel routes for surface/sheath structures on carbon fibers : exploratory experiments with silica." Thesis, Georgia Institute of Technology, 1987. http://hdl.handle.net/1853/11792.
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Oliveira, Fernando Jose Volpi Eusebio de. "Organofuncionalização de silica e filossilicato a partir de agentes sililantes incoporados com tioureia." [s.n.], 2006. http://repositorio.unicamp.br/jspui/handle/REPOSIP/250046.
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Orientador: Claudio AiroldiDissertação (mestrado) - Universidade Estadual de Campinas, Instituto de Quimica
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Resumo: Novas matrizes de sílica gel organofuncionalizadas foram preparadas através da incorporação da molécula de tiouréia nos agentes sililantes comerciais de cadeias lineares contendo de um a três átomos de nitrogênio em suas estruturas, na presença de sulfato de amônio, como catalisador. Utilizou-se um novo método de preparação do novo agente modificado não envolvendo a presença de solvente na etapa inicial, o que difere daqueles que usam algum tipo de solvente orgânico, não só na etapa inicial, como também em reações sucessivas de imobilização. As matrizes foram denominadas conforme o número de nitrogênios contidos em suas superfícies, sendo S-NT, S-2NT e S-3NT, de acordo com os crescentes átomos de nitrogênio contidos no agente de origem. Através do processo sol-gel foram sintetizados os filossilicatos correspondentes às superfícies de sílica modificada. Nessa etapa, os agentes incorporados com tiouréia foram dissolvidos em etanol e adicionados a uma solução de nitrato de níquel em meio básico, obedecendo a relação molar Si/Ni como sendo 4/3. Assim, foram obtidos filossilicatos similares ao talco, que apresenta o magnésio nos sítios octaédricos, envoltos por duas camadas de silicato, onde o silício está acomodado nos sítios tetraédricos. Para a síntese da estrutura similar ao talco natural é fundamental que a razão molar mencionada seja obedecida. As técnicas de caracterização utilizadas permitiram a compreensão das estruturas, bem como algumas de suas propriedades. Para os filossilicatos, foi fundamental a análise por difração de raios-X, para observar os planos de reflexões correspondentes aos da amostra de estruturas do tipo talco e comparar os sinais e as distâncias interlamelares de todos os materiais. A capacidade de adsorção de íons cobre foi estudada para as três matrizes de sílica. Os materiais apresentaram capacidade máxima de adsorção crescente na seguinte ordem. S2NT < SNT < S-3NT, ou seja, a matriz contendo dois átomos de nitrogênio em sua estrutura apresentou menor capacidade, que por sua vez é menor do que a matriz contendo três átomos de nitrogênio nas cadeias. Esse resultado está de acordo com os percentuais de nitrogênio para cada amostra, calculados pela análise elementar. A energética da interação íons cobre/centros básicos de Lewis foi determinada por titulação calorimétrica. Os dados permitiram obter a isoterma de Langmuir e através de sua regressão linear, calcular os parâmetros termodinâmicos que se apresentaram favoráveis à complexação do cobre.
Abstract: New silica gel organofunctionalized surfaces were synthesized by incorporating the thiourea molecule in the commercial silylanting agents with linear chains containing from one to three nitrogen atoms on their structures, in presence of ammonium sulphate as catalyst. This method for new modified silylating agent preparation does not require any solvent for the first step reaction. The most usefull described processes are based on the use of solvent not only on the first step, but also on the immobilization reactions. The materiaIs were named following to the number of nitrogen atoms attached to the aliphatic organic chains containing on surfaces, as S-NT, S-2NT and S-3NT, from one to three nitrogen atoms derived from silylating agents, respectively. From sol-gel process the analogous phyllosilicates from modified silica surfaces were synthesized. In this step, the functionalized agent was dissolved in ethanol and added to a nickel nitrate solution, in basic condition, following the molar ratio Si/Ni as 4/3. Therefore, the obtained talc-like phyllosilicate, presented the magnesium atom in octahedral sites, which are located between two tetrahedral silicate layers. To synthesize a talc-like structure, the mentioned molar ratio must be obeyed. The characterization techniques allowed the understanding of the structures, as well as some of properties. For phyllosilicates, the X-ray diffraction patterns were of fundamental importance for observing the typical reflection plans associated with the samples that have a talc-like structure and to compare the signals and the interlamellar space for all materials. The copper adsorption capacity was studied for alI three silica matrices. The materials presented an increasing order of adsorption capacity as: S-2NT < SNT < S-3NT, e.g., the matrix containing two nitrogen atoms on its structure had lower capacity than the others, including that one of three nitrogen atoms. These data are in agreement with nitrogen percentage values for each sample, evaluated by elemental analysis. The energetic of the interactions between copper ions/nitrogen Lewis basic centers were followed by calorimetry. Through calorimetric titrations was possible to adjust the results to the Langmuir isotherm and by linear regression and the thermodynamic parameters were calculated and presented favorable for copper complexation.
Mestrado
Quimica Inorganica
Mestre em Química
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Lin, Yuanzhi Gallagher Patricia M. "Colloidal silica transport mechanisms for passive site stabilization of liquefiable soils /." Philadelphia, Pa. : Drexel University, 2006. http://hdl.handle.net/1860/1162.
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Fardad, Mohammad Ali. "Fabrication of sol-gel silica-on-silicon waveguides doped with semiconductor quantum dots for integrated optics." Thesis, Imperial College London, 1995. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.307565.
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Lima, Samantha Pinheiro Buás de. "Estudo da Produção e Aplicação em Pastas Cimentícias de Sílica Gel Proveniente das Cinzas da Casca do Arroz." Universidade Federal do Amazonas, 2009. http://tede.ufam.edu.br/handle/tede/3483.
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Previous issue date: 2009-05-18Fundação de Amparo à Pesquisa do Estado do Amazonas
The experimental program of this research was developed in order to evaluate the silica gel performance in cement based pastes. Thus, parameters of silica gel from rice husk ash were studied extraction. The incorporation of silica gel was made by the partial replacement of 0%, 2,5% e 5% of the cement mass in 0,45 water-cementitious material (w/cm) paste, and 0%, 5%, 7% in 0,5 w/cm paste. The silica gel behavior was evaluated based on X- ray diffraction, thermal analysis and compressive strength after 3, 7 and 28 days of curing. The results showed that is possible the production of pastes with excellent mechanical performance from the silica gel application as pozzolan. In particular, the compressive strength of the silica gel paste was about 46% higher than the reference paste. Moreover, there was a decrease of the more than 50% of calcium hydroxide content in the silica gel paste, indicating the pozzolanic activity of the silica gel produced in this work.
O programa experimental realizado no presente projeto foi desenvolvido de forma a avaliar o desempenho da sílica gel em matriz de cimento Portland. Para tal, foram estudados os parâmetros de extração da sílica gel da cinza da casca de arroz. O gel de sílica foi aplicado em pastas como substituto parcial do cimento Portland nos teores de 0%, 2,5% e 5% em massa, para uma relação água-aglomerante de 0,45, e de 0%, 5%, 7% em massa, para uma relação água-aglomerante de 0,50. O comportamento da sílica gel foi avaliado através de ensaios de difração de raios-x, análise térmica e resistência à compressão nas idades de 3, 7 e 28 dias. Os resultados indicaram que é possível a produção de pastas de excelente desempenho mecânico a partir da aplicação de sílica gel como pozolana. Em particular, a sílica gel promoveu um aumento da resistência à compressão de até 46% aos 28 dias e consumiu mais de 50% do hidróxido de cálcio, fato que se atribui a elevada atividade pozolânica da sílica gel.