Thesis (M.Eng.). / Written for the Dept. of Mining, Metals and Materials Engineering. Title from title page of PDF (viewed 2009/06/15). Includes bibliographical references.

L'importance du traitement du signal et la transmission favorise de nouvelles applications pour les matériaux optiques non linéaires, tels que des convertisseurs de fréquence. Les cristaux sont des matériaux pour ces applications bien connues en raison de leur comportement non linéaire optique forte. Cependant, ils sont coûteux à fabriquer et dépendent fortement de l'orientation cristalline. Les verres sont des candidats possibles à cause de leurs propriétés optiques et la facilité de fabrication, mais ils ne possèdent pas de second ordre non-linéarité en raison de leur structure centrosymétrique. Cependant, un matériau composite vitrocéramique avec des cristaux ferro-électriques noyées dans une matrice de verre peut combiner les propriétés de cristaux non linéaires avec la facilité de fabrication de lunettes.Germanotellurite verre et la céramique, verre dopés avec différentes quantités d'oxyde d'argent, dans la (100-x) (70TeO2 - 10GeO2 - 10Nb2O5 - 10 - K2O) xAg2O système (x = 0 à 6% en mole), a été étudiée. L'étude se compose de l'élaboration et la caractérisation d'une céramique de verre qui peuvent répondre aux exigences de matériaux optiques non linéaires, avec une grande transparence et une activité non linéaire intense. Les caractéristiques des verres et de la céramique de verre ont été déterminées par analyse thermique, diffraction des rayons X, la microscopie électronique, UV-Vis et spectroscopie Raman. Cristallisation en vrac a été observé pour les verres d'argent dopé avec une phase cristalline unique (Ag, K) [Nb1 / 3Te2 / 3] 2O4.8, qui présente une activité seconde génération harmonique (SHG). Un seul traitement thermique a abouti transparence supérieure à un traitement thermique en 2 étapes avec un premier chauffage à la température de nucléation et un second traitement pour la croissance cristalline. Pour les modes de transmission et XRD UV-Vis similaires, les échantillons de chaleur 1-étape traités ont montré une réponse SHG deux ordres supérieur à la 2-étape.Cette différence d'intensité provient de la taille des domaines à l'intérieur des deux céramiques de verre. Le traitement thermique une étape a été trouvé, de promouvoir micron de taille domaines cristallisés, alors que le traitement thermique en deux étapes a abouti à des tailles de sous-domaine de longueurs d'onde. La réponse macroscopique SHG global a été trouvé pour présenter le comportement dipolaire typique. Ce dipôle nature vient de chaque domaine agissant comme SHG émetteur. Une caractérisation basée sur une technique de micro-Raman / micro-SHG corrélative, qui peut fournir à la fois des informations structurelles et les réponses de SHG locales dans les mêmes régions sub-micron, a été réalisée, ce qui indique que l'organisation de cristallites dans les domaines rend leur réponse SHG indépendante de polarisation de la lumière. Un modèle structural a été proposé pour expliquer la propriété dipolaire général et l'indépendance de la polarisation de la lumière. / The importance of signal processing and transmission promotes new applications for nonlinear optical materials, such as frequency converters. Crystals are well known materials for these applications because of their strong optical nonlinear behaviour. However, they are costly to manufacture and are strongly dependant on crystal orientation. Glasses are possible candidates because of their optical properties and ease of fabrication but they possess no second-order nonlinearity due to their centrosymmetric structure. However, a glass-ceramic composite with ferroelectric crystals embedded in a glass matrix can combine the nonlinear properties of crystals with the easiness of fabrication of glasses.Germanotellurite glass and glass ceramics, doped with different amounts of silver oxide, in the (100-x)(70TeO2 – 10GeO2 – 10Nb2O5 – 10 K2O) – xAg2O (x=0-6 mol%) system, has been studied. The study consists of elaboration and characterization of a glass ceramic that can fulfil the requirements of nonlinear optical materials, with high transparency and intense nonlinear activity. The characteristics of the glasses and glass ceramics were determined by thermal analysis, X-ray diffraction, electron microscopy, UV-Vis and Raman spectroscopies. Bulk crystallization has been observed for the silver-doped glasses with a unique crystal phase, (Ag,K)[Nb1/3Te2/3]2O4.8, which presents second harmonic generation (SHG) activity. A single heat treatment yielded higher transparency than a 2-step heat treatment with a first heating at the nucleation temperature and a second treatment for crystal growth. For similar UV-Vis transmission and XRD patterns, the 1-step heat treated samples showed a two order higher SHG response than the 2-step one.This intensity difference comes from the size of domains within the two glass ceramics. The 1-step heat treatment was found to promote micron sized crystallized domains, while the two step heat treatment yielded sub-wavelength domain sizes. The global SHG macroscopic response was found to present typical dipolar behaviour. This dipole nature comes from each domain acting as SHG emitter. A characterization based on a correlative micro-Raman/micro-SHG technique, which can provide both structural information and local SHG responses within the same sub-micron areas, was performed, indicating that the organization of crystallites inside the domains makes their SHG response independent of light polarization. A structural model has been proposed to explain the general dipolar property and the light polarization independence.

OBJECTIVES: To evaluate the flexural strength of 5 ceramic dental materials and to compare the marginal fit of crowns made with e.max press and a new experimental (EXP) press ceramic. MATERIALS AND METHODS: The materials tested for flexural strength included: E.max press, E.maxCAD, ENAMIC, Experimental press, and Experimental-CAD. Each group (N= 10) was tested using the Instron 5566A using the piston-on-three-balls test. For the crown fit experiment an Ivorine tooth was prepared with a chamfer finish and used as the master die. Wax up crowns were made on the die and pressed with E.max press and the Experimental press. 5 crowns per material were obtained. A similar procedure was used with standard aluminum crown dies. Copings were waxed up and pressed: 3 copings of E.max and 6 copings of EXP. Eight measurements of marginal fit per restoration were obtained with an optical microscope at 200×. The data was analyzed using ANOVA and a post hoc Tukey-HSD test (Significance level = 0.05). RESULTS: Mean and SD Flexural Strength values (MPa) per group were: E.max press: 486.96 (30.42). EXP press 378.16 (88.13). E.maxCAD 493.28 (55.2). EXP-CAD 420.63 (86.05). ENAMIC 157.59 (6.27). Mean and SD values for margin fit per group (Microns) were: E.max press 74 (19). EXP press 65 (19). CONCLUSIONS: E.max press has 28.8% higher FS than EXP press (P=0.0044). ENAMIC had the lower FS (as expected). EXP press had significantly lower marginal gap than E.max press by 12.2%. / 2018-09-28T00:00:00Z

Orientadora: Profa. Dra. Juliana Kelmy Macário de Faria Daguano / Dissertação (mestrado) - Universidade Federal do ABC. Programa de Pós-Graduação em Engenharia Biomédica, 2016. / Alterações associadas ao envelhecimento e algumas doenças podem afetar o controle postural influenciando de maneira negativa a qualidade de vida das pessoas. Há muitos testes que podem ser utilizados para descrever o controle postural do ser humano, entretanto, ainda não há um consenso de quais são os melhores testes a serem empregados durante a avaliação para extrair informações relevantes da condição de equilíbrio do Vitrocerâmicas do sistema Li2O.SiO2, contendo como fase majoritária o dissilicato de lítio, têm sido utilizadas clinicamente como biomateriais quase inertes na área de reparação óssea, devido à boa resistência mecânica, apesar de, por vezes, não apresentarem biocompatibilidade e biofuncionalidade completamente satisfatórias. Assim, vitrocerâmicas bioativas à base de Li2O.SiO2 surgem como uma alternativa promissora. O objetivo deste trabalho é avaliar a biocompatibilidade in vitro de um vidro base e duas vitrocerâmicas ¿ contendo metassilicato de lítio e dissilicato de lítio, visando à aplicação como reparador ósseo. Amostras dos três grupos foram caracterizadas por difração de raios X (DRX). Após análise das fases, os materiais foram submetidos aos testes in vitro de bioatividade e biodegradação, bem como ao de citotoxicidade e de adesão e proliferação em meio celular. O teste de bioatividade avaliou a formação de hidroxiapatita carbonatada (HCA) na superfície dos materiais após imersão em solução simuladora de fluído corpóreo (SBF) por períodos de até 14 dias, com o auxílio da técnica de espectroscopia no infravermelho por transformada de Fourier (FTIR), e o teste de biodegradação foi utilizado para quantificar a liberação de lítio (pela técnica de espectrometria de absorção atômica com chama - FAAS) e a perda de massa do material em solução tampão TRIS-HCl, por períodos de imersão de até 28 dias. Após os diversos períodos de imersão, as amostras foram analisadas por Microscopia Eletrônica de Varredura (MEV). Surpreendentemente, apenas a vitrocerâmica contendo majoritariamente a fase dissilicato de lítio (índice de cristalinidade ~ 79%) se mostrou bioativa após 14 dias de imersão em SBF. Em relação à avaliação da biodegradação, houve maior perda de massa para o vidro após 28 dias, e somente este grupo apresentou a concentração de íons Li+ na solução dentro da faixa considerada tóxica, após 14 dias de imersão em TRIS-HCl. Acerca da citotoxicidade, nenhum dos grupos se mostrou citotóxico. Em relação à adesão e à proliferação celular, o dissilicato de lítio apresentou os melhores resultados, podendo se verificar a formação de matriz mineralizada após 21 dias. Os resultados mostram que dentre os materiais analisados, a vitrocerâmica à base de dissilicato de lítio apresenta grande potencial para uso como biomaterial na área de regeneração óssea. / Glass-ceramics based on Li2O.SiO2 system, containing lithium disilicate as major phase, have already been used clinically as almost inert biomaterials due to good mechanical strength, although sometimes they do not have completely satisfactory biocompatibility and biofunctionality. Therefore, bioactive Li2O.SiO2 glass-ceramics appear as a promising alternative. The aim of this study is to evaluate the in vitro biocompatibility of three experimental groups: a base glass and glass-ceramics - containing lithium metasilicate and lithium disilicate, looking for bone repair. Samples of the three experimental groups were characterized by X-Ray Diffraction (XRD). After analyze the phases, these materials were subjected to in vitro bioactivity and biodegradation tests as well as cytotoxicity and adhesion and proliferation in cellular medium tests. The bioactivity test evaluated the formation of hydroxycarbonate apatite (HCA) on the surface of the material after immersion in Simulated Body Fluid (SBF) for periods up to 14 days with the aid of Fourier Transform Infrared Spectroscopy (FTIR), and the biodegradation test was used to quantify the release of lithium (for Flame Atomic Absorption Spectrometry - FAAS) and the weight loss of the material in TRIS-HCl buffer solution, for periods up to 28 days. After several periods of immersion, the samples were analyzed by Scanning Electron Microscopy (SEM). Surprisingly, only the glass ceramic containing lithium disilicate as majoritary phase (Crystallinity Index ~ 79%) proved to be bioactive after 14 days of immersion in SBF. Regarding the evaluation of biodegradation, there was a greater weight loss for glass after 28 days and only this group showed the concentration of Li+ ions in the solution within the range considered toxic, after 14 days of immersion in TRIS ¿HCl. About the cytotoxicity, none of the groups showed to be cytotoxic. Regarding cellular adhesion and proliferation, the lithium disilicate showed the best results, being able to verify the formation of mineralized matrix after 21 days. The results showed that between the 3 experimantal groups analyzed, the lithium disilicate glass-ceramic have great potencial to be used as biomaterial for bone repair.

Ce travail de thèse porte sur l'étude des verres alumino-silicatés de calcium dopés à l'europium et le processus de leur cristallisation sous forme des vitrocéramiques dans le cadre de la recherche de nouveaux phosphores pour application LED à émission blanche. Nous avons étudié trois échantillons vitreux avec différentes teneurs en silice et avons élaboré des vitrocéramiques cristallisées. La caractérisation des verres et des vitrocéramiques a été réalisée par différentes techniques expérimentales : l'analyse thermique, la diffraction des rayons X et la spectroscopie de diffusion Raman. Les propriétés spectroscopiques de l'ion europium dans les verres et les vitrocéramiques synthétisés ont été étudiées. Le contrôle de la cristallisation des vitrocéramiques GC34 et GC50 par la diffraction des rayons X a permis d'identifier deux phases la mélilite et l'anorthite. Dans le cas de la vitrocéramique GC7, une seule phase alumino-calcique qui est la mayenite est cristallisée majoritairement. L'étude par la spectroscopie de diffusion Raman a permis d'une part, de suivre l'évolution de la cristallisation pendant les traitements thermiques en surface et en profondeur dans l'ensemble des vitrocéramiques. Nous avons montré que le processus de cristallisation a eu lieu en surface des échantillons et correspond typiquement à une nucléation hétérogène. D'autre part, une étude comparative avec des échantillons naturels analogues prise de la base de données RRUFF nous a permis de valider l'ensemble des résultats trouvés. Dans le cas des vitrocéramiques GC34 et GC50, les mesures des spectres d'émission et les durées de vie de l'ion Eu3+ montrent bien son incorporation dans les phases cristallines formées. L'ion Eu3+ tend à occuper seulement les sites Ca2+ (CN= 8) de la mélilite majoritaire dans la vitrocéramique GC34 alors, qu'il tend à s'incorporer dans les sites Ca2+ (CN= 6 et 7) et Ca2+ (CN=8) respectivement, des phases anorthite et mélilite formées dans la vitrocéramique GC50. Ces résultats ont été confirmés par les mesures d'affinement de raies. L'étude des spectres d'émission de l'ion Eu2+ a permis de mettre en évidence une modification de son environnement durant la cristallisation traduite par son incorporation dans les sites Ca2+ après réduction de l'ion Eu3+ pendant les recuits. Dans le cas de la vitrocéramique GC7, les spectres d'émissions et les mesures du déclin de luminescence de l'ion Eu3+ montrent bien que l'ion Eu3+ est incorporé dans la phase mayenite formée. En terme d'application, les mesures des coordonnées trichromatiques suggèrent que la dévitrification des verres semble être une technique efficace permettant d'obtenir de nouveaux matériaux luminophores (LED blanches) à émission intensifiée (cas des vitrocéramiques GC34 et G50) et accordable en modifiant leur composition et l'excitation / This work concerns the study of calcium aluminosilicate glass doped with europium and their process of crystallization as glass-ceramics as part of the search for new phosphors for white LED application. We studied three glass samples with different silica contents and have elaborated crystallized glass-ceramics. Characterization of glasses and glass-ceramics was performed by different experimental techniques: thermal analysis, X-ray diffraction and Raman spectroscopy. The spectroscopic properties of the europium ion in the glass and glass-ceramic synthesized were studied.Control of crystallization of GC34 and GC50 glass-ceramics by X-ray diffraction have been identified two phases, melilite and anorthite. In the case of the GC7 glass-ceramic, a single aluminum calcium phase, mayenite which crystallized predominantly. The study by Raman spectroscopy allowed to follow the evolution of the crystallization during heat treatment in the surface and of glass-ceramics. We have shown that the crystallization process initiate at the surface of the samples and corresponds typically to a heterogeneous nucleation. On the other hand, a comparison with similar natural samples allowed us to validate all the identifications.In the case of GC34 and GC50 glass-ceramics, emission spectra and lifetimes of Eu3+ ion clearly show its incorporation into the new-formed crystalline phases. The Eu3+ ion occupy the Ca2+ sites (CN = 8) in the major mélilite phase of the the GC34 glass-ceramic while, it incorporates the Ca2+ sites (CN = 6 and 7) and Ca2+ (CN = 8) of anorthite and mélilite phases formed in the GC50 glass-ceramic, respectively. These results were confirmed by Fluorescence Line Narrowing (FLN) measurements. The study of emission spectra of the Eu2+ ion allowed highlighting changes during crystallization associated with the reduction of the Eu3+ ions during annealing. In the case of the low silicate GC7 glass-ceramic, emission spectra and lifetimes measurements of the Eu3+ ion show that the Eu3+ ions are incorporated into the mayenite phase. In terms of application, the analyses of the trichromatic coordinates suggest that the glass devitrification appears to be an efficient technique to achieve new white LED phosphor materials with intensified (mainly for GC34 and G50 glass-ceramics) and tunable emission by varying composition and/or excitation

Orientador: Agda Eunice de Souza Albas / Resumo: Neste trabalho, vidro e material vitrocerâmico foram obtidos a partir de uma composição baseada no diagrama ternário SiO2-Al2O3-CaO, utilizando escória de ferro fundido, provenientes de empresas de fundição, e, cal hidratada (comercial). A escória foi caracterizada através de: espectrometria de fluorescência de raios X (FRX), para determinar sua composição química; difratometria de raios X (DRX), para a identificação das fases cristalinas e análise térmica (TG), para evidenciar as reações térmicas associadas à desidratação e decomposição dos compostos presente no material. O vidro foi obtido através do processo de fusão/resfriamento (melt-quenching), fundido na temperatura de 1450°C. Foram caracterizados através de: calorimetria exploratória diferencial (DSC), para determinar as temperaturas de transição vítrea e de cristalização e difratometria de raios X (DRX), para identificar a sua estrutura amorfa. O estudo da cinética de cristalização do vidro foi realizado através de métodos cinéticos não isotérmicos baseados na descrição teórica formulada por Johnson-Mehl-Avrami (JMA). Estes métodos descrevem os processos de nucleação e cristalização utilizando dados provenientes da curva de DSC. O estudo cinético teve início com a obtenção do material vitrocerâmico tratado termicamente à 900ºC por 1,5h e identificação das fases cristalinas formadas, utilizando DRX. Considerando a formação de três fases cristalinas, os parâmetros cinéticos foram determinados a partir dos ajustes dos d... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: In this work, glass and glass-ceramic materials were obtained from a composition based on the ternary diagram SiO2-Al2O3-CaO using cast iron slag from foundry companies and hydrated lime (commercial). The slag was characterized by: X-ray fluorescence (XRF) to determine its chemical composition; X-ray diffractometry (XRD), to the crystalline phases identification and thermal analysis (TG), to show the thermal reactions associated with dehydration and decomposition of the compounds present in the material. The glass was obtained by melt quenching at 1450°C. They were characterized by differential scanning calorimetry (DSC) to determine glass transition and crystallization temperatures and X-ray diffraction (XRD) to identify their amorphous structure. The study of crystallization kinetics was performed by non-isothermal kinetic methods based on the theoretical description formulated by Johnson-Mehl-Avrami (JMA). These methods describe the nucleation and crystallization processes using data from the DSC data. The kinetic study began by obtaining heat-treated glass-ceramic material, at 900ºC for 1.5h, and identifying the crystalline phases formed using XRD. Considering three crystalline phases formation, the kinetic parameters were determined from the DSC data adjustments by the Kissinger, Augis-Bennett, and Matusita and Sakka methods. The best fit resulted in three crystallization peaks. The activation energy (Ea) of the crystallization process was obtained using the Kissinger an... (Complete abstract click electronic access below) / Mestre

Experimental results of damage development in and mechanical response of heat-treated NicaloniCAS-II laminates subjected to monotonic flexure and axial loading and to cyclic tensile loading are reported. The specimens were subjected to post-processing heat treatments at 900°, 1000°, and l100°C in air for 100 hours. Changes at the fiber/matrix interface/interphase due to post-processing heat treatments were also characterized. The combined effect of fiber debonding and transverse matrix cracking in both 90° and 0° plies plays an important role in damage development in [0/90]₄₅ Nicalon/CAS-II laminates, especially in developing the secondary damage modes such as longitudinal matrix cracking and delamination. Frictional wear effects found in cyclically loaded specimens may be responsible for the observed temperature profiles during the intermediate stage of fatigue life. It is also believed that frictional wear is critical to the failure of notch sensitive fibers. Different damage modes such as "brittle" matrix crack propagation and "quasi-brittle" matrix crack propagation were observed in heat-treated specimens. Results obtained from microanalysis using an analytical scanning transmission electron microscope equipped with an energy dispersive spectrometer, and microindentation indicated that the changes of damage and failure modes were directly related to the changes of characteristics at the fiber/matreix interface/interphase. / Ph. D.

Orientador: Marcelo Nalin / Resumo: Sistemas foto-termo-refrativos obtidos a partir de alumino-silicatos dopados com Ce4+, Ag+, Sb3+ e Sn2+ tem sido amplamente estudado nestas últimas década por Glebov e Nikonorov devido a crescente necessidade de desenvolvimento de novos dispositivos que atuem em sistemas ópticos e fotônicos. Estes sistemas produzidos atualmente apresentam índice de refração ~ 1,5 o que limita a observação de efeitos não lineares e transparência na região de baixa energia restrita ao infravermelho próximo. Além disso, como os sistemas atualmente conhecidos são multicomponentes, a compreensão do mecanismo por trás da foto-termo sensibilidade ainda não está completamente elucidada. Neste contexto, a síntese de novas composições de sistemas vítreos, com mecanismos mais simples, com índice de refração mais elevado e transparência na região do infravermelho médio se mostram interessantes pois ampliam as possibilidades de aplicações nas áreas acima citadas. Neste trabalho foram sintetizados e caracterizados vidros foto-termo-refrativos contendo óxidos e oxifluoretos de metais pesados com índice de refração > 2 e transparência desde a região do UV-Vis até o infravermelho médio (~ 7µm). As sínteses foram feitas combinando diferentes óxidos e fluoretos, tais como, Ga2O3, GeO2, PbO, Bi2O3, LaF3 e NaF e utilizando a técnica de fusão seguida de choque térmico, com posterior tratamento térmico controlado. As propriedades térmicas dos novos materiais foram estudadas por calorimetria diferencial de varredura... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Photo-thermo-refractive systems obtained from Alumino-silicates doped with Ce4+, Ag+, Sb3+ and Sn2+ has been extensively studied in recent decades by Glebov and Nikonorov due to the growing need for new devices that act in optical and photonic systems. These systems present refractive index ~ 1.5, which limits the observation of nonlinear effects and as well as the transparency in the region of low energy restricted to near infrared. In addition, as the currently known systems are multi-component, the understanding of the mechanism behind the photo-thermo sensitivity is is complex and not completely elucidated yet. In this context, the synthesis of new vitreous compositions with simplest mechanisms, with higher refraction index and transparency extended up to middle infrared region are interesting because they broaden the possibilities of applications in the areas mentioned above. In this work, we synthesized and characterized photo-thermo-refractive glass containing heavy metals oxides and oxifluorides components with refractive index higher than 2 and transparency window from UV-Vis to the medium infrared (~ 7 µm). The syntheses were made by combining different oxides and fluorides, such as, Ga2O3, GeO2, PbO, Bi2O3, LaF3 and NaF and using the melt-quenching technique with subsequent controlled heat treatment. The thermal properties of the new materials were studied by differential scanning calorimetry (DSC). The structural properties were evaluated by Raman spectroscopy and... (Complete abstract click electronic access below) / Doutor

A implantação de materiais vítreos e vitrocerâmicos bioativos representa estratégia terapêutica importante para se promover a formação de matriz extracelular mineralizada em defeitos ósseos críticos. Quando expostos a fluidos biológicos, estes biomateriais sofrem alterações químicas e topográficas de superfície que afetam as interações de células com sua superfície, reduzindo o espraiamento celular e alterando o padrão de marcação de proteínas do citoesqueleto. O objetivo deste estudo foi avaliar se as alterações no padrão de marcação para as proteínas citoesqueléticas actina e tubulina observadas in vitro em células osteogênicas sobre superfícies do vidro Bioglass® 45S5 e da vitrocerâmica Biosilicato®, são decorrentes de redução quantitativa na expressão do RNAm e das proteínas correspondentes. Células osteogênicas foram obtidas a partir da digestão enzimática de calvárias de ratos Wistar recémnascidos e plaqueadas sobre superfícies de Bioglass® 45S5, Biosilicato® e borosilicato (controle bioinerte) para a avaliação dos seguintes parâmetros: 1) detecção de actina e tubulina por microscopia de fluorescência; 2) expressão de RNAm para actina e tubulina por reação em cadeia da polimerase em tempo real (Real time PCR); 3) quantificação de actina e tubulina por ensaio imunoenzimático direto (ELISA), e 4) análise da morfologia celular por microscopia eletrônica de varredura (MEV). Aos 3 e 7 dias, células crescidas sobre borosilicato exibiam padrões de marcação para actina e tubulina típicos de células aderidas e espraiadas sobre substratos planos in vitro, enquanto que sobre Bioglass® 45S5 e Biosilicato® as células apresentavam áreas circulares destituídas de marcação para essas proteínas. Nos mesmos períodos, culturas crescidas sobre os materiais bioativos apresentavam alterações significantes da expressão de RNAm para actina e tubulina, embora fossem observadas apenas discretas variações na quantidade das proteínas correspondentes em relação ao borosilicato. Além disso, apenas para culturas crescidas sobre borosilicato observava-se correlação positiva entre RNAm e proteína e correspondência entre as observações por epifluorescência e os dados quantitativos. Aos 3 dias, imagens de MEV revelaram células aderidas e espraiadas sobre os materiais bioativos, parcial ou totalmente recobertas por acúmulos de material de aspecto semelhante ao da topografia do substrato, por vezes impedindo a visualização dos limites celulares. Com base nos resultados obtidos, conclui-se que as superfícies bioativas de Bioglass® 45S5 e Biosilicato® afetam a expressão de RNAm para actina e tubulina, mas não de proteína. Assim, as alterações nos padrões de marcação por fluorescência para essas proteínas devem ser atribuídas, pelo menos em parte, a acúmulos de material sobre as células, possivelmente decorrentes das reações de superfície a que estão submetidos Bioglass® 45S5 e Biosilicato® quando em contato com fluidos biológicos. / Bioactive glasses and glass-ceramics have been successfully applied in various therapeutic strategies to promote the formation of mineralized matrix in bone defects. The exposure of these materials to biological fluids results in chemical and topographical modifications that may affect the interactions of cells with the biomaterial surface, with potential effects on cytoskeletal protein expression and/or organization and cell spreading. The aim of the present study was to evaluate whether changes in the labelling pattern for the cytoskeletal proteins actin and tubulin in osteogenic cells cultured on bioactive Bioglass® 45S5 and Biosilicate® are due to altered mRNA and protein expression levels. Osteogenic cells were obtained by enzymatic digestion of newborn Wistar rat calvarial bone and plated on Bioglass® 45S5, Biosilicate® and borosilicate (bioinert control) for periods of up to 7 days. The following parameters were assayed: i) qualitative epifluorescence analysis of actin and tubulin distribution; ii) quantitative mRNA expression for actin and tubulin by real time polymerase chain reaction (real time PCR); iii) quantitative actin and tubulin expression by enzymelinked immunoabsorbent assay (ELISA), and iv) qualitative analysis of cell morphology by scanning electron microscopy (SEM). At days 3 and 7, cells grown on borosilicate showed typical actin and tubulin labeling patterns of adherent and spread cells on flat, rigid substrates, whereas those on Bioglass® 45S5 and Biosilicate® showed dark areas devoid of fluorescent signals for the cytoskeletal proteins. At the same time points, cultures grown on the bioactive materials showed significant changes in mRNA expression for actin and tubulin, although only slight differences in the amount of actin and tubulin were detected compared with borosilicate. Moreover, a positive correlation between mRNA and protein expression levels as well as a correspondence between epifluorescence imaging and the quantitative data were only detected for cultures grown on borosilicate. SEM analysis revealed that cells cultured on bioactive surfaces were partly or totally covered with material accumulations, whose characteristics resembled the ones for the substrate topography, and which, in some cases, prevented the visualization of the cell limits. In conclusion, Bioglass® 45S5 and Biosilicate® affect actin and tubulin mRNA levels, but not the corresponding protein expression, in osteogenic cell cultures. Thus, the observed changes in the labeling pattern for these proteins should be attributed, at least in part, to the accumulation of materials on the cell surface, likely due to substrate reactions that take place on Bioglass® 45S5 and Biosilicate® when exposed to the cell culture medium.

O desenho planar para as células a Combustível de Óxido Sólido (SOFC) é melhor do que o tubular devido a sua maior densidade de corrente e menor custo de fabricação. No entanto, o projeto de SOFC planar requer selantes para evitar o vazamento de combustível e a mistura de gases em altas temperaturas. Os vidros e os vitrocerâmicos têm demonstrado serem os mais adequados por apresentarem boa compatibilidade com outros componentes da célula nas temperaturas de trabalho das SOFCs (700-1000°C). No presente estudo, uma série de composições pertencentes ao sistema BaO-Al2O3-SiO2 (BAS) com a adição de B2O3 foram sintetizados tomando as proporções apropriadas de cada óxido constituinte. Propôs-se melhorar este sistema utilizando-se formadores e teores relevantes de modificadores estruturais, de forma a compatibilizar tanto o desempenho térmico por meio do coeficiente de expansão térmica (CET) como a compatibilidade química com os demais componentes da célula. A originalidade deste estudo está na busca destas características em regiões de composições ainda não exploradas, localizadas dentro do triangulo de compatibilidade BS-B2S-BAS2 na região rica em bário do sistema ternário. Entre estes vidros sintetizados quatro composições (BAS-4, BAS-5, BAS-6 e BAS-7) foram escolhidas porque são as mais adequadas às solicitações termomecânicas exigidas para um material vítreo atuar como selante em SOFC. / The design for planar cells Fuel Solid Oxide (SOFC) is better than the tubular due to its higher current density and lower manufacturing cost. However, the design of planar SOFC requires sealant to prevent leakage of fuel and the mixture of gases at high temperatures. Glasses and glass-ceramics have proven to be the most suitable because they have good compatibility with the other components of the cell at working temperature (700-1000°C). In the present study, a series of compositions belonging to the BaO-Al2O3-SiO2 (BAS) system with the addition of B2O3 were synthesized having the appropriate proportions of each component oxide. It was proposed to improve this system using relevant levels of formers and structural modifiers oxides, in order to match both the thermal performance of thermal expansion coefficient (TEC) and chemical compatibility with other components of the cell. The originality of this study is to search for these characteristics in regions of compositions not yet explored, located inside the compatibility triangle BS-B2S-BAS2 at the barium rich part of the ternary diagram. Among the synthesized glasses four batch compositions (BAS-4, BAS-5, 6-BAS, BAS-7) were chosen because best matched the thermo-mechanical required for a glassy material to act as SOFCs sealant.