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In this thesis, the discharge products formed at the cathode and the performance and cell chemistry of sodium-oxygen batteries have been studied. This was carried out using different NaOTf salt concentrations. The influence of different salt concentrations on sodium-oxygen batteries was investigated since it has been shown that increasing the salt concentration beyond conventional concentrations could result in advantages such as increased stability of the electrolytes towards decomposition, higher thermal stability and lower volatility. An increase in salt concentration has also been shown to influence the electrochemical potential window. The solubility of NaOTf was investigated in two different solvents, DME and diglyme. NaOTf was found to be more soluble in DME compared to diglyme but due to the volatile nature of DME, three different concentrations of NaOTf were prepared with diglyme as solvent. Experimentation involved discharging the batteries to either maximum or limited capacity. The discharge products were examined and characterized using XRD and SEM. The main discharge product was identified as sodium superoxide although sodium peroxide dihydrate was also identified in one battery. A trend of higher capacity and voltage plateaus with higher salt concentration was also found. The influence of trace amounts of water was suggested as one explanation as it works as a catalyst, promoting sodium superoxide cube growth due to improved transportation of superoxide. Another or contributing explanation could be a possible change in donor number with increased salt concentration, resulting in higher solubility and longer lifetime of superoxide, promoting the growth of sodium superoxide cubes.

Ce travail de thèse s’inscrit dans le cadre du projet ISS/FSL/FASES dont l’objectif est de comprendre les mécanismes de vieillissement des émulsions en microgravité. Ce manuscrit est dédié à l’étude au sol des émulsions de ce projet et notamment de celles stabilisées par des mélanges tensioactifs/nanoparticules. Ces émulsions sont diluées et constituées d’une phase continue d’huile de paraffine et d’une phase dispersée aqueuse contenant un tensioactif et des nanoparticules. Leur étude et leur caractérisation est réalisée par microscopie tomographique optique et cryo-microscopie électronique à balayage. Une étude préalable de la phase dispersée permet de démontrer que les proportions respectives en tensioactif et nanoparticules modifient les propriétés rhéologiques et microscopiques de ces mélanges. Ces modifications permettent de caractériser le couplage entre les molécules tensioactives et les nanoparticules. Lorsque cette phase dispersée est émulsifiée dans l’huile de paraffine, une transition dans la morphologie des gouttes peut être mise en évidence. Les gouttes de phase dispersée présentent une topologie dépendante du ratio des concentrations en tensioactif et nanoparticules : de sphérique (pour les grandes valeurs de ce ratio) elles deviennent polymorphes (pour les petites valeurs). L’observation de ces émulsions en cryo-microscopie électronique à balayage permet de visualiser des microstructures de nanoparticules et d’expliquer l’origine de la déformation des gouttes. / This thesis is part of the ISS/FSL/FASES project which aims at understanding emulsion ageing mechanisms in microgravity. This manuscript is dedicated to the ground study of these emulsions, and particularly to those stabilized by surfactant/nanoparticles mixtures. These emulsions are diluted and composed of a paraffin oil continuous phase and an aqueous dispersed phase composed of the surfactant/particle mixtures. Emulsion characterization is performed with optical tomographic microscopy and cryo-scanning electron microscopy. A preliminary investigation of the dispersed phase shows that the proportion of surfactant and nanoparticles changes the rheological and microscopic properties of these mixtures. These changes allow the characterization of the coupling between surfactant molecules and nanoparticles. When these mixtures are emulsified in paraffin oil, a transition in the droplets morphology is evidenced. Indeed, dispersed phase droplets exhibit different shapes depending on the ratio of surfactant and nanoparticle concentrations: from spherical (for high ratios) they become polymorphous (for small ratios). Observations of these emulsions with cryo-scanning electron microscopy show the existence of nanoparticles microstructures that helps the understanding of the origin of droplets deformation.

The thesis deals with the study of properties of a new system for detection of true secondary and backscattered electrons in high pressure conditions of the specimen chamber of a newly built environmental scanning electron microscope AQUASEM II. Detection system contains three detectors. For the first time is introduced and analyzed the working principle of ionisation detector with electrostatic separator, which is in many experiments compared with ionisation detector of secondary electrons. Experimentally demonstrated are unique properties of this detection system, especially the ability of energy separation of detected signal electrons. For the various working conditions are also analyzed signal levels detected by the BSE YAG detector, which is designed as a part of the new detection system and which worked together with both ionisation detectors.

Master of Science / Department of Biological and Agricultural Engineering / Donghai Wang / Algae proteins have similar amino acid compositions as conventional plant proteins, and are comparatively richer in the essential amino acids. Algae protein has the potential to be used in the development of a wide variety of products, including foods, animal feeds, bioplastics, and adhesives. The utilization of algae protein for value-added products would increase the economic feasibility of algae biodiesel. This research evaluated the adhesion, rheological, morphological, and thermal properties of adhesives made from algae protein extracted from Cladophora sp. and modified with either sodium hydroxide (pH 9, 10, 11) or sodium dodecyl sulfate (SDS, 0.5, 1, and 3%). Both alkali-modified and SDS-modified algae protein adhesives displayed improved dry shear strength compared to unmodified algae protein. However, only 3% SDS-modified algae protein significantly improved the water resistance as shown in wet and soak shear strength tests. Thermal analysis using differential scanning calorimetry showed that SDS modification caused complete denaturation of the algae protein. SDS modification also increased the viscosity of the adhesive and created rougher particle surface texture. These data suggest that SDS modification can effectively increase shear strength and water resistance of algae protein adhesives caused by protein denaturation and protein structure change.

Durante e após o processo de reparo alveolar pós-extração, ocorre certa remodelação óssea com reduções dimensionais deste tecido podendo comprometer a terapia em implantodontia. A fim de preservar/reconstruir tal tecido, vários métodos são propostos usando diferentes tipos de biomateriais e técnicas, os quais demonstram capacidade em formar osso. O osso autógeno ainda é considerado a referência padrão como enxerto ósseo, devido ao seu potencial osteogênico, osteoindutor e osteocondutor, mas morbidade relativa a este é conhecida. Por isso algumas biocerâmicas têm sido utilizadas, pois são sintéticas, biocompatíveis e com boas propriedades osteopreenchedoras, mas com baixa osteogenicidade. A engenharia tecidual óssea constituída de células tronco mesenquimais diferenciadas em osteoblastos é uma estratégia para o fornecimento adicional celular ao defeito ósseo em reconstrução. O objetivo deste estudo foi qualificar e quantificar a reparação óssea após o enxerto de uma associação de osso autógeno e células osteoblásticas carreadas por uma biocerâmica em defeitos ósseos produzidos pela extração dentária. Os animais foram divididos de acordo com o material implantado no alvéolo dentário pós-extração em: Controle (c), osso autógeno (oa), células osteoblásticas (co), biocerâmica (bc), osso autógeno + células osteoblásticas (oa+co), osso autógeno + biocerâmica (oa+bc), biocerâmica + células osteoblásticas (bc+co), e biocerâmica + células osteoblásticas + osso autógeno (bc+co+oa). O sacrifício ocorreu aos 7, 21 e 42 dias pós-cirurgia e as amostras teciduais foram processadas para análise em microscopia de luz e eletrônica de varredura. Através de um sistema de análise de imagens foi avaliado a qualidade dos biomateriais implantados e o volume de osso, biocerâmica, conjuntivo e coágulo no defeito ósseo. Os resultados qualitativos revelaram que a biocerâmica implantada foi biocompatível e estava intimamente unida ao osso. O uso das células osteoblásticas, do osso autógeno ou da biocerâmica não desencadearam reações imunogênicas, de corpo estranho ou formação tumoral. Histometricamente as células osteoblásticas carreadas pela biocerâmica mostraram um preenchimento ósseo 19,0% maior do que quando não carreadas. A associação biocerâmica/células osteoblásticas + osso autógeno promoveu, aos 7 dias, uma deposição óssea 56,52% mais efetiva nos arredores do biomaterial do que a enxertia da biocerâmica isoladamente (1%). Conclui-se que a biocerâmica em questão pode ser um viável carreador às células osteoblásticas a serem enxertadas em sítios de reconstrução óssea, e que este composto híbrido recebe um efeito sinérgico quando da associação ao osso autógeno, sendo capaz desta forma de acelerar o processo de neoformação óssea principalmente nos períodos iniciais da reparação alveolar. / During and after the process of alveolar repair post-extraction, bone remodeling occurs with certain dimensional reductions of this tissue that can compromise the therapy in implantology. In order to preserve/reconstruct such tissue, various methods are proposed using different types of biomaterials and techniques which demonstrate the capacity to form bone. The autogenous bone is still regarded as the gold standard bone graft, due to their osteogenic, osteoinductive and osteoconductive potential, but morbidity is known about it. Therefore some bioceramics have been used, as they are synthetic, biocompatible and with good properties of bone fill, but with low osteogenic potential. The bone tissue engineering consists of mesenchymal stem cells differentiated into osteoblasts is a strategy for providing additional cell in the bone defect reconstruction. The aim of this study was to qualify and quantify bone healing after grafting of an association of autogenous bone and osteoblastic cells carried by a bioceramic in bone defects produced by tooth extraction. The animals were divided according to the implanted material in dental socket after extraction: Control (c), autogenous bone (ab), osteoblastic cells (oc), bioceramic (bc), autogenous bone + osteoblastic cells (ab+oc), autogenous bone + bioceramic (ab+bc), bioceramic + osteoblastic cells (bc+oc), and bioceramic + autogenous bone + osteoblastic cells (bc+oc+ab). The animals were sacrificed at 7, 21 and 42 days post-surgery and tissue samples were processed for light microscopy and scanning electron microscopy. Through an image analysis system the quality of implanted biomaterials and the volume of bone, bioceramic, conjunctive tissue and blood clot was evaluated inside the bone defect. Qualitative results revealed that the grafted bioceramic was biocompatible and intimately bonded with the bone. The use of osteoblastic cells, autogenous bone or bioceramic didnt trigger immunogenic reactions, foreign body or tumor formation. Histometrically, the osteoblast cells carried by bioceramic showed a bone filling 19.0% higher than when not carried. The bioceramic/osteoblastic cells + autogenous bone association promoted, at 7 days, a bone deposition 56.52% more effective around the biomaterial than the grafting of bioceramic alone (1%). It was concluded that the bioceramic in question may be a viable carrier to osteoblastic cells to be grafted on sites of bone reconstruction, and this hybrid compound receives a synergistic effect when associated to autogenous bone, thus being able to accelerate the bone formation especially in the early periods of alveolar repair.

É cada vez maior a utilização de polímeros reforçados com fibra de vidro no mercado nacional. Entre eles utiliza-se a poliamida 6 que apresenta ótima resistência à tração, ao impacto e à absorção de umidade comparada à poliamida 6 sem reforço de fibra de vidro, sendo atualmente utilizada na indústria automobilística em peças sob o capô, em especial em carcaças de radiadores. Este trabalho foi realizado com o objetivo de estudar o efeito da radiação ionizante nas propriedades mecânicas (resistência à tração, à flexão e ao impacto Izod) e térmicas (resistência ao fio incandescente e temperatura de fusão) da poliamida 6 com reforço de fibra de vidro, submetida à diferentes doses de radiação (100 a 600 kGy). As amostras foram preparadas e irradiadas em um acelerador JOB 188 com feixe de elétrons de energia de 1,5 MeV em diferentes doses e uma taxa de dose de 22,61 kGy/h. Após a irradiação, as propriedades das amostras da poliamida 6 com reforço de fibra de vidro irradiada foram determinadas e comparadas com as amostras não irradiadas e constatou-se que as propriedades mecânicas de resistência à flexão e à tração aumentaram e a de resistência ao impacto diminuiu. Em relação à propriedade térmica de temperatura de fusão diminuiu de 224,4ºC para 212,5ºC mas a perda de massa diante do aumento constante da temperatura também diminuiu. Em relação à propriedade de resistência ao fio incandescente a poliamida 6 com reforço de fibra de vidro irradiada teve um bom desempenho. As imagens captadas por Microscopia Eletrônica de Varredura mostram que a irradiação provocou uma boa integração entre a fibra de vidro e o polímero o que foi responsável pelo bom desempenho na propriedade de resistência ao fio incandescente. / It is each time more common the use of polymers reinforced with fibreglass in the domestic market. Between them it is used polyamide 6 that it presents good tension resistance, to the impact and the humidity absorption compared with non-reinforced, being also at the present time used in the automobile industry in parts underneath the hood, especially in the radiator frames. The aim of this work is to study the effect of ionizing radiation on properties of polyamide 6 with fibreglass reinforcement, undergone to different radiation doses. Samples were prepared and irradiated on JOB 188 accelerator with an electron beam energy of 1.5 MeV in air with different doses (100 to 600 kGy) and a dose rate of 22.61 kGy/h. Afterward the irradiation, the properties of the samples of irradiated polyamide 6 with fibreglass reinforcement were evaluated and compared with the samples non-irradiated. It evidenced that the mechanical properties flexural resistance and tension resistance increased and the resistance to the impact decreased. Regarding the thermal properties of the temperature of fusing decreased of 224,4ºC for 212,5ºC but the loss of mass ahead of the constant increase of the temperature also decreased. In the property of resistance to the glow wire the polyamide 6 with fibreglass reinforcement had a good performance. The images caught for Scanning Electronic Microscopy show that the irradiation provoked a good integration enters the fibreglass and polymer what was responsible for the good performance in the property of resistance to the glow wire.

Os estudos sobre contaminação apresentam difícil comparação devido a variedade dos delineamentos experimentais como o tipo de substrato testado, o momento na sequência do procedimento adesivo em que a contaminação acontece e a forma como essa contaminação é tratada de maneira a limpar este campo operatório. Assim, novos estudos fazem-se necessários para investigar com maior profundidade as condições já descritas na literatura e assim, obter um protocolo de conduta mais seguro para lidar com a contaminação. Esse estudo objetivou analisar,através de Microscopia Eletronica de Varredura (MEV), a interface adesiva de restaurações realizadas com sistema adesivo autocondicionante de dois passos (Clearfill SE Bond Kuraray), contaminadas por sangue em dois momentos diferentes, recebendo essa contaminaçao dois tratamento distintos. Para tanto foram selecionados 15 molares humanos que foram divididos em 5 grupos experimentais (n=3): G1 controle (sem contaminaçao); G2 contaminação antes do primer, com tratamento de lavagem e secagem; G3 contaminação antes do primer com tratamento de secagem; G4 contaminação após bond fotopolimerizado com tratamento de lavagem e secagem; G5 contaminação após bond fotopolimerizado com tratamento de secagem. Os dentes foram submetidos ao corte do terço oclusal da coroa para obtenção de superfície dentinária plana. Essa superfície foi regularizada com lixas SiC e a camada de esfregaço padronizada foi obtida com lixa SiC #600 por 1 min. Os espécimes foram contaminados, de acordo com os grupos experimentais, com sangue obtido de um único doador o próprio autor armazenado em tubos Vacuette® com heparina sódica e utilizado em até 7 dias. Então foram restaurados com uma camada de resina flow (Filtek Z-350 Flow 3M-ESPE) e duas camadas de resina microhibrida (Filtek Z-350 3MESPE). Após a construção dos espécimes, estes foram seccionados ao meio e passaram por preparo para análise em MEV. Os resultados obtidos foram descritos de duas formas: Análise Morfológica: onde foram observadas alterações na formação da camada híbrida (CH) em grupos com a presença do contaminante, e Análise Morfométrica, que foi analisada estatisticamente, e pode-se constatar uma relação entre a presença do contaminante e a diminuição do tamanho de tags em m, quando comparados ao grupo controle (p 0,05). Adicionalmente, foi observado que o tratamento de lavagem com água não foi suficiente para reestabelecer a formação de camada híbrida semelhante a observada no grupo controle. / Studies on contamination are difficult to compare due to the variety of experimental designs as the type of substrate, the time when contamination takes place during the adhesive procedure and how this contamination is treated in order to clean the operatory field. Thus, further studies are needed to investigate more thoroughly the conditions described in the literature and obtain a protocol to deal with contamination. This study aimed to observe, by scanning electron microscopy (SEM), the interface of adhesive restorations performed with a two-stepself-etching adhesive system (Clearfill SE Bond - Kuraray), contaminated with blood at two different times, receiving two different treatment to the contamination . Therefore, 15 selected human molars were divided into five experimental groups (n = 3): G1 - control (no contamination), G2 - contamination before primer, and rinsing and drying treatment, G3 - contamination before priming treatment, thendrying; G4 - contamination after light curing bond, rinsing and drying treatment; G5 - after light curing bond and drying. The teeth were then seccioned in order to obtain a flat dentin surface. This surface was regularized with SiC sandpaper and a standardized smear layer was obtained with SiC sandpaper # 600 for 1 min. The specimens were subsequently contaminated, according to the experimental groups, with blood obtained from a single donor - the author stored inVacuette ® tubes with sodicheparin and used within 7 days. They were restored with a layer of flowable composite (Filtek Z-350 Flow - 3M-ESPE) and two layers of microhybridresin (Filtek Z-350 - 3M-ESPE). After construction, the specimenswere divided in two, exposing the center of restorationand passed through preparation for SEM analysis. The results were described in two ways: Morphological Analysis where changes were observed in hybrid layer (HL) formation of groups in the presence of the contaminant, and Morphometric Analysis, which was analyzed statistically andaassociation between presence of the contaminant and a decreasing size of tags was found when compared to the control group (p 0.05). Additionally, it was observed that treatment of washing with water was not sufficient to restore the formation of hybrid layer similar to that observed in the control group.