Submitted by Maria Eneide de Souza Araujo (mearaujo@ipen.br) on 2017-03-10T17:07:28Z No. of bitstreams: 0 / Made available in DSpace on 2017-03-10T17:07:28Z (GMT). No. of bitstreams: 0 / Este estudo teve como objetivo avaliar a adaptação marginal em restaurações classe II em dentina e esmalte dental utilizando um sistema adesivo universal de acordo com três técnicas diferentes de aplicação: Autocondicionante, condicionamento seletivo e condicionamento total, através do sistema de tomografia por coerência óptica (OCT), antes e após ao envelhecimento por termociclagem (TC). Preparos classe II foram confeccionados nas paredes mesial e distal, em 30 molares hígidos humanos, com término da cavidade em esmalte e em dentina. Todos os espécimenes foram restaurados (adesivo Single Bond Universal e resina composta Filtek Z350 XT) nas três técnicas de aplicação. Os dentes foram distribuídos aleatoriamente em três grupos (n=10), sendo um para cada técnica de aplicação adesiva: Grupo I: autocondicionante, Grupo II: condicionamento seletivo e Grupo III: condicionamento total; em seguida os grupos foram avaliados antes e depois a termociclagem pelo sistema de tomografia por coerência ótica. De posse dos corpos de prova devidamente restaurados, partimos para os procedimentos de termociclagem (1000 ciclos de 1 minuto com intervalo de 30 segundos) e a avaliação pelo sistema de Tomografia por Coerência Óptica. Em seguida, as amostras foram examinadas por meio de imagens geradas pelo OCT e os dados foram submetidos ao teste estatístico não-paramétricos de Kruskal-Wallis e Dunn (p<0.05). Foi observada diferença estatisticamente significante da adaptação marginal entre os grupos com término em esmalte (p= 0.0073); para os grupos com término em dentina, não foi observada diferença estatisticamente significante na adaptação marginal (p=0.2063). Conclui-se que o OCT foi, então, capaz de diagnosticar a microinfiltração marginal nas restaurações em cavidades classe II. Existe deterioração das margens e alteração de padrão de infiltração marginal com as diferentes técnicas adesivas dos preparos classe II restauradas com resina em esmalte. Atribui-se à termociclagem a falha de vedamento marginal observada nos espécimes após em esmalte. / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Este estudo apresenta uma abordagem para a avaliação do comportamento de um ferro fundido branco de alto cromo e um aço ferramenta AISI D2 submetido a ciclos térmicos. Para a realização do estudo foi desenvolvido um procedimento para ensaios de fadiga térmica submetidos a números de ciclos variados, usando para aquecimento um sistema indutivo e para resfriamento um tanque de água. Devido a complexidade dos fenômenos envolvidos, um modelo de elementos finitos foi elaborado para a solução do campo de temperaturas e tensões superficiais atuantes. O controle da tensão superficial atuante foi realizado por meio da mudança de geometria do corpo de prova, sendo esta geometria resultante de teste por simulação computacional. Os corpos de prova foram caracterizados quando a sua microdureza e fração volumétrica de carbonetos antes do ensaio e após ensaio foram caracterizados quanto a sua microdureza, número e profundidade das trincas. O regime de propagação durante os primeiros 50 ciclos foi controlado por mecanismo de fadiga de baixo ciclo, exibindo as maiores velocidade de propagação das trincas e o regime de propagação depois dos 50 ciclos foram controlados por mecanismos de fadiga de alto ciclo. A nucleação das trincas ocorreu predominantemente pela interface matriz/carboneto e pelo próprio carboneto, sendo a propagação das trincas predominantemente pela interconexão de carbonetos fraturados na superfície do material e predominantemente na interface matriz carboneto em camadas mais profundas do corpo de prova. Os resultados obtidos mostraram uma boa correlação entre o ensaio e o modelo numérico, permitindo uma maior confiabilidade para execução do modelo mecânico subsequente. Baseado nos resultados foi possível propor uma metodologia para a avaliação de ambos materiais submetidos a ciclos térmicos. / This study presents an approach to evaluate the behavior of high chromium white cast iron and AISI D2 tool steel submitted at thermal cycles. It was developed a procedure for a thermal fatigue test in different times of cycles were done, using induced heating and water cooling. Due to the complexity of the phenomena involved, a FEM study was performed for solving the temperatures and superficial stresses fields. The control of superficial stress was done by changing the geometry of the test specimens, what was defined by computational simulation. The test specimens were evaluated the microstructure, microhardness and carbides contends before the test. After the test were evaluated microhardness, amount and depth of thermal fatigue cracks. The propagation during the earlier cycles was defined by mechanics of low cycle instead of after 100 cycles that was defined by mechanics of high cycle fatigue. This mechanics was observed by crack velocity analyses in both periods. The nucleation of thermal fatigue cracks initiate mostly at the matrix/carbide interface or at the carbide itself, being the cracks propagation was mainly by the interconnection of fractured carbides at surface and mainly at the interface matrix/carbide in the inner layer of the specimens test. The results obtained showed an adherence between the test and the numerical model, allowed a greater reliability to the subsequent mechanical model. Based on the results was possible propose a methodology for evaluation of both materials subjected a thermal cycles.

Este estudo in vitro teve como objetivo determinar a infiltração marginal e resistência à remoção por tração de coroas totalmente metálicas, cimentadas com cimento de fosfato de zinco e que foram submetidas à abertura oclusal para tratamento endodôntico. Foram usados 20 dentes molares (Banco Permanente de Dentes Humanos da FOUSP). Os dentes foram fixados sobre uma base acrílica de secção circular e foram torneados configurando preparos para coroas totais com dimensões de altura e diâmetro padronizadas. Coroas metálicas em Ni Cr foram fundidas através da técnica de enceramento direto e cimentadas com cimento de fosfato de zinco com carga axial de 5 Kg por 10 minutos. Os corpos de prova foram divididos em: Grupos Controle GC1 e GC2, que utilizaram os mesmos corpos de prova, e Grupo Experimental (GE). Todos os corpos de prova foram mantidos em água destilada para que não se desidratassem. Os espécimes dos grupos GC1 e GC2 foram mantidos sem nenhuma intervenção e os do grupo GE foram perfurados com broca de carbide de tungstênio, simulando uma cirurgia de acesso endodôntico. As amostras dos grupos GC2 e GE foram submetidas à ciclagem térmica de 700 ciclos entre 5º e 55º C. Em seguida foram mantidos em uma solução de azul de metileno 0,5%, ph 7,2 por 4 horas a 37º C. Foram submetidos ao ensaio mecânico de tração das coroas em uma máquina universal de ensaios Kratos SV 100, regulada para trabalhar a uma velocidade de ensaio de 0,5 mm/minuto. Os resultados obtidos foram submetidos à análise estatística pelos testes t de Student e as infiltrações avaliadas pela correlação linear de Spearman. A análise inferencial dos resultados dos testes de tração demonstrou com um nível de significância p=0,108, entre os grupos GC1 e GC2, e p=0,502, entre os grupos GC2 e GE, não haver diferença estatisticamente significante. As médias dos valores obtidos nos testes de tração e os seus respectivos desvios padrão foram: GC1 13,96+/-4, 48, GC2 11,26+/-2,269 e GE 10,09+/-4,86 (valores em Kgf). A análise visual subjetiva da infiltração nos corpos de prova indicou que o grupo GE apresentou o maior grau de infiltração marginal com presença do corante atingindo o terço oclusal das paredes axiais (mediana dos scores 3). O grupo GC2 apresentou infiltração marginal no terço médio (mediana dos scores 2). O grupo GC1 apresentou infiltração marginal no terço cervical e médio (mediana dos scores 1). / This in vitro study had the objective to determine the marginal microleakage and the retentive strength of totally metallic crowns, cemented with zinc phosphate cement and subjected to occlusal access for endodontic treatment. 20 human molars (Banco Permanente de Dentes Humanos da FOUSP) have been used for the experiment. The teeth were fixed on a circular acrylic section base and were prepared with standardized dimensions. Metallic crowns in Ni Cr were cast with the direct waxing technique and cemented with zinc phosphate cement with vertical load of 5 kg for 10 minutes. The specimens were divided in groups: Group Control 1 (GP1), Group Control 2 (GP2) and Group Experimental (GE). All the specimens were kept on distillated water so that they wouldn’t dehydrate. The specimens of the groups GC1 and GC2 were kept without any intervention and the ones of the group GE were drilled with a tungstein carbide bur, simulating an endodontic access surgery. Next, the samples of groups GC2 and GE were subjected to a thermal cycling of 700 cycles between 5º and 55º C. To verify the existence of micro infiltration, it was used the methylene blue dye test, 0,5%, ph 7,2 for 4 hours at 37ºC. The specimens were subjected to the load of tension in a universal tensile testing machine Kratos SV 100 at speed 0,5 mm/min. Statistical analyses with t tests showed no significant difference between crown retention before and after endodontic access preparation (p=0,108). The mean displacement forces were: GC1 13,96+/-4,48, GC2 11,26+/-2,269 e GE 10,09+/-4,86 (value in Kgf). With the Spearman’s evaluation test the microleakage was measured. The results showed a greater median of score in GE (score 3). The GC2 and GC1 showed median scores 2 and 1 in order.

Dans le but de l’intégration des supercondensateurs dans des applicationstransport, la connaissance et l’étude de leur comportement au cours du vieillissementest nécessaire. L’objectif de cette thèse est donc la compréhension et lamodélisation des phénomènes de vieillissement observés sur lessupercondensateurs. Pour cela, des méthodologies de caractérisation électriques etdes protocoles expérimentaux originaux combinant les différentes contraintes devieillissement ont été mis en oeuvre. Des mesures du courant de fuite et des tests devieillissement combinés ont été effectués. Les résultats obtenus sont présentés. Ilsont ainsi servis au développement et l’implémentation de modèles permettant le suivide l’évolution des performances des supercondensateurs avec le vieillissement. / The study of the behavior of supercapacitors during ageing is required in orderto integrate them in transportation applications. The aim of this thesis is tounderstand and model ageing phenomena observed on supercapacitors. For thispurpose, electrical characterization methodologies and original experimentalprotocols combining various constraints of ageing have been implemented.Measurements of leakage current and combined ageing tests were conducted. Theobtained results were used for developing models allowing the monitoring of theevolution of supercapacitors performance during ageing.

L’introduction des composites dans des pièces structurelles critiques pour les aéronefs représente une réelle rupture technologique et nécessite des études spécifiques afin de maîtriser leur comportement et leur durabilité. Ce travail a pour objectifs de caractériser et de comprendre les mécanismes de vieillissement de composites interlock 3D à fibres de carbone et à matrice polymère lorsqu’ils sont soumis à des cycles thermiques.Dans ce but, un essai de cyclage thermique (-55°C/120°C), dont l’environnement thermique et gazeux est totalement maitrisé, a été mis en place pour le vieillissement d’échantillons composites représentatifs du motif interlock élémentaire. L’analyse des mécanismes de dégradation induits a été réalisée grâce i/ à la mise au point d’une méthode de caractérisation quantitative 3D de l’évolution des microfissures au cours du cyclage, basée sur des observations par microtomographie RX et sur le développement d’une procédure de traitement d’images spécifique, ii/ au développement d’un essai de cyclage thermique in situ synchrotron couplé à une technique de corrélation d’images volumiques 3D, et iii/ à des simulations par éléments finis prenant en compte l’architecture réelle des échantillons à l’échelle mésoscopique et le comportement thermo-viscoélastique de la matrice.Les résultats obtenus mettent en évidence des couplages thermo-chimio-mécaniques complexes,qui s’expriment à travers quatre paramètres influents : le temps (et le nombre de cycles),l’architecture de l’interlock, la ténacité de la matrice et sa sensibilité à la thermo-oxydation. / The introduction of composite materials in critical structural parts for aircrafts represents a real technological breakthrough and requires specific studies to understand their behavior and durability. This work aims to characterize and understand the ageing mechanisms incarbon/epoxy 3D interlock composites when they are submitted to thermal cycling.For this purpose, a thermal cycle test (-55°C/120°C), whose heat and gaseous environment istotally mastered, was set up for the ageing of composite samples of elemental interlock pattern dimensions. Analysis of induced degradation mechanisms was achieved by i/ the development ofa 3D quantitative characterization method of the evolution of microcracks during cycling, basedon observations by microtomography RX and the development of a specific image processing procedure, ii/ the development of an in situ thermal cycle test under synchrotron light, coupled to a digital volume correlation technique, and iii/finite elements simulations taking into account the actual mesoscopic architecture of the samples and the thermo-viscoelastic behavior of thematrix.The results reveal complex thermo-chemo-mechanical couplings that are linked to four important parameters: time (and the number of cycles), the interlock architecture, the matrix toughness andits sensitivity to thermo-oxidation.

This thesis focuses on the different degradation mechanisms of the stainless steel in a travelling grate in a Grate-Kiln iron ore pellet indurator. The travelling grate is a conveyor belt that transports green-body pellets to a rotary kiln while the pellets are being dried and pre-heated to a temperature of 900-1100 °C by recycled hot air. After unloading of the pellets to the rotary-kiln for further sintering, the travelling grate is cooled in room temperature while returning to the loading zone of the wet pellets. The steel was tested during thermal cycling in a test-rig, in order to simulate the influence of thermo mechanical fatigue and oxide spallation. The influence of erosion-deposition was investigated in a modified horizontal industrial combustion kiln at 800 °C, with slag and coal from production used as erosive media and combustion fuel, respectively. The influence of minor alloying additions of Mn, Si and Ti on the microstructure was explored by eight different casted alloy compositions. Isothermal heat treatments were performed at 800 °C during 200 hours on steel immersed in deposits recovered from a travelling grate in production. The three main degradation mechanisms found in this work are thermal spallation, erosion-deposition and deposit induced accelerated corrosion (DIAC). Thermal spallation of the oxide layer is caused by the thermal expansion difference between the oxide and the metal during heating and cooling. It has been found that Ti improves the spallation resistance while Si reduces it. Spallation of deposits is another cause believed to increase the degradation. Erosion-deposition appears due to simultaneous erosion and deposition of particles on the travelling grate that causes erosion or deposition depending on the amount of alkali metals in the environment. The velocity of the particles also influences erosion and deposition in the way that higher velocities increase erosion. DIAC is proposed to form on the travelling grate due to the concentration of chloride- and sulphate containing alkali metals in the deposits.  Other than these major degrading mechanisms, minor degradation mechanisms such as internal oxidation, sigma formation, carburization and sensitization towards inter-granular attack have been found inside the steel during heating. Thermo mechanical fatigue (TMF) causes intergranular cracks in the material of the travelling grate. Casting issues such as micro-segregation have also been addressed in this thesis. A few different ways to improve degradation resistance have been proposed, such as homogenization heat treatments, optimization of process parameters and inhibitor solutions.

Les contraintes environnementales ont amené les constructeurs et équipementiers automobiles à développer de nouveaux types de transmission aux contraintes d'encombrement axial importantes. Pour la première fois, ce travail se concentre sur la caractérisation et l'identification du comportement sous sollicitations thermiques et mécaniques de la garniture d'embrayage, un matériau composite complexe. Les sollicitations de traction ont été réalisées à différentes températures et fréquences sur des échantillons prélevés dans le disque ou le disque complet. Nous avons ainsi identifié les caractéristiques élastiques et viscoélastiques en fonction de la température ainsi que les mécanismes d'endommagement. La dilatation thermique de la garniture a été observée sur les disques complets. Ainsi, grâce à l'utilisation de la stéréo-corrélation couplée avec des méthodes d'identification inverse nous avons pu décrire le couplage entre l'hétérogénéité du matériau et l'effet de la structure annulaire. Enfin au travers de cycles thermiques lents et homogènes, l'étude présente l'évolution du coefficient d'expansion thermique et de la tenue mécanique du matériau. / The clutch facing is an annular shaped continuous fiber composite which transmits the rotary motion from the engine to the wheels. In use it is submitted to thermal and mechanical loadings which can cause changes in the dimensions. New clutch technologies call for a better control of these changes. For the first time, this thesis was dedicated to the understanding of the dimensional stability of the clutch facing. Tensile tests were carried out under different temperature and for different frequencies on small cut specimens or on the entire annular disc. We were then able to identify the elastic and viscoelastic properties as well as the damage mechanisms until failure. The thermal expansion was measured on the entire disc as well. Thanks to digital image stereo correlation and reverse identification methods we were able to describe the coupling between the material's heterogeneities and its annular shape. Finally, this thesis presents the evolution of the material properties after homogeneous thermal cycling.

This diploma thesis aims to verify the properties of lead-free solders, which are subjected to accelerated aging by thermal cycling. The theoretical part describes in detail the most used lead-free solders and their characteristics. The next section describes fluxes and their important functions in the soldering process. Intermetallic compounds are also mentioned, which significantly affect the quality and service life of the soldered joint. In the practical parts, the test motif was on two different substrates - corundum ceramics and the widely used substrate FR-4 (Glass fiber fabric saturated with epoxy resin). SAC solder was chosen as the reference solder for the experiment, followed by solder containing bismuth (Sn42 / Bi58) and lead solder (Sn62 / Pb36 / Ag2). Accelerated aging by thermal cycling was performed in the temperature range from -20 ° C to 125 ° C, followed by performing a test of the mechanical strength of the soldered joint by means of a shear test. SnBi solder shows higher mechanical strength at the beginning of testing than SAC solder and lead solder, during temperature cycles, it significantly loses its mechanical properties, this is caused by increasing oxidation of the alloy. SAC solder seems to be promising, which has an almost constant decrease in mechanical strength during all temperature cycles on both corundum and FR-4 substrates.

Semester project deals with the theoretical processing of reflow soldering. Describes the process of reflow soldering, description of intermetallic compounds, the influence of heating factor on the reliability and strength of soldered joints.Also deals with the preparation of cross-section, X-ray control, thermal cycling and description of test boards.

Cette étude porte sur la caractérisation des mécanismes d'adhésion et d'endommagement de produits colaminés à froid, afin de pouvoir proposer des procédés optimisés. Celle-ci s’inscrit dans le cadre de la participation au projet MeGaN (pour Module Electronique GaN) qui porte le développement de nouvelles technologies de modules de puissances à base de composants à grand gap « GaN », compatibles avec des applications hautes températures et hautes tensions. Notre travail porte essentiellement sur l’intégration d’un substrat innovant (i-TBC), un composite architecturé cuivre invar doté de ponts thermiques pour un bon compromis dialatation thermique/conductivité thermique pour accueillir les composants électroniques développés dans le cadre de ce projet. Ainsi, une première partie de ce travail est axée sur la caractérisation microstructurale du substrat i-TBC durant les étapes de son élaboration, l’objectif est de comprendre l’impact du procédé de colaminage sur la formation de l’adhésion des interfaces de cuivre dans les ponts thermiques. On a ainsi mis en évidence que la recristallisation de grains et la microstructure continue à travers l'interface Cu-Cu était garante d'une bonne adhérence de celle-ci. Dans la seconde partie, nous nous sommes focalisés sur la caractérisation de la tenue mécanique du substrat i-TBCdans des conditions de cycles thermiques passifs. Pour ce faire, des essais de fatigue thermique et de choc thermique nous permettent de déterminer la sensibilité de la tenue mécanique des interfaces à la fois à l’amplitude et à la vitesse de variation de température. La conclusion de cette étudeest que les paramètres de colaminage doivent permettent un compromis entreadhérence du pont Cu-Cu et des interfaces Cu-Invar pour augmenter significativement la durée de vie du composant. Enfin, nous avons procédé à l'analyse thermo-mécanique des propriétés intrinsèques du substrat seul et de l'assemblage électronique complet. Les propriétés intrinsèques ont été établies en termes de comportement mécanique du composite Cu-Invar et d'endommagement des interfaces sous la forme de propagation d'une fissure à l'interface Cu-Cu. / This work is part of ‘MeGaN” project which focuses on the development of new power module technologies based on "GaN" wide gap components, compatible with high temperature and high voltages applications. In This study, a new substrate an innovative thermal bridge composite (i-TBC) has been developed, obtained by roll bonding of two copper sheets separated by perforated invar. The i-TBC is an “architectured” composite material that combines good thermal conductivity associated to copper and limited CTE due to the presence of invar. A particularity of the i-TBC consists of the formation of copper bonding area through the invar perforations during the cold rolling called thermal bridges. These thermal bridges, ensure good thermal conductivity of the i-TBC. Thus, a first part of this work focuses on the microstructural characterization of the i-TBC substrate during the stages of its elaboration, the objective is to understand the impact of the elaboration steps on the adhesion formationof the copper interfaces. in thermal bridges. It was thus demonstrated that the cold welding obtained along the interface Cu-Cu was a guarantee of good adhesion. In the second part, we focused on the characterization of the mechanical strength of the i-TBC substrate under passive thermal cycling conditions. To do this, tests of thermal fatigue and thermal shock allow us todetermine the sensitivity of the mechanical resistance of the interfaces to both the amplitude and the speed of temperature variation. The conclusion of this study is that the parameters of cold rolling must allow a compromise between adhesion of the Cu-Cu bridge and Cu-Invar interfaces to significantly increase the lifetime of the substrate. Finally, a finite element analysis (FEA) wasperformed. firstly, the thermal modeling validated the thermal performance of the i-TBC substrate in an electronic assembly.Then, the intrinsic properties were established in terms of mechanical behavior of the Cu-Invar composite and deterioration of the interfaces in the form of propagation ofa crack at the Cu-Cu interface.