O tratamento preconizado para dentes permanentes avulsionados devido a traumatismos dentários em crianças é o reimplante dental. Entretanto, sabe-se que o sucesso após o reimplante depende, especialmente, do tempo em que o dente permanece fora do alvéolo e do meio de conservação no qual o dente é armazenado. Nesse sentido, para que se tenha sucesso após o reimplante faz-se necessário que o dente seja imediatamente reimplantado e/ou seja mantido em um meio capaz de manter a vitalidade das células da superfície radicular. Se isso não for possível, o tratamento da superfície radicular deverá ser instituído com o objetivo de prevenir a reabsorção radicular. Dessa maneira, esta pesquisa teve como primeiro objetivo avaliar a influência de diferentes meios de conservação para dentes avulsionados, por meio de uma revisão sistemática, com a finalidade de estabelecer se há um consenso sobre o meio mais adequado para conservação capaz de prevenir sequelas como anquilose e reabsorção dentária. A seguir, o segundo objetivo desse estudo foi testar o Denosumab, um anticorpo monoclonal anti-RANKL, como substância para o tratamento tópico da superfície radicular, a fim de evitar a anquilose e a reabsorção dentária por substituição. Para tanto, foram utilizados 36 incisivos superiores direitos de ratos submetidos à extração cirúrgica, manutenção em meio extra-alveolar seco por 60 minutos e posterior reimplante. No grupo I, controle positivo, foi realizado o reimplante tardio sem tratamento de superfície; nos grupos II e III, grupos experimentais, previamente ao reimplante tardio foi realizado o tratamento da superfície radicular com solução de Denosumab a 60 mg/mL e a 30 mg/mL, respectivamente, por 10 minutos. Os canais radiculares dos animais dos três grupos foram preenchidos com pasta à base de hidróxido de cálcio, via retrógrada, e em seguida os dentes foram reimplantados. Decorridos 15 e 60 dias do reimplante, os animais foram submetidos à eutanásia e as peças, contendo dente e osso, foram removidas para o processamento histotécnico. A seguir cortes histológicos foram realizados, corados por hematoxilina e eosina (HE), para descrição das características da superfície dentária e do ligamento periodontal e para mensuração do comprimento (perímetro) da anquilose e/ou reabsorção por substituição e das áreas de reabsorção dentária, em microscopia de luz e, para mensuração da área do ligamento periodontal, em microscopia de fluorescência. Espécimes sequenciais foram analisados por meio de coloração de Brown & Brenn modificada para identificação de micro-organismos e imunohistoquímica para identificação dos marcadores RANKL, OPG e Periostina (PRT). As análises foram realizadas de forma descritiva e quantitativa. Dados quantitativos foram submetidos à analise estatística por meio do teste paramétrico ANOVA de uma via e pós-teste de Tukey e dos testes não-paramétricos de qui-quadrado e exato de Fisher, com nível de significância de 5%. Ao final da revisão sistemática da literatura pudemos concluir que não há evidência para estabelecer qual o melhor meio de conservação para dentes avulsionados. Dentre os meios que foram encontrados estão a água de coco, água da torneira, leite de soja, leite integral, solução salina, saliva, própolis, soro fisiológico, solução Euro-Collins, solução salina balanceada de Hanks (HBSS) e Viaspan®. Ainda que esta revisão tenha sido conduzida em modelo animal experimental, a baixa qualidade dos estudos bem como a sua heterogeneidade indicam que a extrapolação para humanos deva ser cautelosa. No estudo experimental em modelo animal, o tratamento de superfície com Denosumab a 60 mg/mL preveniu a anquilose, a reabsorção por substituição e a reabsorção dentária, após 60 dias, comparado com o grupo sem tratamento. A coloração de Brown & Brenn evidenciou uma menor contaminação nos tecidos mineralizados quando do tratamento de superfície com Denosumab, independente da concentração utilizada. Com relação à imunohistoquímica, o tratamento com Denosumab inibiu a síntese de RANKL sem modular OPG. A Periostina foi observada no ligamento periodontal dos dentes reimplantados. Porém, essa marcação estava ausente nas áreas de anquilose, em ambos os períodos experimentais, indicando que durante o processo de anquilose a síntese de periostina é inibida, o que resulta na fusão do osso à superfície radicular. / The treatment of choise for permanent dental avulsion is replantation. However, it is known that the success of the repair after replantation depend especially the extracellular and the storage medium in which is stored the tooth. Accordingly, in order to have success after replantation is necessary that the tooth is replanted immediately and/or to be kept in a medium capable of maintaining the cell´s vitality of the root surface. If that is not possible, treatment of the radicular surface should be done in order to prevent radicular resorption. Thus, the firstly aim was to perfom a systematic review to evaluate the in vivo effectiveness of different storage media for avulsed teeth. So, the second aim of this study is to test the substance as Denosumab, a monoclonal antibody, for the topical treatment of the root surface in order to prevent dental ankylosis and replacement resorption. For this, we used 36 rat incisors rights, extracted and replanted, and divided into: group I, positive control, delayed replantation without root surface treatment; groups II and III , experimental groups, delayed replantation without root surface treatmen with Denosumab 60 mg/mL and 30 mg/mL, respectively, for 10 minutes. The canals were filling with calcium hydroxide and the teeth were replanted. After periods of 15 and 60 days of the replantation, the animals will be euthanized. Then, samples are removed and processed for microscopic analysis. Histological sections were performed, stained with hematoxylin and eosin, to describe the characteristics of the dental surface and the periodontal ligament and to measure the length of ankylosis, replacement resorption and dental resorption by conventional microscopy, and for the measure the area of periodontal ligament, by fluorescence microscopy. Sequential specimens were analyzed by Brown & Brenn, for localization of bacteria; and markek by immunohistochemistryfor RANKL, OPG and Periostin (PRT). The analysis were displayed qualitatively or quantitatively. Data were subjected to statistical analysis by oneway ANOVA and the Tukey post-test and by chi-square and Fisher\'s exact tests. The significance level was set at 5%. The systematic review does not provide enough evidence to determine the best storage medium to achieve successful tooth replantation. This systematic review has identified many storage media that have been used to preserve avulsed teeth, including coconut water, tap water, soy milk, whole milk, saline solution, saliva, propolis, physiologic saline, Euro-Collins solution, HBSS, and Viaspan®. Although this review was conducted in an experimental animal model, a poor quality of the studies as well as their heterogeneity indicates that a human extrapolation should be cautious. In the experimental study in animal model, root surface treatment with Denosumab 60 mg/mL prevented ankylosis, replacement resorption, and tooth resorption, 60 days after replantation, compared with the untreated group. Brown & Brenn staining showed a lower contamination in the mineralized tissues in the Denosumab surface treatment group, regardless of the concentration used. As for immunohistochemistry, Denosumab inhibited the synthesis of RANKL without modulating OPG. Periostin was observed in periodontal ligament of tooth replanted. However, this labeling was absent in the ankylosis areas, in both experimental periods, indicating that during the ankylosis process, the periostin synthesis is inhibited, resulting in the fusion between bone and root surface.

This thesis presents Photocatalytic TiOx layers created by own PECVD reactor assembled in the building of Department of Applied Physics and Technics. Parameters of depositions were optimalized as well as the PECVD reactor itself. Final layers are compared to layers made by Degussa P25. As a result based on the included measurements, this thesis tries to answer the question whether PECVD is the suitable method for depositions of photocatalytic layers.

Bien que dits « inoxydables », les aciers inox peuvent être sujets à diverses formes decorrosion localisée telles que la piqûration. La formation de piqûres, nuisible à l’aspect et à l’intégritéstructurelle du matériau, est notamment contrôlée par les propriétés du film passif protecteur qui seforme à la surface des inox. De nombreuses études ont été menées sur les mécanismes de piqûration desurfaces modèles préparées au laboratoire. Cette thèse, au contraire, étudie les relations entre lespropriétés physico-chimiques et électroniques, d’une part, et la résistance à la corrosion par piqûres,d’autre part, de films passifs formés sur des inox par des finis de surfaces industriels.Les propriétés des films passifs ont été caractérisées par des méthodes variées, utiliséesclassiquement ou de façon plus originale : multi-piqûres et transitoires électrochimiques pour lapropriété d’usage, XPS et SDL pour la chimie de surface, spectroscopie d’impédance électrochimique,chrono-ampérométrie et photoélectrochimie pour les propriétés semi-conductrices des films.Il a été montré que la résistance à la piqûration des finis industriels pouvait valablement êtredéterminée par la méthode des transitoires électrochimiques et par la multi-piqûres, utiliséesauparavant pour les seules surfaces modèles. Par ailleurs, l’analyse comparée des résultats depiqûration et de ceux d’XPS et SDL a mis en évidence que la composition chimique des films passifsne suffit pas à rendre compte des différences de résistance à la piqûration des différents finisindustriels testés. En revanche, l’analyse des propriétés semi-conductrices des différents films passifs apermis de proposer des explications à ces écarts de comportements en corrosion localisée, confirmantque structure et taux de défauts du film passif sont deux paramètres clef de la résistance à la corrosionpar piqûres des films passifs.Enfin, une amélioration du comportement en piqûration des surfaces industrielles a pu êtremise en évidence, soit après un traitement court de ces dernières en milieu nitrique acide, soit àl’application aux échantillons d’un balayage en potentiel en milieu sulfate neutre. / Stainless steels can suffer localized corrosion like pitting corrosion which can damage thestructural integrity of the material. The pit formation is mainly controlled by properties of theprotective layer formed on the stainless steel surface, which is called passive film. Many studies haveexamined pitting mechanism on model surface prepared in the laboratory. This work is dedicated tostudy the relations between physicochemical and electronic properties of industrially processedpassive films and their pitting corrosion resistance.The properties of passive films have been characterized with several methods which can beconventional or in a more innovative way: multi-pitting statistics and electrochemical noise for the useproperty, XPS and SDL for the surface chemistry, electrochemical impedance spectroscopy,chronoamperometry and photo-electrochemistry for semi-conductive properties of the passive films.Multi-pitting statistics and electrochemical transients which were usually used on modelsurfaces have been shown to be accurate for the evaluation of the pitting resistance of industrialsurface finishing samples. Furthermore, the comparison of the results of pitting resistance and of XPSand SDL analyses has shown that the chemical composition of passive films is not sufficient to explainthe difference of pitting resistance behavior among tested industrial passive films. However, the semiconductiveproperties characterizations are able to explain these differences of localized corrosionresistance. They confirm that structuration and defect level are two key parameters of pitting resistanceproperties of passive films.At last, this study highlighted that the pitting resistance of industrial passive films can beimproved by a short nitric acid treatment or by sweep voltammetry in neutral sulfate medium.

Made available in DSpace on 2014-10-09T12:42:05Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:52Z (GMT). No. of bitstreams: 0 / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Made available in DSpace on 2014-10-09T12:42:05Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:05:52Z (GMT). No. of bitstreams: 0 / Células a combustível de membrana polimérica têm cada vez mais se destacado como meio na obtenção de energia, pela sua alta eficiência e potencial para fazê-la de modo sustentável. Entretanto muitos ainda são os desafios para consolidá-la comercialmente. Dentre eles, a aglomeração e a perda de área ativa em catalisadores suportados em carbono recebem um destaque especial, principalmente em células PEM de temperatura elevada de operação. Eletrocatalisadores não suportados, baseados em nanoarquiteturas de geometria controlada, têm se tornado uma tendência em diversas frentes de pesquisa. Tal fato se deve à alta eficiência e estabilidade atingidas por sistemas nanométricos organizados, além da possibilidade em se criar superfícies funcionais adaptadas a reações específicas. O trabalho de pesquisa buscou o desenvolvimento de sistemas catalíticos não suportados, de alta área superficial, como alternativa a eletrocatalisadores nanoparticulados suportados em carbono, a fim de se reduzir a perda sobre a área ativa quando submetidos às condições de operação em células a combustível. O trabalho explorou dois conceitos, a confecção de nanotubos de platina e a confecção de nanofios nanoporosos à base de platina vítrea. Para este desenvolvimento foram estudados e caracterizados os efeitos da dissolução seletiva, em escala nanométrica, acoplados à conformabilidade de metais amorfos e à utilização da troca galvânica como ferramenta de síntese de superfícies. Tais estudos foram utilizados como base para o projeto de sistemas catalíticos não suportados. Os materiais propostos foram avaliados quanto a sua atividade e estabilidade frente a reações comuns em células a combustível. Tais sistemas demonstraram uma alta estabilidade em relação à sua área ativa, em ensaios de durabilidade, assim como uma alta utilização do metal nobre, tornando-os promissores para a tecnologia de células a combustível. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Made available in DSpace on 2014-08-20T14:30:09Z (GMT). No. of bitstreams: 1 Dissertacao_aline_oliveira_ogliari.pdf: 2899521 bytes, checksum: 3a5e7870376f999dd52a171e479c76e9 (MD5) Previous issue date: 2012-12-10 / The aim of this study was to develop a simplified method for bonding to yttriastabilized zirconia ceramic. The method was based on deposition of a reactive silica layer on the ceramic surface followed by heat treatment. The study comprised six steps: (i) preparation of solutions using four concentrations of tetraethyl orthosilicate (TEOS) and zirconium tert-butoxide (ZTB) diluted in hexane; (ii) cutting and polishing of the zirconia substrate; (iii) organic silica-based treatment before (infiltration, INF) or after (coating, COA) zirconia sintering; (iv) analysis by scanning electron microscopy and energy dispersive spectroscopy (SEM-EDS); (v) G-Raman confocal spectroscopy analysis; (vi) shear bond strength to zirconia tested after 24-h and failure analysis. An untreated (control) and a commercial reference (Rocatec Plus, 3M ESPE) groups were tested. Quantitative data were analyzed using ANOVA and Tukey s post hoc test (P < 0.05). SEM micrographs showed that zirconia surface was covered by silica nanoparticle clusters. EDS and G-Raman analyses confirmed composition of this layer. The bond strength results showed that most groups that received coating (COA) and infiltration (INF) presented higher bonding potential than the untreated (control) group. Almost all experimental groups were similar to commercial reference. Mixed failures were predominant. In conclusion, the present study introduces a novel, simple, and cost-effective method to provide adhesion to yttria-stabilized zirconia ceramic. Both the method of silica deposition (if before or after zirconia sintering) and concentration of organic silica precursors have a significant impact on the adhesion of methacrylates to the treated zirconia / O objetivo deste estudo foi desenvolver um método simplificado para obtenção de adesão a uma cerâmica de zircônia estabilizada por ítria. O método foi baseado na deposição de uma camada reativa de sílica na superfície cerâmica seguida por tratamento térmico. O estudo compreendeu seis etapas: (i) preparo de 4 soluções contendo tetraetilortosilicato (TEOS) e tert-butóxido de zircônio (ZTB) diluídos em hexano; (ii) corte e polimento do substrato de zircônia; (iii) tratamento com os precursores orgânicos antes (infiltração, INF) ou depois (cobertura, COA) da sinterização da zircônia; (iv) análise por microscopia eletrônica de varredura e espectroscopia de energia dispersiva (MEV-EDS); (v) análise por espectroscopia confocal G-Raman; (vi) avaliação de resistência de união ao cisalhamento 24h após preparo e análise de falha. Grupos sem tratamento (controle) e uma referência comercial (Rocatec Plus, 3M ESPE) foram testados. Dados quantitativos foram analisados usando ANOVA e teste post hoc de Tukey (P < 0,05). Os resultados de MEV mostraram que a superfície da zircônia foi coberta por aglomerados de nanopartículas de sílica, sendo esta composição confirmada por EDS e análise de G-Raman. Os resultados do teste mecânico mostraram que a maioria dos grupos que receberam cobertura (COA) e infiltração (INF) apresentaram maior resistência de união que o grupo sem tratamento (controle). A maioria dos grupos experimentais foram similares à referência comercial. Falhas do tipo mistas foram predominantes. Em conclusão, o presente estudo introduz um método novo, simples e de baixo custo para promover adesão a cerâmicas de zircônia estabilizada por ítria. Tanto o método de deposição de sílica (se antes ou após sinterização da zircônia) e a concentração de precursores orgânicos de sílica têm impacto significativo na adesão de metacrilatos à cerâmica tratada

Le couplage des traitements de surface mécaniques et thermochimiques a fait l’objet de nombreuses études ces dernières années. L’objectif d’un tel couplage est l’amélioration des cinétiques de diffusion d’espèces chimiques résultant en une augmentation des profondeurs de diffusion, et/ou une diminution de la température du traitement thermochimique sur les matériaux prétraités mécaniquement. Dans cette thèse, le procédé SMAT (Surface Mechanical Attrition Treatment) de nanocristallisation superficiel par déformation plastique sévère a été combiné avec la nitruration plasma sur un acier inoxydable 316L de qualité médicale. Ce procédé duplex permet une amélioration notable sur la capacité de diffusion de l’azote sous la surface de l’acier SMATé. Une étape intermédiaire entre le SMAT et la nitruration plasma a été proposée ; son rôle significatif pour la diffusion de l’azote a été démontré. Ainsi, la comparaison des résultats obtenus après la nitruration plasma sur les échantillons SMATés avec ceux uniquement nitrurés a permis de constater une augmentation jusqu’à 60% de l’épaisseur des couches nitrurées. Par ailleurs, de nombreux moyens de caractérisation ont été mis en œuvre à travers divers essais mécaniques de fatigue et de tribologie. Un modèle numérique multi-échelle de diffusion a également été développé pour simuler les profils de concentration d’azote après traitement duplex. Les profils de concentration d’azote simulés sont en bon accord avec les résultats expérimentaux / Coupled mechanical and thermochemical surface treatments have been the subject of much research effort in recent years. The goal of such a coupling is to improve diffusion kinetics leading to increased penetration depths, and/or to decrease the treatment temperature for mechanically pretreated materials. In this work, SMAT (Surface Mechanical Attrittion Treatment), used to refine the grain size by severe plastic deformation, is combined with plasma nitriding of a 316L medical-grade stainless steel. This duplex process significantly improves nitrogen diffusion. An intermediate treatment between SMAT and plasma nitriding is also proposed and its significant effect on the nitrogen diffusion is demonstrated. Comparisons between nitrided-only samples and duplex-treated samples have shown up to 60% increase of the nitrided layer thickness. In order to better understand the link between the generated microstructures and the mechanical fatigue and tribological responses, the samples have been characterised by many different techniques. Also, a multiscale numerical model of the diffusion process is proposed in order to simulate the nitrogen concentration profiles after duplex treatment. The simulated and experimental profiles correspond rather well

Cette thèse est consacrée à l’étude de films minces ouverts de cristaux liquides colonnaires sur un substrat solide. Ces matériaux, capables de s’auto-organiser en de larges domaines orientés, sont généralement obtenus à partir de molécules discotiques dérivées de colorants aromatiques. Ces différentes caractéristiques, associées à une bonne mobilité de charges, permettent d'envisager l'utilisation des cristaux liquides colonnaires en film mince dans des dispositifs photovoltaïques. Afin de bénéficier de leurs bonnes propriétés optoélectroniques, les cristaux liquides colonnaires doivent être déposés en film mouillant, d’épaisseur inférieure à 100 nm, et leur orientation contrôlée. Ainsi, pour des applications photovoltaïques, un alignement homéotrope (colonnes normales au substrat) est requis. Inversement, l’orientation planaire uniaxe (colonnes parallèles au substrat), est quant à elle requise pour une utilisation de ces composés dans les polariseurs ou dans les transistors organiques à effet de champ. Dans ce travail, différentes méthodes permettant de contrôler l’alignement de films minces ouverts de cristaux liquides colonnaires ont été développées, permettant d’obtenir aussi bien un ancrage homéotrope par traitement thermique spécifique, qu’un ancrage planaire uniaxe par dépôt préalable d’une couche de téflon. Le contrôle de l’orientation a ainsi permis d’une part de produire un film mince (e ? 50 nm) mouillant en ancrage homéotrope ouvrant la voie vers des cellules solaires organiques efficaces, et d’autre part de déterminer l’ensemble des propriétés optiques (indices complexes anisotropes) de ces matériaux cristallins liquides colonnaires. La dynamique du démouillage et l’état d’équilibre d’un film mince ouvert de cristal liquide colonnaire ont également été étudiés. Les résultats expérimentaux révèlent la formation de gouttelettes anisotropes et la présence d’un film nanométrique lors du démouillage de ce film mince / This thesis deals with columnar liquid crystal studied in the geometry of open supported thin films. Columnar liquid crystals are usually made of disk-shaped molecules derived from aromatic dyes. They are efficient charge transporters with the added capacity to self-assemble in large oriented domains. Consequently, such materials may be used in photovoltaic devices. In order to benefit from their good uniaxial charge mobility, their organization has to be controlled in uniform oriented thin films in the range of thicknesses of typically 100 nm. Homeotropic alignment (columns normal to the interface) is required for solar cells whereas uniaxial planar anchoring (columns parallel to the interface) is needed for applications such as polarizers or organic field effect transistor. Different methods to monitor the alignment in open thin films have been developed in this work, which make possible to achieve either homeotropic anchoring by a specific thermal treatment, or uniaxial planar orientation using a Teflon layer. Based on these orientation skills, a uniform ultra-thin film, free of dewetting and homeotropically oriented, is achieved (down to 50 nm thick) opening the way towards efficient solar cells, and a complete study of the optical properties has been performed (with the determination of the anisotropic complex indices) for different columnar liquid crystals. The dynamics of dewetting and the equilibrium state of a thin supported film have also been investigated. Experimental results show the formation of anisotropic droplets and reveal a nanometric film during dewetting.

Complex thermal barrier coating systems are one the most efficient high-temperature surface treatments which open up practical applications in land-based turbines and air jet engines. In the case of most exposed rotor and stator jet engine components, the combination of thermal barrier coatings together with the inner cooling system made it possible to increase working temperature by several tens of degrees of Celsius. Nevertheless, it is very difficult to achieve any further increase in working temperature by using the conventional thermal barrier coatings based on the ZrO2-Y2O3 ceramic top coat and the MCrAlY metallic bond coat, which currently work at their material limits. The working temperature inside the combustion chamber of the jet engine is proportional to engine’s efficiency and inversely proportional to fuel consumption and production of undesirable CO2 emission. Therefore, a considerable effort has recently been devoted to research and development of new types of ceramic coatings that can withstand long term extreme working conditions. New design approaches of multi-layer composite thermal barrier coating systems can sustain the required trend of increasing working temperature of jet engines mainly because of possibility of optimization of high-temperature durability and long lifetime. The theoretical part of thesis provides a fundamental overview of thermal barrier coatings, their properties, deposition technologies and testing methods. The experimental part is focused on optimization of deposition parameters of conventional ZrO2-Y2O3 / MCrAlY thermal barrier coatings prepared by means of atmospheric plasma spraying. Furthermore, a novel multi-layer thermal barrier coating system based on ZrO2-Y2O3-Al2O3-SiO2 / ZrO2-Y2O3 / MCrAlY, which contains amorphous and/or nanocrystalline regions, is developed, tested and characterized as well. Structural stability, phase transformations and growth of the thermally grown oxide in both conventional and experimental systems after high-temperature isothermal oxidation, cyclic oxidation and burner-rig tests were evaluated by means light microscopy, scanning electron microscopy with energy-dispersive microanalysis and X-ray diffraction. In comparison with the conventional thermal barrier coatings, the novel multi-layered systems have lower thermal conductivity, slower thermally grown oxide kinetic, better structural stability, and generally higher lifetime in all high-temperature tests.

This diploma thesis is focused on the description and summary of existing knowledge about vibro-pressed concrete products with treated surface with protective coating, that is hardering by ultravioled and infrared radiation. The theoretical part describes the production of vibro-presses products, possible wayt of finishing the surface including the description of the most commonly used materials and the methods of application and hardering of protrctive coating on the surface. Another point of the theoretical part is creating of lime efflorescence on the concrete surface and their subsequent disappearance. The experimental part of the thesis is ficused on obtaining information about the properties of the modified pavements by these techologies and comparing the acquired properties with the charakteristice of the reference pavements that do not have any protective coating on their surface.