Avaliação da \"qualidade\" da microarquitetura óssea contribui na prevenção e risco de fraturas associado a osteoporose. Amostras de ossos trabeculares de corpos vertebrais da região T12, L1 e L4 de 30 de indivíduos (cadáveres humanos), classificados pela técnica de ultrassonometria de calcâneo como normais, osteopênicos e osteoporóticos foram utilizadas. Os parâmetros histomorfométricos, físicos e mecânicos da microarquitetura analisados pela técnica de microtomografia de raios-X, ensaios mecânicos de compressão axial e nanoindentação. Baseado nestes parâmetros, constantes elásticas efetivas globais foram obtidas pela técnica homogeneização assintótica para estrutura tipo-placa. Teste ANOVA apresentou diferenças, muito e extremamente significativas para densidade linear estrutural (p = 0,017), grau de anisotropia (p = 0,042), auto valor (p = 0,045), número de Euler (p = 0,016), idade (p = 0,009), separação trabecular (p = 0,009), densidade de conectividade (p = 0,006), módulo de elasticidade (p = 0,001), tensão máxima no limite de resistência a fratura (0,001), índice de qualidade óssea do calcâneo (p = 0,0001), fração de volume ósseo (p = 0,0001), espessura trabecular (p = 0,0002), dimensão fractal (p = 0,0002), momento de inércia polar médio (p = 0,00005), excentricidade (p = 0,0002), fração de porosidade (p = 0,0001) e densidade mineral óssea aparente (p = 0,00005) entre os grupos. O teste de Spearman identificou correlação moderada, alta e muito alta dos valores da tensão máxima no limite de resistência a fratura com os parâmetros de idade (r = -0,684), fração de volume ósseo (r = 0,762), fator de forma trabecular (r = -0,754), espessura trabecular (r = 0,675), densidade linear trabecular (r = 0,622), autos valores (r = -0,615), dimensão fractal (r = 0,855), momento de inércia polar médio (r = 0,816), excentricidade (r = -0,569) e fração de porosidade (r = -0,762). Estes parâmetros são indicadores da qualidade da microarquitetura óssea trabecular e risco de fratura associado a osteoporose. / Evaluation of the \"quality\" of bone microarchitecture can contribute to the prevention and risk of fractures associated with osteoporosis. Samples of trabecular bone from the vertebral regions T12, L1 and L4 from the bodies of 30 individuals (human cadavers), classified by ultrasonometry technique calcaneus as normal, osteopenic and osteoporotic were used. The histomorphometric, physical and mechanical parameters of the microarchitecture were analyzed by X-ray microtomography technique, mechanical tests of axial compression and nanoindentation. Based on these parameters, globally effective elastic constants were obtained by asymptotic homogenization technique for type-plate structure. ANOVA test showed differences that were very and extremely significant for the following: structural linear density (p = 0.017) anisotropy (p = 0.042), auto value (p = 0.045), Euler number (p = 0.016), age (p = 0.009), trabecular separation (p = 0.009), connectivity density (p = 0.006), elastic modulus (p = 0.001), maximum stress fracture strength limit (0.001), bone quality score of the calcaneus (p = 0.0001), bone volume fraction (p = 0.0001), trabecular thickness (p = 0.0002), fractal dimension (p = 0.0002), mean polar moment of inertia (p = 0.00005), eccentricity (p = 0.0002), porosity fraction (p = 0.0001) and apparent bone mineral density (p = 0.00005) between groups. The Spearman test identified moderate correlation, high and very high values of maximum stress fracture resistance limit for the following parameters: age (r = -0.684), bone volume fraction (r = 0.762), trabecular bone pattern factor (r = -0.754), trabecular thickness (r = 0.675), trabecular linear density (r = 0.622), auto value (r = -0.615), fractal dimension (r = 0.855), mean polar moment of inertia (r = 0.816), eccentricity (r = -0.569) and porosity fraction (r = -0.762). These parameters are quality indicators of the microarchitecture of trabecular bone and fracture risk associated with osteoporosis.

Un 1er travail a étudié les effets osseux mandibulaires de l’injection unilatérale dans les muscles masticateurs de toxine botulique (BTX) chez le rat adulte. Ceci entraine une perte osseuse mandibulaire condylienne et alvéolaire homolatérale importante. Une hypertrophie osseuse de l’enthèse d’insertion mandibulaire du muscle digastrique a été observée et pourrait correspondre à une étiologie pour les tori. Les effets de la BTX sur le cartilage articulaire condylien mandibulaire dans le même modèle animal ont été recherchés par analyse microtomographique du cartilage articulaire après augmentation de contraste à l’acétate d’uranyle. Aucune différence d’épaisseur cartilagineuse n’a été mise en évidence entre les groupes contrôles et BTX.Le 3ème travail a consisté en l’étude histologique et microtomographique des tori mandibulaires chez l’homme.Les tori sont différents des exostoses des os longs par plusieurs caractéristiques (dont l’absence de Fe et Al dans la matrice osseuse) et une asymétrie du remodelage osseux a été mise en évidence.La 4ème partie a consisté en l’étude de la qualité osseuse et de la microvascularisation alvéolaire dans un modèle animal d’ostéonécrose mandibulaire (ONM) aux bisphosphonates (BP). Des signes cliniques et microtomographiques d’ONM ont été observés dans la majorité des cas. La minéralisation osseuse était plus élevée après imprégnation en BP. La microvascularisation osseuse alvéolaire apparaissait augmentée après avulsion dentaire chez les animaux contrôles mais pas chez les animaux ayant reçu des BP témoignant ainsi d’un effet anti angiogénique in vivo des BP qui pourrait jouer un rôle dans la physiopathologie de l’ONM. / First, bone changes at the mandible were studied after a unilateral botulinum toxin (BTX) injection in masticatory muscles in adult rats. A major alveolar and condylar bone loss was evidenced. The occurrence of a hypertrophic bone metaplasia at the digastric muscle enthesis was evidenced as well. This could constitute an etiological factor for tori. Then, condylar articular cartilage changes at the mandible were studied in the same BTX animal model, using microtomography after contrast enhancement of cartilage with uranyl acetate. Cartilage thickness measurement showed no difference when comparing control and BTX groups.A third work studied mandibular tori in human using histologic and microtomographic techniques. Tori appeared different from long bone exostoses by several characteristics (absence of Fe and Al in the bone matrix) and a specific asymmetric bone remodeling was evidenced.The fourth part consisted in the study of alveolar mandibular vascularization and quality of the bonematrix in an animal model of osteonecrosis of the jaws(ONJ) after bisphosphonates (BP) injections. Clinical and microtomographic signs of ONJ were found in mostof the cases. An increased mineralization of the alveolar bone was observed after BP impregnation. Microvascularization was increased after tooth extraction in the alveolar bone of control animals but it was impaired in ZA treated rats. Such an in vivo antiangiogenic effect of BPs could play a role in the pathophysiology of ONJ.

Les roches mantelliques exposées sur le plancher océanique et/ou en contact avec l’atmosphère au niveau d’une ophiolite, sont en déséquilibre et s’altèrent, via les réactions de serpentinisation (i.e. d’hydratation et oxydo-réduction) et les réactions de carbonatation. Ces réactions d’altération jouent un rôle important dans les échanges chimiques entre la Terre profonde et les enveloppes externes, en particulier dans le cycle des volatils (C, H et O) via la minéralisation du CO2 atmosphérique, la production d’hydrogène et la formation d’hydrocarbures et de molécules prébiotiques. L’ophiolite d’Oman est un « laboratoire naturel » idéal pour étudier ces réactions depuis l’hydrothermalisme océanique jusqu’à l’altération continentale actuelle.Cette thèse présente les résultats d’une étude multi-technique et multi-échelle réalisée sur une série de péridotites serpentinisées et carbonatées échantillonnées sur deux sites, Wadi Dima et Batin (Massif de Wadi Tayin), considérés comme représentatifs des processus d’altération affectant l’ophiolite d’Oman. Ces travaux combinent caractérisations (micro-)structurales (EBSD, µ-tomographie), pétrographiques et minéralogiques (Raman, Cathodoluminescence, (3D-)XANES), et analyses géochimiques (EPMA, (LA)-ICPMS) et isotopiques (isotopes du O, C micro-bulk et in-situ).L’étude des harzburgites de Wadi Dima a permis d’identifier la succession des épisodes de serpentinisation et de carbonatation qui ont affecté les péridotites lors du refroidissement de la lithosphère jusqu’à la mise en place de l’Ophiolite d’Oman. La serpentinisation commence en domaine océanique (appauvrissement en REE, anomalie négative en Ce) durant le refroidissement initial de la lithosphère océanique et/ou au début du détachement intra-océanique à < 200-220°C, par la formation des veines de lizardite. Cette serpentinisation continue avec la formation de chrysotile au centre de la structure maillée, remplaçant l’olivine. Le dernier stade de serpentinisation a lieu simultanément au premier stade de carbonatation et engendre l’altération complète de la péridotite à < 100°C. Le système est contrôlé par des hétérogénéités locales (anomalies en Ce et variation de la composition isotopique en carbone). La carbonatation continue à < 50°C lors de la transition en domaine continental. Des veines de carbonates se forment par interaction avec des fluides issus des sédiments durant la convergence et avec des fluides de surface et de sub-surface durant l’altération actuelle de l’ophiolite. Ce processus marque le passage d’un régime hydrothermal océanique dont la chimie est dominée par la composition de la roche, à un régime hydrothermal continental dont la chimie est contrôlée par la composition du fluide dans des fractures. Paradoxalement, la structure initiale du manteau contrôle l’orientation et la distribution des veines de carbonate.Le site de Batin se distingue par sa structure complexe avec la présence de nombreux filons de gabbros et de pyroxénites et des évidences d’imprégnation magmatique. La serpentinisation y est marquée par la formation de textures atypiques en anneau ("fingerprint") caractérisées par des variations des teneurs en Fe-Mg et du redox à micro-échelle et par des compositions isotopiques en oxygène en déséquilibre. Ces caractéristiques sont interprétées comme résultant de déséquilibres locaux dans les processus de transport-nucléation-réaction pouvant être liés à plusieurs paramètres : forts gradients de température, redox, composition du fluide, et de perméabilité.Cette thèse apporte de nouvelles données vis-à-vis des relations temporelles et spatiales entre les réactions de serpentinisation et de carbonatation, les hétérogénéités chimiques à micro-échelle et l’impact de ces réactions d’altération sur les bilans globaux des volatils (C, H et O) en Oman. Elle met particulièrement en évidence la possibilité de stocker du CO2 et de produire de l’H2 simultanément lors de l’altération du plancher océanique. / Mantle rocks exposed in seafloor and/or directly in contact with atmosphere in ophiolite system are thermodynamically and chemically in disequilibrium. Mantle alteration is driven by serpentinization (ie, hydration and oxidation-reduction reactions) and carbonatization reactions. These reactions play an major role in the chemical exchanges between the deep mantle and the outer envelops, especially in the global mass budget of volatiles (C, H and O) via CO2 mineralization, hydrogen production and formation of hydrocarbons and prebiotic molecules. Oman ophiolite is an ideal "natural laboratory" for studying alteration reactions in mantle rocks from ocean hydrothermalism to modern continental weathering.This thesis presents the results of a multi-technical and multi-scale study on carbonate-hosted serpentinized peridotites in two sites, Wadi Dima and Batin (Wadi Tayin massif), considered representative of the alteration processes affecting the Oman ophiolite. This work combines (micro-) structural (EBSD, µ-tomography), petrographical (EPMA), mineralogical (Raman, Cathodoluminescence, (3D-)XANES), geochemical ((LA)-ICPMS) and isotopic studies (O, C in situ and micro-bulk).Studies in Wadi Dima harzburgites have highlighted successive episodes of serpentinization and carbonatization in Oman peridotites from oceanic lithosphere cooling to Oman Ophiolite emplacement. Serpentinization occurs in oceanic setting (REE depletion, negative Ce anomalies), probably during the onset of the oceanic lithosphere cooling and / or of the intra-oceanic detachment, at < 200-220°C, driven by the formation of lizardite veins constituting the mesh structure. Serpentinization continues at lower temperature with the formation of chrysotile in the center of the mesh structure, replacing olivine. The last stage of serpentinization is concurrent with early carbonatization and generates the complete peridotite alteration at < 100°C. In this rock-dominated system, fluid flow paths are controlled by nano-porosity (etch pits), by pore scale weakness and by local heterogeneity in permeability, generating local chemical heterogeneities (Ce anomalies variability and carbon isotope heterogeneity). Carbonatization continues at < 50°C during the transition in continental setting. Carbonate veins are formed during interaction with sediment-derived fluids during intra-oceanic detachment at the onset of obduction and with surface and sub-surface fluids during modern continental Ophiolite weathering. This process records the transition from oceanic diffuse-flow rock-dominated to cooler continental fluid-focused-flow fluid-dominated hydrothermal systems. Paradoxically, initial mantle structure controls orientation and distribution of carbonate veins.Batin site is distinguished by its complex structure with the presence of abundant gabbros and pyroxenites dikes, evidence of magmatic impregnation peridotites. Serpentinization is charcheterized by the formation of an uncommon texture in rings ("fingerprint") at the expense of olivine, marked by chemically variation in Fe-Mg and redox at microscale and by disequilibrium oxygen isotopic composition. These features are interpreted as resulting from local disequilibrium in the transport-nucleation-reaction processes that may be related to several parameters: high temperature gradient, redox, fluid composition, and permeability.This thesis brings new constraints on temporal and spatial relations between serpentinization and carbonatization reactions, on local chemical heterogeneities at micro-scale and on the global chemical budget of volatiles (C, H and O) in Oman peridotites. It has highlighted the possibility to store CO2 and producing H2 simultaneously during subseafloor alteration.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Nesta dissertação de Mestrado do programa de Pós-Graduação em Ciência e Tecnologia dos Materiais é apresentado um estudo para a caracterização do concreto reforçado com fibras de polipropileno e de aço pela análise das imagens de microtomografia computadorizada por transmissão de raios X (&#956;CT). Foram produzidos corpos de prova de concreto para determinar a sua resistência mecânica à compressão. As imagens foram obtidas no sistema Skyscan, modelo 1174, reconstruídas e analisadas. Foi possível observar na análise das imagens a estrutura da fibra de aço dispersa na matriz do concreto e quantificá-las pelo programa de análise de imagens Ctan e perceber um ganho na resistência mecânica em relação ao concreto sem fibras. Não foi feito a quantificação das amostras de fibras de polipropileno dispersas na matriz de concreto, mas foi observada a presença de aglomerados dessa fibra que resultaram na perda da resistência mecânica em relação ao concreto sem fibras. / In this dissertation Masters Program Graduate in Science and Technology of Materials is presented a study for characterization of concrete reinforced with polypropylene fibers and steel by image analysis of computed microtomography X ray transmission (&#956;CT). Concrete samples were produced to determine their mechanical resistance to compression. The images were obtained in the SkyScan model 1174, reconstructed and analyzed. It was possible, in image analysis, to observe the structure of steel fiber dispersed in the concrete matrix and quantify them by image analysis program Ctan and observed a gain in strength compared to concrete fiber less. The quantification was not did to samples of polypropylene fibers dispersed in the matrix of concrete, but we observed the presence of clusters fibers resulting in the loss of mechanical strength compared to concrete fiber less.

O desenvolvimento econômico brasileiro depende da crescente produção agropecuária, aliada ao conservacionismo. O sistema de plantio direto é o manejo de solo que reúne o mais amplo conjunto de preceitos da agricultura conservacionista. As áreas agrícolas cultivadas sob plantio direto, entretanto, têm apresentado duas camadas de solo distintas: uma entre, aproximadamente, 0 e 7 cm de profundidade, com condições físicas e químicas favoráveis ao desenvolvimento radicular; e uma entre, aproximadamente, 7 e 20 cm de profundidade, com menor permeabilidade do solo ao ar e a água, elevada resistência à penetração e baixa fertilidade química do solo. Estas condições promovem a concentração do sistema radicular das plantas agrícolas cultivadas na camada mais superficial do solo (0 a 7 cm), motivando perdas de produtividade por estresse hídrico. A magnitude desse problema se estende a mais de 30 milhões de hectares de lavoura cultivada sob plantio direto no Brasil, colocando em risco as projeções de exuberância da agricultura no país. Assim, o desenvolvimento desta tese teve o objetivo de estudar fatores que, além do processo de compactação mecânica do solo, possam estar promovendo a estratificação física e química de solos altamente intemperizados cultivados sob sistema de plantio direto. Dentre os possíveis fatores causadores deste tipo de degradação, foram avaliados: i) a aplicação excessiva de calcário, exclusivamente em superfície, ocasionando, na camada de 0 a 7 cm, a elevação do pH do solo para além do ponto de carga zero do solo, elevando o potencial eletronegativo do solo e por consequência, promovendo a dispersão de argila; ii) a migração da argila dispersa no perfil do solo, pela água de percolação, como um fator promotor de degradação física em subsuperfície; iii) o aporte de fitomassa ao solo em quantidade e qualidade para manter a estabilidade estrutural dos solos cultivados. Os resultados obtidos mostraram que o movimento de calcário no perfil dos solos estudados é muito lento, limitando o efeito deste produto a poucos centímetros abaixo do local onde ele é depositado ou incorporado (2,5 cm em 130 semanas), independentemente da dose aplicada (até 33,2 Mg ha-1). Assim, a calagem superficial promove e intensifica a estratificação dos atributos químicos no perfil do solo, aumentando, demasiadamente, o pH próximo à superfície e sendo ineficiente em mitigar a acidez na subsuperficie destes solos. A concentração de calcário na camada mais superficial dos solos altamente intemperizados aumenta a eletronegatividade do solo, resultando na dispersão de argila. A migração dos argilominerais dispersos no perfil do solo, pela água de percolação, promove uma série de alterações estruturais, incluindo a diminuição da porosidade total e da continuidade dos poros e o aumento da densidade e da resistência do solo à penetração na camada subsuperficial. A diminuição da estabilidade estrutural dos Latossolos sob cultivo também está ligada ao aporte de material orgânico ao solo em quantidade e qualidade inferiores à que ocorre no solo sob sistema nativo. Os Latossolos cauliníticos são mais propensos a diminuição da estabilidade estrutural quando submetidos ao cultivo. Portanto, a recomendação de calagem em solos altamente intemperizados cultivados sob plantio direto, precisa considerar a mineralogia do solo e a possível degradação estrutural promovida pela calagem em excesso. / The economic development of Brazil depends upon the increasing agricultural production associated with conservation practices. The no-tillage system is the soil management practice that brings together the broadest set of principles for conservation agriculture. Areas under no-till system, however, generally have two completely different soils layers: a surface layer, around 0 to 7 cm, with physical and chemical conditions favorable for root development; and a sub-surface layer, around 7 to 20 cm, with lower permeability to air and water, high soil penetration resistance, and low soil fertility. The existence of these stratified layers dramatically restricts the development of the root system into the sub-surface soil layer, which may result in reducing plant productivity by water deficit. This problem exists on more than 30 million hectares cultivated under no-tillage system in Brazil, and can compromise the optimistic projections of agricultural growth in the country. Therefore, more research is necessary to explore challenges that come with no-tillage. The aim of this thesis was to study the factors that can promote the physical and chemical stratification of highly weathered soils cultivated under no-till system. Among the factors that could cause this degradation, the following were studied: i) the application of excessive lime only on surface soil, or into the uppermost soil layer, which can increase its pH to levels beyond of the zero point of charge of soil, raising its electronegative potential and promoting, as a consequence, the clay dispersion; ii) the dispersed clay migration thtough the soil profile, by the percolation water, as a factor of physical degradation of sub-surface of soil cultiveted under no-tillage; and iii) the aplication of phytomass to the soil in insufficient amount and quality to maintain the soil structural stability of the soil. The results of this study showed that lime movement into the deeper soil profile, is very slow, as its impacts are limited to just a few centimeters below of where it is applied or incorporated (2.5 cm after 130 weeks), independent of the applied amount of lime. Thus, the surface lime application intensifies the chemical stratification of the clayey soils under no-tillage, increasing to much the soil pH of the uppermost soil layer, and being inefficient to decrease the soil acidity in the subsurface soil layer. The concentration of lime into the uppermost soil layer can significantly increase the electronegativity of the soil system and result in clay dispersion in the topsoil layer (0 to 5 cm). The resulting clay migration into the soil profile led to a series of structural alterations in subsurface layers, including: decrease of both soil porosity and pore continuity; and increase of both soil bulk density and soil penetration resistance in the sub-superficial layer. The structural stability decreasing of Oxisols under no-till system also is linked with the low addition of organic matter to the cultivated soil, in relation to the non-cultivated soils. The kaolinitic Oxisols are more susceptible to degradation than the gibbsitic Oxisols. Thus, it could be conclude that liming practices (rate and application methods of lime), mainly under no-till systems, need to consider both type and mineralogy of soil, as well as considering soil structure degradation promoted by over-liming in the uppermost soil layer.

Submitted by Daniella Santos (daniella.santos@ufma.br) on 2017-06-20T14:13:09Z No. of bitstreams: 1 Lauber Jose.pdf: 935752 bytes, checksum: 4853ee9a573d926513f92f2560f03c9a (MD5) / Made available in DSpace on 2017-06-20T14:13:10Z (GMT). No. of bitstreams: 1 Lauber Jose.pdf: 935752 bytes, checksum: 4853ee9a573d926513f92f2560f03c9a (MD5) Previous issue date: 2017-06-12 / FAPEMA / The polymerization shrinkage (PS) and the detrimental effects have been the focus of studies with the aim of improving the performance of composite resins. The simplicity of technique due to the possibility of single fill in large quantities have allowed bulk fill composite resins (BFC) to be indicated to minimize this shrinkage. This thesis, divided in two chapters, aimed to evaluate the behavior of bulk fill composite resins in class I restorations by mans computerized microtomography (μCT) and microtensile bond strength (μTBS). Chapter I evaluated the PS and μTBS in BFC and conventional class I restorations composite resins, and the correlation between these factors. Class I cavities (4 x 5 x 4 mm), (factor-C = 4.2), were created in human third molars that were free of caries, which were randomized and divided into 4 groups (n = 6): Z350 XT(+): incremental insertion (II) and manual fill (MF); Z350 XT(-): single insertion (SI) and MF; TBF (Tetric N-Ceram Bulk Fill: SI and MF); and SFU [SonicFill: SI and ultrasonic fill (UF) ]. The teeth were scanned and analyzed in μCT at two times: T0- after the filling of the cavity with composite resins and T1- after the polymerization for PS. After 1 week, the teeth were sectioned crosswise in the buccolingual and mesiodistal directions to obtain specimens with approximately 1 mm² thickness and fixed to universal test machine device to perform μTBS. The data showed a statistically significant difference for PS between the groups Z350 XT(+) e Z350 XT(-), and between SF e Z350 XT(-) (Kruskal-Wallis and Dunn, p<0.05). he μTBS was higher for Z350 XT (+) than the other groups (p <0.05) and there was no correlation between PS and μTBS (p> 0.05). It was concluded that the BFC type present a PS similar to that of the conventional nanoparticulate composite resin inserted using the incremental technique. The bond strength was higher for the composite resin incrementally inserted, which presented a lower number of pre-test failures when compared to bulk fill composites. No correlation was observed between the PS and bond strength when bulk fill and conventional composites were used. Chapter II evaluated the volume of polymerization shrinkage (VS), gap (VG) and void (VV) using μCT in BFC and conventional class I restorations, and their correlations. Class I cavities (4 x 5 x 4 mm), factor-C = 4.2, were created in human third molars that were free of caries, which were randomized and divided into 5 groups (n = 6): Z350 XT(+) (II/MF); Z350 XT(-) (SI/MF); TBF (SI/MF); SFM [ (SonicFill: SI and MF) ] and SFU (SI/UF). The teeth were scanned and analyzed in μCT at two times: T0- after the filling of the cavity with composite resins and T1- after the polymerization for VG and VV, and for VS (T1-T0). After 1 week, the teeth were sectioned crosswise in the buccolingual and mesiodistal directions to obtain specimens with approximately 1 mm² thickness and fixed in a universal testing machine to perform μTBS. Kruskal-Wallis and Dunn tests showed statistically significant difference in VS for groups Z350 XT(+) and Z350 XT (-), and between SFU and Z350 XT(-), and difference between VV for Z350 XT(+) and BFC (p <0.05). There was no difference in VG between the conventional and BFC (p>0.05). There is a positive correlation between VS versus VG and between VS versus VV (Spearman, p <0.05). It was concluded that BFCs of both sonic and manual insertion showed polymerization shrinkage and gap formation similar to the incrementally inserted nanoparticulate conventional resin. There is a positive correlation between polymerization shrinkage and final gap formation, as well as between polymerization shrinkage and void in composite resins. The final gap was formed mainly by the initial gap generated during the insertion/filling of the composite in the cavity and not to the polymerization shrinkage. / A contração de polimerização (CP) e seus efeitos prejudiciais vêm sendo o foco de estudos com o intuito de melhorar o desempenho das resinas compostas. A simplicidade da técnica devido a possibilidade de preenchimento único em grande quantidade tem permitido que resinas bulk fill (RBF) sejam indicadas para minimizar essa contração. Esta tese, dividida em dois capítulos, teve por objetivo avaliar o comportamento de resinas bulk fill em restaurações classe I por meio de microtomografia computadorizada (μCT) e resistência de união por microtração (μTBS). O capítulo I avaliou a CP por μCT e a μTBS em restaurações classe I de RBF e convencional, e a correlação entre esses fatores. Cavidades classe I (4x5x4 mm), (fator-C=4,2) foram realizadas em terceiros molares livres de cárie, que foram randomizados e divididos em 4 grupos (n=6): Z350 XT(+): inserção incremental(II) e preenchimento manual (PM); Z350 XT(-): inserção única (IU) e PM; TBF (Tetric N Ceram Bulk Fill: IU e PM); e SFU [SonicFill: IU e preenchimento ultrassônico (PU) ]. Os dentes foram escaneados e analisados em μCT em dois tempos: T0- após o preenchimento da cavidade com resinas compostas e T1- depois da polimerização para CP. Após 1 semana os dentes foram seccionados transversalmente no sentido vestíbulo-lingual e mesio-distal para obtenção de espécimes com aproximadamente 1mm² de espessura, e fixados em dispositivo para máquina de ensaio universal para realizar μTBS. Os dados demonstraram diferença estatisticamente significante para a CP entre os grupos Z350 XT(+) e Z350 XT(-) e entre SFU e Z350 XT(-) (Kruskal-Wallis e Dunn, p<0.05). A μTBS foi maior para Z350 XT(+) em relação aos demais grupos (p<0.05) e não houve correlação entre CP e a μTBS (p>0.05). Concluiu-se que RBF apresentaram CP semelhante à resina convencional nanoparticulada inserida de forma incremental. A resistência de união foi maior para a resina convencional inserida pela técnica incremental que apresentou menor falhas pré-teste, quando comparada às RBF. Não foi observada correlação entre a CP e a resistência de união quando utilizadas RBF e convencionais. O capítulo II avaliou o volume de contração de polimerização (VC), gap (VG) e poro (VP) usando μCT em restaurações classe I de RBF e convencional, e suas correlações. Cavidades classe I (4x5x4 mm), fator-C=4,2, foram realizadas em terceiros molares humanos livres de cárie que foram randomizados e divididos em 5 grupos (n=6): Z350 XT(+) (II/PM); Z350 XT (-) (IU/PM); TBF (IU/PM); SFM [ (SonicFill (IU/PM) ] e SFU (IU/PU). Os dentes foram escaneados e analisados em μCT em dois tempos: T0- após o preenchimento da cavidade com resinas compostas e T1- depois da polimerização para VG e VP, e VC (T1-T0). Após 1 semana os dentes foram seccionados transversalmente no sentido vestíbulo-lingual e mesio-distal para obtenção de espécimes com aproximadamente 1mm² de espessura, e fixados em máquina de ensaio universal para realizar μTBS. Os testes de Kruskal-Wallis e Dunn, demonstraram diferença estatisticamente significante no VC em μCT para os grupos Z350 XT(+) e Z350 XT (-) e entre SFU e Z350 XT(-), e diferença entre o VP para Z350 XT(+) e as RBF (p<0.05). Não houve diferença para o VG entre as RBF e convencional (p>0.05). Houve correlação positiva entre a VC versus VG e entre VC versus VP (Spearman, p<0.05). Concluiu-se que as RBF tanto de inserção sônica quanto manual mostraram contração de polimerização e formação de gap semelhante à resina convencional nanoparticulada inserida de forma incremental. Há uma correlação positiva entre a contração de polimerização e a formação de gap final, assim como entre a contração de polimerização e poro nas resinas compostas. O gap final foi formado principalmente pelo gap inicial gerado durante a inserção/preenchimento da resina na cavidade e não à contração de polimerização.

Cette thèse sinscrit dans une dynamique de recherche qui a vu le jour assez récemment dans le domaine du séchage des boues de station dépuration. Conscientes des problèmes de gestion que va entraîner laugmentation des quantités de boue produites suite à lapplication de la législation européenne, différentes équipes de recherche se sont lancées dans létude du séchage des boues. Considérant que lépandage agricole et la valorisation énergétique demeureront les principales filières délimination pour les boues, le séchage constitue, dans les deux cas, une étape essentielle après la déshydratation mécanique. Lambition de ce travail est de contribuer à améliorer les connaissances dans le domaine du séchage convectif des boues et à mieux appréhender les changements de texture qui surviennent au cours du séchage à laide de la microtomograhie à rayons X. Le chapitre I décrit le contexte général dans lequel se situe le travail, cest-à-dire lépuration des eaux usées et la production de boues qui en résulte. La place du séchage dans les différentes filières de valorisation, compte tenu des exigences de la législation européenne, est présentée. Ensuite, un état des connaissances dans le domaine du séchage des boues ainsi quune présentation des technologies de séchage actuellement mises en oeuvre sont effectués. Ce chapitre met en évidence que létat divisé de la matière se situe au cur du travail et pose les objectifs majeurs de la présente étude. Le chapitre II est consacré à la définition des notions essentielles à létude du séchage. Le concept disotherme de sorption à leau est présenté avant de passer en revue les différents types deau que lon trouve dans les boues. Les modes de transport deau pendant le séchage sont ensuite rappelés. La suite du chapitre se concentre sur la manière dont les données de séchage sont exploitées et reprend, brièvement, les progrès effectués en modélisation de la cinétique. La fin du chapitre décrit le retrait qui constitue un phénomène indissociable du séchage des matériaux déformables dont font partie les boues. Lensemble des dispositifs expérimentaux et des méthodes utilisés au long de ce travail sont décrits dans le chapitre III. Les principaux dispositifs expérimentaux sont la cellule de filtration sous pression, le système dextrusion des échantillons, le microsécheur convectif et le microtomographe à rayons X. Les méthodes décrites concernent la caractérisation des boues, la déshydratation des boues, le filtrage des courbes de séchage, lexploitation des coupes tomographiques par analyse dimages et la manière de rassembler les informations issues du séchage et de la microtomographie. Le chapitre IV est consacré au développement dune procédure de conditionnement et de déshydratation permettant dobtenir une boue déshydratée dont la siccité est la plus élevée et la plus reproductible possible. La mise au point de cette procédure permet deffectuer cette étude sur des boues réelles. Les boues sont prélevées après létape dépaississement dans deux stations dépuration gérées par lAIDE, à Retinne et à Embourg. Les gâteaux de boue obtenus sont ensuite caractérisés : les propriétés rhéologiques sont déterminées ainsi que le taux deau liée par lintermédiaire des isothermes de désorption à leau. Des essais de séchage sur des échantillons extrudés à partir du gâteau de filtration montrent que les conditions opératoires de conditionnement et de déshydratation des boues nont pas dinfluence significative sur la cinétique. La procédure de production déchantillons mise au point (conditionnement-filtration-extrusion) est utilisée dans toute la suite du travail. Tout au long du chapitre V, linfluence de trois variables opératoires (la température, la vitesse superficielle et lhumidité absolue de lair) sur le retrait, la cinétique de séchage, la fissuration et le développement de profils dhumidité au cours du séchage dextrudats de chacune des deux boues est étudiée. Pour ce faire, les données issues du microsécheur et du microtomographe sont exploitées conjointement. Une analyse multi-zones permet de relier différents phénomènes observés se produisant de manière simultanée. Le développement de résistances intragranulaires au transfert, lapparition de gradients dhumidité à la paroi et le phénomène de fissuration sont en effet liés. Le chapitre VI aborde une caractérisation plus détaillée de la texture des échantillons, principalement dans leur état séché. À cet effet, des techniques telles la microscopie électronique à balayage, la mesure des isothermes dadsorption-désorption dazote et la porosimétrie au mercure sont utilisées en plus de la microtomographie. Le travail se termine par une conclusion rassemblant lensemble des résultats et par lénoncé de perspectives qui pourraient constituer une suite intéressante à cette étude. This thesis comes within a recent research dynamic in the field of sludge drying, according to European requirements concerning urban wastewater treatment and landfilling of biodegradable materials. Considering landspreading and utilization for energy purposes as the two major issues to eliminate sludges, drying constitutes, in both cases, an essential step after mechanical dewatering. Despite obvious economic, industrial and environmental interests, rather few studies have been devoted to wastewater sludge drying till lately. This work aims to improve the knowledge in the field of sludge drying and to better apprehend the textural changes that occur during drying by using X-ray microtomography. A first part of the work is dedicated to the development of a method allowing the production of sludge samples with a reproducible dryness, in order to realize the study on real sludges. Sludges are collected after secondary settling and thickening in two domestic wastewater treatment plants near university. Conditioning and mechanical dewatering are realized in the laboratory. Filtration cakes are characterized by different techniques : rheology, sorption isotherms, Rheological measurements indicate that, for a same sludge, elastic and viscous modulus only depends on the cake dryness. Drying experiments performed on individual cylindrical extrudates obtained from the cake show that operating conditions used for conditioning (polyelectrolyte dose) and dewatering (filtration pressure drop) have no significant influence on drying kinetics. The next part of the work shows that X-ray microtomography, despite this technique is still few used in chemical engineering, is a choice tool to follow the textural changes of individual samples submitted to convective drying. Contrary to methods traditionally or newly used (caliper, volume displacement methods, NMR,), X-ray microtomography is a non destructive, accurate and easy to use technique. The analysis of the images obtained by microtomography allows quantifying the shrinkage of the sample, the cracks and the moisture gradients at the sample wall at successive drying levels. The study of the influence of three operating variables (temperature, superficial velocity and absolute humidity of air) on the shrinkage, the development of cracks and moisture gradients is performed in a convective microdryer specially designed in the laboratory. Extragranular heat and mass transfer coefficients, intragranular diffusion coefficient and the water evaporation capacity are estimated from experimental data. A multi-zone analysis proposes to relate the different phenomena observed. Moisture gradients are induced by internal diffusional limitations and cause mechanical stresses. Cracks appear when mechanical stress exceeds the breakage level. Results show clearly that the crack extent depends on the value of the moisture gradients. The last part of the work deals with a detailed textural characterization of the dried samples. Several characterization techniques (scanning electron microscopy, mercury porosimetry, analysis of N2 adsorption-desorption isotherms, X-ray microtomography) show that the two sludges considered in the study present very different final textures. 3D images and binary images of cross sections indicate, among others, that the cracks developed during drying have different shapes and configurations. Morphological analysis of these cracks gives some ideas about the way cracks develop and brings to the fore a relation between texture and drying kinetics. Although the presence of cracks is not of the highest importance for the final quality of dried sludges, the methodology developed in this thesis can be applied to a large variety of other soft materials (food, ceramics,) for which crack formation has to be avoided because it impairs the final quality of the dried material. In the future, a fully coupled thermo-hydro-mechanical model will be implemented in a Finite Element code to quantify the evolution of the stress tensor versus the drying level especially at the onset of cracks formation. Results obtained in this thesis will allow validating the model.

Le matériau étudié dans cette thèse est un alliage d'aluminium 5182 contenant des particules intermétalliques de deux types : Alx(Fe,Mn) et Mg2Si. Au cours du laminage industriel, les particules sont brisées et redistribuées dans le volume de la tôle. Or, les particules intermétalliques contrôlent à la fois l'aspect de surface et la formabilité de la tôle finale.<br />Le travail présenté dans la thèse s'articule autour de deux problématiques : mettre en évidence la distribution volumique des particules intermétalliques dans le volume de la tôle, et caractériser leur forme tridimensionnelle complexe au cours du laminage. Ainsi, des échantillons prélevés à différentes étapes du laminage sont observés par micro tomographie aux rayons X (réalisé à l'ESRF). Les images tridimensionnelles obtenues sont segmentées par la méthode de segmentation multi classe. Elle permet d'extraire chaque type de particule de l'alliage. Une base de donnée contenant chaque particule individualisée est créée. Elle permet de reconstruire l'image binaire du matériau et de travailler particule à particule.<br />La dispersion des particules est mise en évidence par l'étude du graphe des distances et de la covariance. Puis l'analyse de l'érosion linéaire et de la covariance permet de modéliser le matériau par un modèle probabiliste de type schéma Booléen à grains primaires sphériques.<br />Une batterie de paramètres morphologiques caractérise la forme tridimensionnelle complexe des particules. Une analyse en composantes principales est ensuite réalisée pour synthétiser l'information. Dans l'espace obtenu, les particules sont classées en cinq familles de forme. Enfin, leur évolution au cours du laminage est étudiée.

Orientador: Osmir Batista de Oliveira Junior / Abstract: A regeneração óssea caracteriza-se por ser um processo fisiológico complexo que envolve a participação coordenada entre angiogênese e osteogênese. Envolve um processo de múltiplas etapas que inclui migração, proliferação e diferenciação de vários tipos de células, como células endoteliais, fibroblastos, osteoblastos e osteoclastos. Sabe-se que os biomateriais sintéticos têm demonstrado ser uma excelente alternativa ao reparo ósseo. Assim, o objetivo deste estudo foi avaliar o efeito do Biosilicato de sódio (BS) e dos compósitos 3D de 30% de hidroxiapatita e ácido poliláctico (3D 30% HA / PLA) e 30% hidroxiapatita e ácido poli (ácido láctico-co-glicólico) (30% HA / PLGA), e em defeitos críticos na calvária de ratos. Cento e vinte ratos machos de 90 dias com 350g de massa corporal em média foram aleatoriamente divididos em grupos de acordo com materiais de enxerto e tempo de análise, apresentando 6 animais em cada um. Os defeitos de tamanho crítico foram criados empregando-se uma trefina de 8 mm de diâmetro interno e preenchidos com os materiais mencionados ou apenas o coágulo sanguíneo como controle. Após 14 (T1), 30 (T2), 60 (T3), 90 (T4) e 120 dias (T5) dias do procedimento cirúrgico, a regeneração óssea foi avaliada por radiografia, microtomografia computadorizada (μ-CT) e histologia. A avaliação macroscópica mostrou biocompatibilidade em torno da área de interesse entre os biomateriais e ossos adjacentes. As imagens de μ-CT e de raios-x revelaram uma considerável formação ... (Complete abstract click electronic access below) / Resumo: The process of bone regeneration requires a coordinated coupling between osteogenesis and angiogenesis involveing a multistep process that includes migration, proliferation, and differentiation of several types of cells such as endothelial, fibroblasts, osteoblasts and osteoclasts. It is known that synthetic biomaterials have been proven to be an excellent alternative to bone repair. Thus, the aim of this study is to evaluate the effect of calcium and sodium Biosilicate (BS), a 3D scaffold of hydroxyapatite and polylactic acid (30% HA / PLA) and a hydroxyapatite and poly (lactic-co-glycolic acid) (30% HA / PLGA) composites in critical-sized calvarial defects. One hundred and twenty 90 days old male rats with 350g of body mass on average were randomly divided into groups (n = 6) according to graft materials and analysis time. Critical-size defects were created by means of a 8 mm inner diameter trephine bur and were filled with a 3D 30% HA/PLGA scaffold, 30% HA/PLA, BS or blood clot as control. After 15 (T1), 30 (T2), 60 (T3), 90 (T4) and 120 (T5) days of the cirurgical procedure, bone regeneration was evaluated by histology, x-ray and micro-computed tomography (µ-CT). Macroscopic evaluation showed no significant inflamation around the interest area. µ-CT results indicates that 30% HA/PLA and 3D 30% HA/PLGA composites were not fully degraded and images revealed considerable bone formation in 90 days and 120 days in relation to these materials. On the other hand, BS presented a ... (Resumo completo, clicar acesso eletrônico abaixo) / Doutor

Ultra high performance fibre reinforced concrete (UHPFRC) is a relatively new fibre reinforced cementitious composite and has become very popular in construction applications. Extensive experimental studies have been conducted, demonstrating its superior properties such as much higher strength, ductility and durability than conventional fibre reinforced concrete (FRC) and high performance concrete. However, the material's damage and fracture mechanisms at meso/micro scales are not well understood, limiting its wider applications considerably. This study aims at an in-depth understanding of the damage and fracture mechanisms of UHPFRC, combining microscale in-situ X-ray computed tomography (µXCT) experiments and mesoscale image-based numerical modelling. Firstly, in-situ µXCT tests of small-sized UHPFRC specimens under wedge splitting loading were carried out, probably for the first time in the world, using an in-house designed loading rig. With a voxel resolution of 16.9µm, the complicated fracture mechanisms are clearly visualised and characterised using both 2D images and 3D volumes at progressive loading stages, such as initiating of micro-cracks, arresting of cracks by fibres, bending and pulling out of fibres and spalling of mortar at the exit points of inclined fibres. Secondly, based on the statistics of pores in the µXCT images obtained for a 20mm cube specimen, an efficient two-scale analytical-numerical homogenisation method was developed to predict the effective elastic properties of the UHPFRC. The large number of small pores were first homogenised at microscale with sand and cement paste, using elastic moduli from micro-indentation tests. 3D mesoscale finite element models were built at the second scale by direct conversion of the µXCT images, with fibres and large pores were faithfully represented. The effects of the volume fraction and the orientation of steel fibres on the elastic modulus were investigated, indicating that this method can be used to optimise the material micro-structure. Thirdly, 3D mesoscale finite element models were built for the specimen used in the in-situ µXCT wedge splitting test, with embedded fibre elements directly converted from the µXCT images. The fracture behaviour in the mortar was simulated by the damage plasticity model available in ABAQUS. Finally, 2D mesoscale finite element models were developed to simulate the fracture behaviour of UHPFRC using cohesive interface elements to simulate cracks in the mortar, and randomly distributed two-noded 1D fibres and connector elements to simulate the pull-out behaviour of fibres. This approach offers a link between the fibres pull-out behaviour and the response of the whole composite at the macroscale, thus it can be used to conduct parametric studies to optimise the material properties.