Investigou-se a influência da inclinação das paredes de dentina (paralela ou perpendicular à ação da gravidade) e da variação regional dos espécimes (terços cervical ou oclusal) na resistência adesiva e na espessura da camada de adesivo. Vinte e cinco molares humanos foram seccionados no sentido mésio-distal e paralelamente ao seu longo eixo, obtendo-se secções vestibulares e linguais, as quais foram lixadas produzindo-se superfícies planas de dentina. Sistemas adesivos (Adper Single Bond-SB e Prime & Bond 2.1- PB2.1) foram aplicados na dentina, ora paralelamente ora perpendicularmente à ação da gravidade, padronizando-se o volume de adesivo (3,5 µl por gota) através do uso de uma micropipeta e seguindo-se as instruções dos fabricantes. Os grupos de estudo foram: 1A (SB, paralelo), 1B (SB, perpendicular), 2A (PB2.1, paralelo) e 2B (PB2.1, perpendicular). Após 24h de armazenamento em água deionizada a 37°C, espécimes foram preparados na forma de palitos de dentina com área adesiva de 0,8 mm2, aproximadamente. Na seqüência, foi determinada a espessura do adesivo de cada espécime, em micrômetros (µm), sob microscopia óptica (200X de aumento) e auxílio do programa Image Pro-Plus 4.5. Posteriormente, os espécimes foram submetidos à microtração sob velocidade de 0,5 mm/min. Todos os espécimes fraturados foram examinados sob microscopia óptica (40X de aumento) para a determinação dos planos de fratura. Os dados coletados foram submetidos aos testes ANOVA a 1 e 2 critérios e SNK (? = 0,05). Para determinação da correlação entre resistência adesiva e espessura do adesivo foi utilizado o teste de Correlação de Pearson. Os valores médios (MPa±d.p.) de resistência adesiva dos grupos 2A (52,93±15,19) e 2B (52,27±16,54) foram superiores àqueles dos grupos 1A (39,09±12,90) e 1B (32,94±12,42), independente da inclinação das paredes de dentina dos mesmos. Não houve diferença nos valores de resistência adesiva à dentina, independente da variação regional do espécime. Os valores médios (µm±d.p.) de espessura da camada de adesivo dos grupos 1A (11,24±2,92) e 1B (18,11±7,31) foram superiores àqueles dos grupos 2A (4,20±1,81) e 2B (3,87±1,29) (p > 0,05). O grupo 1B promoveu os maiores valores de espessura de adesivo, seguido do grupo 1A. As espessuras do adesivo nos grupos 2A e 2B apresentaram-se similares entre si. Houve influência da variação regional do espécime na espessura de adesivo somente para o grupo 1B. Não houve correlação entre resistência adesiva e espessura de adesivos para ambos SB e PB2.1 (r = -0,224, p = 0,112 e r = 0,099, p = 0,491, respectivamente). Conclui-se que a influência da inclinação das paredes de dentina e da variação regional dos espécimes na espessura da camada de adesivo é material-dependente, porém não influem na resistência adesiva dos sistemas adesivos à dentina. / To determine the effect of the inclination of dentin surfaces (parallel or perpendicular to the force of gravity) and the regional variation of specimens (cervical or occlusal thirds) on the dentin bond strength and adhesive layer thickness. Twenty-five extracted human molars were sectioned in a mesio-distal direction to expose flat dentin. Standardized drop volumes of adhesive systems (Single Bond-SB and Prime & Bond 2.1-PB2.1) were applied to dentin according to manufacturers instructions. Teeth were randomly divided into the following groups: 1A (SB, parallel), 1B (SB, perpendicular), 2A (PB2.1, parallel) and 2B (PB2.1, perpendicular). Teeth were stored in 37°C distilled water for 24h and then serially sectioned to obtain sticks with cross-sectional area of approximately 0.8 mm2 for microtensile bond strength test (MTBS). The thickness of adhesive layer of the MTBS specimen was determined in a light microscope at 200X magnification. Forty-eight hours after adhesion procedures the specimens were subjected to MTBS at a crosshead speed of 0.5 mm/min. After testing, the fracture modes of each specimen were determined by examination under a 40X magnification. One and two-way ANOVA and Student- Newman-Keuls-SNK tests were performed do determine differences in MTBS and in adhesive layer thickness among groups. The correlation between MTBS and adhesive layer thickness was compared with Pearson Product Moment Correlation ('alfa' = 0.05). Mean values (MPa±s.d.) for bond strength were higher for groups 2A (52.93±15.19) and 2B (52.27±16.54) than for groups 1A (39.09±12.90) and 1B (32.94±12.42), regardless of the position of dentin surfaces. There was no difference in MTBS, despite the regional variation of specimens. The thickness of adhesive systems (µm±s.d.) was higher for groups 1A (11.24±2.92) and 1B (18.11±7.31) than those for groups 2A (4.20±1.81) and 2B (3.87±1.29). Group 1B provided the greater mean values of adhesive thickness followed by the Group 1A. Similar adhesive thicknesses were found for Groups 2A and 2B, but significantly lower than the other groups. There was a significant influence of the regional variation of specimens on the adhesive thickness of group 1B. No correlation was found between bond strength and adhesive layer thickness for both SB and PB 2.1 (r = -0.224, p = 0.112 and r = 0.099, p = 0.491, respectively). The inclination of dentin surface and the regional variation of specimens on the adhesive layer thickness are materialdependent. These variables do not influence the adhesive systems bond strength to dentin.

Investigou-se a influência da inclinação das paredes de dentina (paralela ou perpendicular à ação da gravidade) e da variação regional dos espécimes (terços cervical ou oclusal) na resistência adesiva e na espessura da camada de adesivo. Vinte e cinco molares humanos foram seccionados no sentido mésio-distal e paralelamente ao seu longo eixo, obtendo-se secções vestibulares e linguais, as quais foram lixadas produzindo-se superfícies planas de dentina. Sistemas adesivos (Adper Single Bond-SB e Prime & Bond 2.1- PB2.1) foram aplicados na dentina, ora paralelamente ora perpendicularmente à ação da gravidade, padronizando-se o volume de adesivo (3,5 µl por gota) através do uso de uma micropipeta e seguindo-se as instruções dos fabricantes. Os grupos de estudo foram: 1A (SB, paralelo), 1B (SB, perpendicular), 2A (PB2.1, paralelo) e 2B (PB2.1, perpendicular). Após 24h de armazenamento em água deionizada a 37°C, espécimes foram preparados na forma de palitos de dentina com área adesiva de 0,8 mm2, aproximadamente. Na seqüência, foi determinada a espessura do adesivo de cada espécime, em micrômetros (µm), sob microscopia óptica (200X de aumento) e auxílio do programa Image Pro-Plus 4.5. Posteriormente, os espécimes foram submetidos à microtração sob velocidade de 0,5 mm/min. Todos os espécimes fraturados foram examinados sob microscopia óptica (40X de aumento) para a determinação dos planos de fratura. Os dados coletados foram submetidos aos testes ANOVA a 1 e 2 critérios e SNK (? = 0,05). Para determinação da correlação entre resistência adesiva e espessura do adesivo foi utilizado o teste de Correlação de Pearson. Os valores médios (MPa±d.p.) de resistência adesiva dos grupos 2A (52,93±15,19) e 2B (52,27±16,54) foram superiores àqueles dos grupos 1A (39,09±12,90) e 1B (32,94±12,42), independente da inclinação das paredes de dentina dos mesmos. Não houve diferença nos valores de resistência adesiva à dentina, independente da variação regional do espécime. Os valores médios (µm±d.p.) de espessura da camada de adesivo dos grupos 1A (11,24±2,92) e 1B (18,11±7,31) foram superiores àqueles dos grupos 2A (4,20±1,81) e 2B (3,87±1,29) (p > 0,05). O grupo 1B promoveu os maiores valores de espessura de adesivo, seguido do grupo 1A. As espessuras do adesivo nos grupos 2A e 2B apresentaram-se similares entre si. Houve influência da variação regional do espécime na espessura de adesivo somente para o grupo 1B. Não houve correlação entre resistência adesiva e espessura de adesivos para ambos SB e PB2.1 (r = -0,224, p = 0,112 e r = 0,099, p = 0,491, respectivamente). Conclui-se que a influência da inclinação das paredes de dentina e da variação regional dos espécimes na espessura da camada de adesivo é material-dependente, porém não influem na resistência adesiva dos sistemas adesivos à dentina. / To determine the effect of the inclination of dentin surfaces (parallel or perpendicular to the force of gravity) and the regional variation of specimens (cervical or occlusal thirds) on the dentin bond strength and adhesive layer thickness. Twenty-five extracted human molars were sectioned in a mesio-distal direction to expose flat dentin. Standardized drop volumes of adhesive systems (Single Bond-SB and Prime & Bond 2.1-PB2.1) were applied to dentin according to manufacturers instructions. Teeth were randomly divided into the following groups: 1A (SB, parallel), 1B (SB, perpendicular), 2A (PB2.1, parallel) and 2B (PB2.1, perpendicular). Teeth were stored in 37°C distilled water for 24h and then serially sectioned to obtain sticks with cross-sectional area of approximately 0.8 mm2 for microtensile bond strength test (MTBS). The thickness of adhesive layer of the MTBS specimen was determined in a light microscope at 200X magnification. Forty-eight hours after adhesion procedures the specimens were subjected to MTBS at a crosshead speed of 0.5 mm/min. After testing, the fracture modes of each specimen were determined by examination under a 40X magnification. One and two-way ANOVA and Student- Newman-Keuls-SNK tests were performed do determine differences in MTBS and in adhesive layer thickness among groups. The correlation between MTBS and adhesive layer thickness was compared with Pearson Product Moment Correlation ('alfa' = 0.05). Mean values (MPa±s.d.) for bond strength were higher for groups 2A (52.93±15.19) and 2B (52.27±16.54) than for groups 1A (39.09±12.90) and 1B (32.94±12.42), regardless of the position of dentin surfaces. There was no difference in MTBS, despite the regional variation of specimens. The thickness of adhesive systems (µm±s.d.) was higher for groups 1A (11.24±2.92) and 1B (18.11±7.31) than those for groups 2A (4.20±1.81) and 2B (3.87±1.29). Group 1B provided the greater mean values of adhesive thickness followed by the Group 1A. Similar adhesive thicknesses were found for Groups 2A and 2B, but significantly lower than the other groups. There was a significant influence of the regional variation of specimens on the adhesive thickness of group 1B. No correlation was found between bond strength and adhesive layer thickness for both SB and PB 2.1 (r = -0.224, p = 0.112 and r = 0.099, p = 0.491, respectively). The inclination of dentin surface and the regional variation of specimens on the adhesive layer thickness are materialdependent. These variables do not influence the adhesive systems bond strength to dentin.

Cette thèse s’est déroulée dans le contexte de l’évaluation non destructive du collage de patches composites employés pour la réparation de structures aéronautiques. Le besoin a été exprimé par la DGA Techniques Aéronautiques (Toulouse). Le travail effectué a consisté en l’exploitation des ondes guidées, de type SH puis Lamb, pour mesurer des caractéristiques mécaniques d'un joint de colle et tenter d’évaluer, de manière non destructive, la qualité du collage. Dans un premier temps, les propriétés viscoélastiques des matériaux assemblés sont déterminées. Elles servent alors de données d’entrée à des modèles, basés sur la méthode SAFE (Semi Analytical Finite Element method), permettant d’obtenir les courbes de dispersion ainsi que les champs des différents modes guidés se propageant le long de l’assemblage collé. Ces simulations numériques permettent alors d’évaluer le potentiel des ondes guidées à caractériser un adhésif. Des mesures expérimentales sont ensuite menées pour confirmer les prédictions numériques. Finalement la résolution d’un problème inverse, qui consiste à évaluer les modules de rigidité de la couche de colle se situant entre une plaque d’aluminium et un patch, est proposée pour établir des pistes d’évaluation non destructive d’un collage répondant au besoin industriel. Cette étude a été financée par la DGA, France. / Repairing of metallic structures using composite patches bonded with an adhesive layer is more and more common in the aeronautic field, and particularly at DGA Techniques Aéronautiques. In order to guarantee the quality of this bond, the sensitivity of ultrasonic guided waves is investigated. Shear-horizontally polarized (SH) waves, and Lamb waves are investigated to infer the stiffness of the adhesive layer. The SAFE method is used to predict the dispersion curves and mode shapes of the different wave modes propagating along the three-layer assembly. Numerical simulations are run for selecting the most appropriate wave modes, i.e. with higher sensitivity to the stiffness of the bond than to other components properties. Experiments are also made for generating-detecting pre-selected SH or Lamb wave modes in order to confirm the numerical predictions. Finally the resolution of an inverse problem, consisting in the evaluation of the stiffness modulus of the bond layer between an aluminium plate and a carbon-epoxy composite patch, at different curing time, is proposed as a contribution to the establishment of possible strategies for bonds testing. This work was supported by DGA, France.

This thesis concerns some aspects that have influence on the strength of adhesive layers. The strength is determined by the stress deformation-relation of the layer. This relation is also referred to as cohesive law. The aspects having influence on the cohesive laws that are studied in this work are temperature, fatigue, multi-axial fatigue and mixed mode loading. For each aspect, a model is developed that can be used to describe the influence of the aspects on the cohesive laws numerically, e.g. by using the finite element method. These models are shown to give good agreement with the experimental results when performing simulations that aims at reproducing the experiments. For the aspect of temperature, a FE-model is suggested that can be used to simulate the mechanical behaviour in pure mode loadings at any temperature within the evaluated temperature span. Also, a damage law for modelling high cycle fatigue in a bonded structure in multi-axial loading is presented. Lastly, a new experimental set-up is presented for evaluating strength of adhesives during mixed mode loading. The set-up enables loading with a constant mode-mix ratio and by the experimental results, a potential model for describing the mechanical behaviour of the evaluated adhesive is presented.

The diploma thesis studies composite of PP and filler particle. As a particle filler was used commercially available CaCO3 (SOCAL 31). The submitted thesis had a goal to find new approaches and technologies of filler surface treatment in order to improve properties of composite materials. The plasma discharge behind static pressure was used for the surface treatment of the fillers. These fillers were afterwards analyzed by using of sedimentation analysis, turbidimetry, infra-red spectroscopy (FT-IR), X-ray diffraction analysis (XRD), scan electron microscopy (SEM), transmission electron microscopy and particle size distribution by laser diffraction. The composites with various volume parts of the fillers were prepared in PIB and studied by short-time tests. Furthermore, the influence of an adhesive layer on fracture mechanical properties of prepared composite was study. Regarding to experimental demand, there was not possible to realize long-term mechanical properties.