Neste trabalho foi medida a tenacidade à fratura de quatro ligas fundidas com composição química base do aço AISI M2 – uma de composição química convencional (liga I), e as demais modificadas por adições de nitrogênio (liga II), cério (liga III) e antimônio (liga IV) – submetidas a tratamentos térmicos visando a decomposição do carboneto M2C, a esferoidização e engrossamento dos carbonetos produto M6C e MC, em altas temperaturas e por diversos tempos. A metodologia empregada nesta avaliação da tenacidade à fratura foi a dos corpos de prova curtos com entalhe chevron segundo ASTM E 1304-97, de forma a superar a necessidade do pré-trincamento por fadiga, procedimento de difícil controle e custoso em materiais como os aços rápidos temperados e revenidos. Verificou-se que a metodologia utilizada para obtenção e ensaio de corpos de prova chevron foi de fácil execução (comparada à metodologia convencional) permitindo grande número de experimentos. Para verificar a consistência dos resultados, em algumas condições, também se utilizou a metodologia convencional segundo a ASTM E 399-90, cujo pré-trincamento foi feito utilizando os procedimentos propostos por Harris e Dunegan. Os resultados obtidos para os aços fundidos foram correlacionados com os obtidos para outros aços rápidos convencionais (VM2, M2 Thyssen) e um aço rápido sinterizado (SINTER 23). A microestrutura foi caracterizada utilizando-se técnicas de ataques metalográficos diferenciais, metalografia quantitativa manual e computadorizada e microscopia eletrônica de varredura. A avaliação microestrutural indica que não ocorreu precipitação eutética do carboneto M6C, em nenhuma das ligas fundidas. O carboneto M2C apresenta morfologia tanto irregular (plaquetas – tipo 1) quanto regular-complexa (lamelas – tipo 2). As ligas I, III e IV, apresentaram a predominância da morfologia tipo 1 enquanto que a liga II modificada pelo nitrogênio, apresentou apenas a morfologia tipo 2. O carboneto MC apresentou-se com morfologia regular-complexa. Medidas do espaçamento interdendrítico indicam que não houve influência significativa dos elementos modificadores sobre este parâmetro. Ensaios de resistência à flexão, indicam pouca influência dos elementos modificadores, mas forte influência dos tratamentos térmicos sobre o limite de resistência à ruptura transversal do aço fundido. Em todas as ligas, a resistência à flexão cresceu com o tempo de tratamento a 1200°C, bem como com a temperatura de decomposição em tratamentos por 2 horas. Análise das fraturas por microscopia eletrônica de varredura indicou que o crescimento das trincas se deu na região interdendrítica. O aço convencional apresentou resistência à ruptura transversal muito superior à dos aços fundidos. Os ensaios de tenacidade à fratura apresentaram resultados compatíveis com a literatura para os aços AISI M2 convencional e SINTER 23. Os resultados obtidos para o aço fundido, indicam queda nos valores de tenacidade à fratura nos materiais tratados a 1050°C com o avanço do tempo de tratamento; pouca variação dos valores com o tempo nas amostras tratadas a 1150°C; e aumento significativo da tenacidade à fratura com o tempo de tratamento a 1200°C. Os valores de tenacidade obtidos para os aços rápidos fundidos foram mais elevados que os obtidos para os materiais trabalhados e para o material sinterizado. / Fracture Toughness of four cast alloys with chemical composition based on the High-Speed Steel AISI M2 were measured. One of the alloys (alloy I) had the conventional AISI M2 composition, while the other three were modified by the addition of N (alloy II), Ce (alloy III) and Sb (alloy IV). The cast alloys were heat-treated in order to promote the decomposition of the M2C carbide as well as spheroidize and coarsen the product M6C e MC carbides. The method chosen for measuring fracture toughness was based on the use of short rod and bar chevron notched samples, according to ASTM E1304 – 97, in order to evade the need for fatigue pre-cracking, notoriously difficult for High Speed Steels quenched and tempered. The chevron-notch method proved straightforward and allowed for successful testing a great number of specimens. Conventional compact sample fracture toughness, according to ASTM E 399-90, with pre-cracking obtained using Harris-Dunegan drop-weight procedure, was used to validate the results. The results for cast alloys were compared with conventionally produced High Speed Steels (VM2, M2 Thyssen) and with a powder metallurgy High Speed Steel (SINTER 23). Microstructural characterization was performed using selective etching of polished surfaces, manual and automated quantitative metallography and SEM. Microstructural evaluation of as-cast alloys showed that there was no eutectic precipitation of M6C carbides. The M2C carbides show an irregular eutectic morphology (Type 1- plates) as well as a regular-complex eutectic morphology. Measurements of interdendritic spacing did not detect any effect of the modification. The bending test rupture strengths did not vary with the addition of modifying elements, but increased with the time and temperature of decomposition, spheroidization and coarsening of carbides. Rupture strengths increased with the heat-treatment time at 1200°C as well as with increasing temperatures for 2 h heat-treatments. SEM examination of the fracture surfaces showed that crack preferential growth path was interdendritical. Conventional High Speed Steels tested in bending presented better results for the rupture strength than cast steels. Fracture toughness results for M2 conventional steels and for the SINTER 23 steel were similar to the results from the literature. Fracture toughness results obtained for cast steels diminished with increasing decomposition time at 1050°C, did not change much with increasing decomposition time at 1150°C, increased markedly withy increasing decomposition times at 1200°C. The fracture toughness results for the as-cast steels were higher than the results obtained for the wrought steels and for the powder metallurgy steel.

Cette thèse porte sur l’influence des transformations de phases solide-solide sur la propagation de fissure. On souhaite ainsi mieux comprendre les variations de ténacité en cours de soudage par exemple, ou bien pendant la réparation d’une fissure. Dans ce travail, la ténacité est obtenue à partir de l’intégrale J. Il existe de nombreuses méthodes expérimentales permettant d’obtenir la ténacité critique JIC mais qui sont difficilement applicables pour des essais se déroulant pendant une transformation de phase. C’est pourquoi nous avons proposé une méthode couplant essai mécanique et mesure par corrélation d’images avec de la simulation par éléments finis. Les essais sont réalisés sur de simples éprouvettes plates pré fissurées, faciles à usiner et simple à chauffer par induction. Les essais sont conduits pour différentes températures et jusqu’à rupture. En sus des mesures d’efforts et déplacements de traverse, la corrélation d’images nous fourni également les champs de déplacement sur chaque face de l’éprouvette. Chaque essai est ensuite simulé par éléments finis où la ténacité critique est calculée par la méthode G-Theta au maximum de la charge supportée par l’éprouvette. Les simulations précédentes intègrent les conditions aux limites obtenues par corrélation et le comportement mécanique considéré est celui que nous avons identifié sur des essais de caractérisation. Deux nuances de matériau ont été étudiées avec cette méthode ; l’acier inoxydale 15-5PH ainsi que l’acier ferritique 16MND5. Pour ces deux matériaux, différentes températures d’essai ont été choisies avant, pendant et après la transformation pour effectuer les essais de rupture ainsi que de caractérisation du comportement mécanique. Les résultats de cette étude montrent que la transformation de phase peut avoir un impact non négligeable sur la ténacité. Ainsi, pour le 15-5PH, le taux d’austénite résiduel est un facteur important et les essais pendant la transformation martensitiques montrent que la ténacité critique peut être inférieure pendant celle ci à celle du matériau purement austénitique. Dans le cas du 16MND5, la ténacité est beaucoup plus faible à 600°C (et bainitique) qu’à température ambiante ce qui est assez logique. Par contre, lors du refroidissement, depuis 600° (austénitique) jusqu’à la température ambiante (bainitique), nous avons obtenu une ténacité critique relativement constante. En conclusion, cette étude apporte une solution quant à la mesure de la ténacité critique de matériau pendant des transformations de phases, ce que ne permettent pas forcément les essais normalisés. Pour le 15-5PH, la ténacité critique semble évoluer pendant la transformation martensitique et est assez dépendante du taux d’austénite résiduelle. Il semble par contre que pour le 16MND5, la ténacité critique soit assez peu dépendante de la fraction volumique d’austénite et la valeur obtenue varie peu au cours du refroidissement du matériau depuis 600°C. / Ou study focuses on the effects of phase transformations on crack propagation. We want to understand the changes of fracture toughness during welding. In this work, fracture toughness is expressed by J-integral. There are many experimental methods to obtain the critical toughness JIC but they are impractical for our investigation during phase transformation. That is the reason why we have proposed a method coupling mechanical tests, digital image correlation and finite element simulation. The fracture tests are implemented on pre-cracked single edge notched plate sample which is easy for machining and heat conduct during phase transformation. The tests are conducted at different temperatures until rupture. Digital image correlation gives us the displacement information on every sample. Each test is then simulated by finite element where the fracture toughness is evaluated by the method G-Theta at the crack propagation starting moment found by potential drop method and digital image correlation technical. Two materials have been studied, 15Cr-5Ni martensitic precipitation hardening stainless steel and 16MND5 ferritic low carbon steel. For these two materials, different test temperatures were chosen before, during and after phase transformation for testing and failure characterization of the mechanical behavior. Investigation result shows that metallurgical phase transformation has an influence on fracture toughness and further crack propagation. For 15-5PH, the result of J1C shows that the as received 15-5PH has higher fracture toughness than the one at 200°C. The toughness is also higher than the original material after one cycle heat treatment probably due to some residual austenite. Meanwhile, pure austenite 15-5PH at 200°C has higher fracture toughness than pure martensitic 15-5PH at 200°C. For 16MND5, the result also proves that the phase transformation affects fracture toughness. The as received material has bigger J1C than the situation where it was heated to 600°C. On the other hand, the material at 600°C just before isothermal bainite transformation after the austenitization during cooling process also has higher fracture toughness than the one at 600°C before austenitization. These two conclusions are consistent well with the result of 15-5PH. But the final situation of 16MND5 after one cycle heat treatment has a slightly smaller J1C than the receiving situation. It means that one cycle heat treatment hasn't an significant influence on 16MND5fracture toughness. Conclusions show that one should pay attention to the heating period before austenitization of the substrate material when people do the welding as the higher temperature will bring the lower fracture toughness during this process. While during cooling period, the fracture toughness doesn't change a lot during, before or after the cooling induced phase transformation. Even for 15-5PH, it has a better fracture toughness after the martensite transformation than before.

The microstructure of concrete contains random features over a wide range of length scales in which each length scale possess a new random composite. The influence of individual material constituents at different scales and their mutual interactions are responsible for the formation of fracture process zone (FPZ). The presence of the FPZ and the various toughening mechanism occurring in it, influences the fatigue and fracture behavior of concrete which also gets influenced by the geometry, spacial distribution and material properties of individual material constituents and their mutual interactions. Hence, in order to study the influence of interfacial transition zone, microcrack and aggregate bridging on the fracture and fatigue behavior of concrete, a multiscale analysis becomes necessary. This study aims at developing a linearized model which helps in understanding the fracture and fatigue behavior of cementitious materials by considering the predominant fracture process zone (FPZ) mechanisms such as microcracking and aggregate bridging. This is achieved by quantifying the critical microcrack length and the bridging resistance offered by the aggregates. Further, the moment carrying capacity of a cracked concrete beam is determined by considering the effect of aggregate bridging. A modified stress intensity factor (SIF) is derived based on linear elastic fracture mechanics (LEFM) approach by considering the material behavior at different scales through a multiscale approach. The model predicts the entire crack growth curve for plain concrete by considering these process zone mechanisms. Furthermore, the fracture and fatigue response of concrete is studied through the development of analytical models which include the properties of the mix constituents using the multiscale based SIF. The effect of the interfacial transition zone, microcracks and resistance offered through aggregate bridging on the resistance to crack initiation and propagation are studied. A fatigue crack growth law is proposed using the concepts of dimensional analysis and self-similarity. Through sensitivity analyses, the influence of different parameters on the overall fracture and fatigue behavior are studied. In addition, studies related to concrete-concrete bi-material interfaces are conducted in order to understand the influence of repair materials on the service life of damaged concrete structures when subjected to fatigue loading. An analytical model is proposed in this study to predict the crack growth curve using the concepts of dimensional analysis and self-similarity in conjunction with the human population growth model. It is seen that a repair done with a patch having similar elastic properties as those of the parent concrete will have a larger fatigue life.

Abstract Quality control is an essential part of manufacturing, and the different properties of the products can be tested with standardized methods. If the decision of qualification is based on only one test specimen representing a batch of products, the testing procedure is quite straightforward. However, when the measured property has a high variability within the product, as usual, several test specimens are needed for the quality verification. When a quality property is predicted, the response value of the model that most effectively finds the critical observations should naturally be selected. In this thesis, it has been shown that LIB-transformation (Larger Is Better) is a suitable method for multiple test samples, because it effectively recognizes especially the situations where one of the measurements is very low. The main contribution of this thesis is to show how to model quality of phenomena that consist of several measurement samples for each observation. The process contains several steps, beginning from the selection of the model type. Prediction of the exceedance probability provides more information for the decision making than that of the mean. Especially with the selected application, where the quality property has no optimal value, but the interest is in adequately high value, this approach is more natural. With industrial applications, the assumption of constant variance should be analysed critically. In this thesis, it is shown that exceedance probability modelling can benefit from the use of an additional variance model together with a mean model in prediction. The distribution shape modelling improves the model further, when the response variable may not be Gaussian. As the proposed methods are fundamentally different, the model selection criteria have to be chosen with caution. Different methods for model selection were considered and commented, and EPS (Exceedance Probability Score) was chosen, because it is most suitable for probability predictors. This thesis demonstrates that especially a process with high diversity in its production and more challenging distribution shape gains from the deviation modelling, and the results can be improved further with the distribution shape modelling. / Tiivistelmä Laadunvalvonnalla on keskeinen rooli teollisessa tuotannossa. Valmistettavan tuotteen erilaisia ominaisuuksia mitataan standardin mukaisilla testausmenetelmillä. Testi on yksinkertainen, jos tuotteen laatu varmistetaan vain yhdellä testikappaleella. Kun testattava ominaisuus voi saada hyvin vaihtelevia tuloksia samastakin tuotteesta, tarvitaan useita testikappaleita laadun varmistamiseen. Tuotteen laatuominaisuuksia ennustettaessa valitaan malliin vastemuuttuja, joka tehokkaimmin tunnistaa laadun kannalta kriittiset havainnot. Tässä väitöskirjassa osoitetaan, että LIB-transformaatio (Large Is Better) tunnistaa tehokkaasti erityisesti tilanteet, joissa yksi mittauksista on hyvin matala. Tämän väitöskirja vastaa kysymykseen, kuinka mallintaa laatua, kun tutkittavasta tuotteesta tarvitaan useita testinäytteitä. Mallinnusprosessi koostuu useista vaiheista alkaen mallityypin valinnasta. Alitusriskin mallinnuksen avulla saadaan enemmän informaatiota päätöksenteon tueksi perinteisen odotusarvomallinnuksen sijaan, etenkin jos laatutekijältä vaaditaan vain riittävän hyvää tasoa optimiarvon sijaan. Teollisissa sovelluksissa ei voida useinkaan olettaa, että vasteen hajonta olisi vakio läpi prosessin. Tässä väitöskirjassa osoitetaan että alitusriskin ennustamistarkkuus paranee, kun odotusarvon lisäksi mallinnetaan myös hajontaa. Jakaumamuodon mallilla voidaan parantaa ennustetarkkuutta silloin, kun vastemuuttuja ei noudata Gaussin jakaumaa. Koska ehdotetut mallit ovat perustaltaan erilaisia, täytyy myös mallin valintakriteeri valita huolella. Työssä osoitetaan, että EPS (Exceedance Probability Score) toimii parhaiten käytetyillä todennäköisyyttä ennustavilla malleilla. Tässä väitöskirjassa osoitetaan, että erityisesti silloin kun tuotantoprosessi on monimuotoinen ja laatumuuttujan jakaumamuoto on haastava, mallinnuttaminen hyötyy hajontamallin käytöstä, ja tuloksia voidaan parantaa jakaumamuodon mallilla.

[pt] O objetivo deste trabalho foi avaliar as propriedades mecânicas, físicas e microestruturais de materiais compósitos cimentícios reforçados por fibras naturais e de laminados de bambu. O trabalho experimental foi direcionado para a determinação da tenacidade. Para se determinar a tenacidade foram utilizados três tipos de ensaios: impacto Charpy, impacto balístico e flexão em 3 pontos. Após os ensaios, a superfície de fratura dos corpos-de-prova foi analisada por microscopia eletrônica de varredura (MEV). Esta análise microestrutural serviu para determinar os modos de fratura e validar as hipóteses feitas nos modelos matemáticos utilizados. Foram usados modelos adaptados da literatura para a determinação da tenacidade e os valores teóricos obtidos foram confrontados com os experimentais. Determinou-se também através de modelos encontrados na literatura a tensão interfacial de todas as fibras utilizadas nesta pesquisa. Os modelos empregados para calcular a tenacidade e a tensão de adesão interfacial, se mostraram eficientes e válidos. Em segundo plano, porém não menos importante, ficou a determinação das propriedades térmicas dos materiais utilizados. Foram efetuados ensaios de condutividade térmica do compósito e ensaios termogravimétricos das fibras vegetais e do bambu. Os compósitos cimentícios foram reforçados por diferentes fibras naturais: polpa refinada de bambu (CPB), polpa de sisal (CPS), polpa de eucalipto (CPE), fibras curtas de sisal (CPFS) e wollastonita (CPW). As proporções das polpas de bambu, sisal e eucalipto utilizadas como reforço nas matrizes cimentícias foram de 8 por cento e 14 por cento em relação à massa do cimento, a da fibra curta de sisal (25 mm) foi de 3 por cento em relação ao volume e a da wollastonita foi de 11,5 por cento em relação à massa. Compóstios híbridos feitos com wollastonita e polpa de bambu (CPBW) foram também produzidos apenas variando a proporção da polpa de bambu em 8 por cento e 14 por cento e mantendo fixa a da wollastonita em 11,5 por cento. Como uma tentativa de se melhorar a resistência ao impacto, laminados CPB/AL foram também fabricados colando duas chapas de alumínio (liga 5052 H34) de espessura 0,8 mm em ambas às faces dos compósitos reforçados por fibra de bambu, formando assim compósitos sanduíche (CPBA). O bambu Moso (Phyllostachys heterocycla pubescens) com 5 anos de idade foi usado para fabricação dos laminados de bambu, sendo tratado com água fervida para a prevenção de ataques biológicos. Técnicas para a extração do laminado a partir de seu formato natural foram estudadas estabelecendo suas vantagens e desvantagens. Para o ensaio de impacto foram utilizados corpos-de-prova com dimensão nominal de 120 mm x 15 mm x 6 mm perfazendo um total de 18 corpos-de-prova. Para o de flexão foram realizados ensaios com uma lâmina simples de bambu (BL) e bambu laminado colado (BLC) com 3 camadas de lâminas dispostas ortogonalmente. Os resultados dos testes de impacto Charpy e flexão em 3 pontos comprovaram a boa tenacidade do bambu laminado quando submetido a cargas de impacto (42,54 kJ/m2) e a cargas estáticas (19,77 kJ/m2 para o laminado e 17,63 kJ/m2 para o laminado colado). Compósitos sanduíche constituídos de alumínio e laminados de bambu foram também fabricados. Estes foram analisados através de ensaios de impacto balísticos seguindo as recomendações da norma NIJ 0101.04. Observações no microscópico eletrônico de varredura foram realizadas para se analisar os mecanismos de falha dos laminados. / [en] The main objective of this work was to evaluate the mechanical, physical and microestructure properties of cementitious composite materials and bamboo laminates. The experimental program was focused on the determination of toughness. Three diferent types of tests were performed in order to establish it: Charpy impact, ballistic impact and three point bending test. After the tests, the fractured surface of the failed test specimens was observed using a Scanning Electron Microscope (SEM) to establish the failure mode. Mathematical models adapted from the available literature were used to determine the toughness from which the values were confronted to the ones obtained experimentally. It was also determined by mathematical models the interfacial bond stress of all fibers used in this research. The two models, used in the toughness and interfacial bond stress calculation, showed to be efficient, providing valid results. In second plan, but not less important, was the determination of the materials thermal properties. Thermal conductivity tests of the composites and thermogravimetry of the fibers and bamboo were performed. The cementitious composites were reinforced by different natural fibers: refined bamboo pulp (CPB), sisal pulp (CPS), eucalyptus pulp (CPE), short sisal fibers (CPFS) and wollastonite. The mass fraction of bamboo, sisal and eucalyptus pulp studied were 8 percent and 14 percent. For the wollastonite fiber the mass fraction studied was 11.5 percent and for the short sisal fiber a 3 percent volume fraction was studied. Hybrid composites made with wollastonite and bamboo pulp (CPBW) were also produced varying the bamboo fraction mass to 8 percent and 14 percent but keeping constant to 11.5 percent the wollastonite mass fraction. The slurry de-watering process was used in the production of all composites described before. To reduce the adverse effects of weathering on the cellulose fibers and to improve the impact load and flexural resistance of the composite, aluminum thin sheets were used to produce a sandwich composite lamina with the CPB, which was denominated as CPBA. Compound Adhesive gel from Otto Baumgart which is a type of epoxy was used to fix the aluminum sheets on the CPB. The use of aluminum has proved to give much higher impact resistance results when compared to the CPB ones. The 5 years old Moso bamboo (Phyllostachys heterocycla pubescens), which was previously treated in boiled water to eliminate biological agents, was used to produce the bamboo laminates. Techniques were developed to extract bamboo laminates from its natural form, establishing its advantages and disadvantages. For the Charpy impact test, a total of 18 specimens with nominal dimensions of 120 mm x 15 mm x 6 mm were tested. Laminated (BL) and 3 layer cross ply laminated bamboo (BLC) were tested in bending. A total of 9 specimens were tested per bamboo configuration. The BL specimens had nominal dimensions of 120 mm x 30 mm x 6 mm and the BLC were 120 mm x 30 mm x 17 mm. The results demonstrated the good toughness of bamboo laminates when subject to dynamic (42.54 kJ/m2) and to static load (19.77 kJ/m2 for the laminate and 17.63 kJ/m2 for the cross ply laminate). Aluminum thin sheets were again used to make sandwich composites, but now using the bamboo laminate (BLCA). The BLCA was tested using the ballistic impact test following the standard NIJ 0101.04. Analysis on the Scanning Eléctron Microscope (SEM) were performed in order to establish the laminate s failure mechanisms.

Modern research being conducted on Mental Toughness is now shifting away from efforts aimed at developing definitions for the construct and instead moving toward efforts at understanding its development. This particular research study focuses on the development and implementation of a Mental Toughness programme designed specifically for, and tailored exclusively to, the needs of schoolboy cricket at Kingswood College in Grahamstown, Eastern Cape. The programme development was an intricate process and the research procedure was guided by the Organisational Development Process model. Data from a focus group as well as various individual interviews were integrated with currently existing Mental Toughness literature and theory to devise this particular Mental Toughness programme. The programme entails educating the athletes on six specific mental skills and incorporates elements of practical application as well as awareness of the importance and influence of Mental Toughness and mental training in a sporting sphere. The programme took the form of mental skills workshops held over a three week period. An analysis was conducted post-programme to document the experience of the athletes as a result of exposure to the programme. Results drawn from the array of analysis procedures were used to help identify the level of success of the Mental Toughness intervention as well as help validify current Mental Toughness models. In addition to highlighting the benefits as a result of the programme experience, various recommendations were drawn in order to shed light on the programme limitations and assist future researchers with understanding the intricacies behind better and more efficient programme implementation.

La solution collage représente un intérêt industriel croissant dans l’assemblage des matériaux. Cependant, à cause des propriétés propres d’un polymère, l’utilisation de cette technologie d’assemblage est limitée par sa température de service. Afin d’augmenter la zone d’opérabilité du joint adhésif, la solution du Joint Multi Adhésifs a déjà été initiée par le passé. Ce joint repose sur la combinaison d’un adhésif résistant à basses températures LTA et d’un second résistant à hautes températures HTA. Le premier joint est placé sur les bords de l’assemblage tandis que le second occupe une position centrale. Partant du concept du Joint Multi Adhésif, l’objectif de ce travail est de proposer un assemblage à un seul joint dont les propriétés seraient modulées le long de la longueur de recouvrement. Ce nouvel adhésif présente une bonne résistance aux contraintes de pelage et de clivage sur les bords de l’assemblage, tout en assurant un rôle structurant à hautes températures. La formulation de cet adhésif consiste à élaborer un joint époxyde présentant une ténacité accrue à ces extrémités, qui diminue graduellement vers le centre de joint polymère. Outre leur capacité à augmenter considérablement la ténacité des thermodurcissables, les copolymères triblocs, de part la structuration à l’échelle nanoscopique qu’ils engendrent au sein ces matériaux, ont l’avantage de ne pas pénaliser les autres propriétés telles que le module d’Young et la température de transition vitreuse. Par ailleurs, grâce à leurs bonnes propriétés d’adhésion, les résines époxydes sont des polymères de choix dans l’élaboration d’adhésif. Par conséquent, tout l’intérêt de ce travail réside dans la synergie des propriétés de ces deux composants. Pour se faire, deux adhésifs époxydes sont formulés. Le premier est un système époxyde classique DER 332-MDEA. Le second est basé sur le même système DER 332-MDEA, mais il est chargé avec 10% en masse de copolymères type PMMA-b-PBA-b-PMMA. Les deux adhésifs massiques sont caractérisés thermiquement, thermomécaniquement et mécaniquement. En second lieu, afin de formuler le joint souhaité, à gradient de propriétés, une étude de la cinétique de diffusion entre les deux adhésifs est entreprise par un suivi rhéologique de l’évolution des modules. Cette étude permet de mettre en évidence les facteurs clefs qui pilotent la diffusion : la température, l’entrefer, la fraction initiale et la polarité du copolymère. Ce travail expérimental permet d’aboutir à l’établissement d’un modèle rhéologique mettant en lumière la compétition diffusion/confinement. L’impact de ce nouveau joint sur la propagation d’une fissure au sein d’un assemblage collé est évalué par un essai de clivage symétrique. / Adhesively bonding technology is of great industrial interest. However, the thermal limited properties of polymers used as adhesive joins limits the operating temperature. To extend the operating temperature range, the Multi Moduli Lap Joint solution has ever been suggested. This solution is an interface with a combination of a low-temperature adhesive LTA (i.e. strengthening for low temperatures) and a high-temperature adhesive HTA (i.e. strengthening for high temperatures), on three joints. Due to its position on each edge of the assembly, the ABT exhibits a great peeling yield, whereas the HTA presents a high shear strength and ensures a structural behaviour. This research aim consists in formulating a new simple lap joint with a gradient of mechanical properties along the bondline. The adhesive formulation has to exhibit a high toughness on its edges which gradually diminishes towards its center. So triblock copolymers are blend into an epoxy resin to obtain a nanostructured adhesive. Thus, a toughness improvement occurs with any depreciation neither of the Young modulus nor the transition glassy temperature. Moreover epoxy resin is well known for its bonding properties. Adhesives are formulated on the basis of the epoxy-amine system: DER 332-MDEA and a DER 332-MDEA nanostructured by 10%wt PMMA-b-PBA-b-PMMA triblock copolymers. First the neat and the nanoscopic-scale-structured thermosets are characterised by thermal, thermomechanical and mechanical tests. Then, to obtain a properties gradient into an adhesive joint, diffusion kinetics between both materials is monitored by rheometer. This study reveals the key parameters that master diffusion phenomenon such as temperature, gap, polarity and weight content of the triblock copolymers. This work allows establishing a rheological model which brings into focus competition between diffusion/wall phenomenon. The impact of this new joint on crack propagation is carried out by cleavage using the wedge test method.

Matériaux incontournables des matériaux fonctionnels, les alliages à mémoire de forme(AMF) peuvent présenter de très larges déformations réversibles. La Transformation de Phase Martensitique (TPM), ayant lieu lorsqu’il est soumis à une action mécanique ou thermique, lui confère des caractéristiques particulières. Le comportement thermomécanique des AMF est à présent bien maîtrisé. Cependant la connaissance de leur comportement `a la rupture reste un enjeu majeur pour leur dimensionnement dans le cadre de leur industrialisation pérenne. Ces travaux de recherche se sont attachés `a la connaissance, la description et la quantification du phénomène de localisation en pointe de fissure liée à la TPM induite sous contrainte, au travers du développement d’un modèle prédictif et de sa corrélation expérimentale par mesures de champs simultanées lors d’essais de rupture sur des éprouvettes fissurées de NiTi. Deux modèles analytiques basés sur la mécanique linéaire de la rupture, intégrant le caractère dissymétrique du comportement des AMF en traction/compression, ont été développés pour la prédiction des zones de transformation au voisinage de la pointe de fissure en tenant compte des différents modes de rupture ( élémentaires et mixtes I+II) et du rayon de courbure en pointe de fissure. Un banc de caractérisation par mesures simultanées de champs cinématiques par corrélation d’images (DIC) et thermique par thermographie infrarouge a été développé pour cartographier les champs expérimentaux d’essais de rupture en mode I sur des éprouvettes pré-fissurées. Cette bonne corrélation des modèles analytiques ouvre de nombreuses perspectives concernant l’analyse du couplage thermo mécanique associé à la TPM en pointe de fissure, l’enrichissement des modèles analytiques initiaux, et la confrontation avec les résultats expérimentaux pour des modes de rupture plus complexes (II et mixte I+II). / Major player among functional materials, Shape Memory Alloys (SMA) may undergo verylarge reversible strain. SMA exhibit a Martensitic Phase Transformation (MPT) when they aresubmitted to mechanical or thermal actions, and that gives them some specific characteristics.The thermomechanical behavior of SMA is now well controlled. However, the knowledge of theSMA fracture behavior is a major challenge for their design and sizing for their sustainableindustrialization. This research project has focused on the understanding, describing and quantifyingof the phenomenon of localization at the crack tip due to stress-induced MPT. The study includestwo main aspects: the development of an analytical model and its experimental correlation bysimultaneous field’s measurements during tests on cracked NiTi specimens. Two analytical modelsbased on the linear fracture mechanics and those introduce the asymmetrical nature of the SMAbehavior in tension/compression, were developed for the prediction of transformation zones in thevicinity of the crack tip, taking into account the fracture mode (elementary and mixed ones)and the radii of curvature of the crack tip. A testbench with the measurement of simultaneouskinematic field with Digital Image Correlation (DIC) and thermal field with infrared thermographywas designed for mapping the experimental fields during fracture tests in mode I on pre-crackedspecimen. This good correlation of analytical models opens up many perspectives on the analysisof thermomechanical coupling associated with the MPT at the crack tip, the enrichment of the initialanalytical models, and comparison with experimental results for more complex failure modes (II andmixed I+II).

Previous thread rolling methods for the plastic limit are shown to be inadequate and inaccurate. Alternative methods for the plastic limit are shown to be imprecise and unreliable. The strength-based concept and use of the fall-cone test to determine the plastic limit are shown to be flawed. An apparatus that replicates Atterberg’s rolling technique, devised and developed by the author, is described, referred to as the Barnes Apparatus. A thread of soil is rolled between two plates configured to permit extrusion and reduction of diameter with much less operator interference than with the standard test and judgement of the crumbling condition is eliminated. Using a loading device nominal stresses are derived and from dial gauge readings diametral strains are determined for each rolling traverse of the soil thread. Toughness has previously only been studied in an empirical or qualitative manner. From plots of nominal stress vs. strain the workability or toughness of the plastic soil is determined as the work/unit volume. The apparatus and test are appropriate to a wide range of soils. Threads are tested over a range of water contents from near the sticky limit to the brittle state. Good correlations between toughness and water content display an abrupt ductile-brittle transition and give an accurate definition of the plastic limit. From the correlations useful properties are obtained such as the maximum toughness at the plastic limit, the toughness limit, the water content at zero toughness, the stiffness transition, the toughness coefficients, the toughness index and the workability index. An investigation into the significance of the soil thread diameter of 3 mm in the standard plastic limit test has found that as the water content of a soil reduces it undergoes a transition from fully plastic, to cracked, to brittle, largely regardless of the diameter of the thread. It is recommended that the 3 mm diameter requirement is withdrawn from the standard test procedure as unnecessary and emphasis placed on observing the behaviour of the soil thread as it is rolled by hand. A review of the relationship between the clay matrix and the granular particles in a soil has found that the linear law of mixtures and activity index are appropriate only at high clay contents. The terms granular spacing ratio and matrix porosity are introduced to explain the effect of the granular particles on the toughness and plastic limit. An analysis confirms that with small diameter soil threads large granular particles affect the results disproportionately. An aggregation ratio term is introduced to explain the change in toughness in the clay matrix as its water content reduces towards the plastic limit. To assess the effect of granular particles in a clay matrix on the toughness and plastic limit the results of tests conducted on mixtures of a high plasticity clay and silt, and sand particles of two different sizes are discussed. Smaller particle sizes are found to have a greater effect on reducing the toughness and the plastic limit of the clay. In the ceramics industry mixing different clays together to obtain suitable properties is common. The toughness and plastic limits of two pairs of mixed clays do not follow the linear law of mixtures but are dependent on the total clay content and the content of a dominant clay mineral.

The effect of individual and combined zirconium and manganese additions have been compared for an AA2198 6 mm thick sheet in T351 temper regarding their influence primarily on recrystallisation resistance and secondly on fracture toughness and overageing resistance. A complete characterisation of the dispersoid distributions was carried out for a deeper understanding of the effects of the Al3Zr and Al20Cu2Mn3 particles, involving studying their formation from the as-cast and homogenised stage.The most important finding in this work was the lower recrystallisation resistance in the alloy containing 0.1 wt%Zr + 0.3 wt%Mn compared to that containing only 0.1 wt%Zr. This result was rather unexpected, if one considers the opposite microsegregation patterns of Zr and Mn during casting, which leads to dispersoids occupying the majority of the grains’ volume and minimising dispersoid-free zones that could be potential sites for nucleation of recrystallisation. The other two alloys with dispersoid additions 0.05 wt%Zr + 0.3 wt%Mn and 0.4 wt%Mn, were partially and fully recrystallised respectively in the rolled T351 condition.Equally important in this work, was the observation that the opposite microsegregation trend of Zr and Mn sufficed to restrict grain growth in unrecrystallised areas. The 0.1Zr-0.3Mn alloy exhibited the lowest grain size of all alloys, both in the T351 temper and after annealing at 535oC for up to 144 hours. The reason for this was the combined action of Al20Cu2Mn3 dispersoids and Mn solute in the regions where the Zr concentration was low (i.e. near the grain boundaries), which offered additional pinning pressure to those areas compared to the 0.1Zr alloy.The lower recrystallisation resistance of the 0.1Zr-0.3Mn alloy was explained on the grounds of two main factors. The first was the lower subgrain size and hence stored energy within bands of Al20Cu2Mn3 dispersoids, which increased the driving force for recrystallisation in these regions. The second was the interaction between Zr and Mn that led to a decrease in the Al3Zr number density and pinning pressure. Since Zr was the dominant dispersoid family in terms of inhibiting recrystallisation, inevitably this alloy became more prone to recrystallisation. The Al3Zr pinning pressure was found to be much lower especially within bands of Al20Cu2Mn3 dispersoids. The detrimental effect of the Mn addition on the Al3Zr distribution was proven not to result from the dissolution of Zr within Mn-containing phases, and several other phases, at the grain interior and also in grain boundaries. The observed effect could not be precisely explained at this stage.Concerning mechanical properties, the 0.1Zr alloy exhibited the best combination of properties in the Kahn tear tests for fracture toughness. Further, it had a higher overageing resistance compared to the 0.1Zr-0.3Mn alloy.As an overall conclusion from this work, considering all the studied properties here that are essential for damage tolerant applications, the addition of 0.1 wt%Zr to the AA2198 6 mm thick sheet was found to be superior to that of the combined addition of 0.1 wt%Zr + 0.3 wt%Mn.