Esse trabalho tem como objetivo estabelecer um método simples de ensaio que permita determinar a resistência à tração e módulo elástico de partículas individuais de agregados graúdos naturais submetidas à carga de compressão. O método de ensaio foi desenvolvido baseado no ensaio de carga pontual (Point Load Test) que permite obter a resistência à tração de partículas. Para a determinação do módulo de elasticidade foi acoplado ao método um LVDT e foi satisfeita a condição para aplicação da teoria de contato de Hertz (contato curvo-plano entre as partículas e as fixações de aplicação da carga). Inicialmente a metodologia foi avaliada utilizando como material de referência partículas de vidro (com geometrias similares aos agregados). Após a validação no vidro, o método de ensaio foi aplicado em agregados graúdos de granito. Propôs-se um método de seleção de partículas com base na sua distribuição de frequência de absorção, com o intuito de reduzir a quantidade de partículas testadas mecanicamente necessárias para obter a distribuição de Weibull da resistência à tração (e módulo de elasticidade). Para tanto, foi feita a determinação da absorção de água individual de centenas de partículas selecionadas por amostragem a esmo da população de agregados. Com base nos resultados, foi possível determinar a distribuição de Weibull da resistência à tração e módulo de elasticidade das partículas. Observou-se que as resistências à tração variaram de 3 a 15 MPa. Os agregados possuíam aproximadamente 10% da população de partículas com resistência à tração inferior a 5 MPa, o que pode influenciar as classes de resistência à compressão de concretos >50MPa. Os módulos elásticos dos agregados também foram variáveis (18-67 GPa) e aproximadamente 10% da população de partículas com módulo elástico <30 GPa. Isso pode limitar o módulo de elasticidade do concreto (que geralmente é em torno de 27 GPa), dependendo do processo de escolha dos agregados. As funções exponenciais inversas fundamentais entre essas propriedades mecânicas e a porosidade foram confirmadas (para valores médios). / The aim of this work is to establish a simple test method to determine the tensile strength and elastic modulus of individual natural aggregate particles subjected to a compression load. The test method was developed based on the Point Load Test, that allows to obtain the tensile strength of particles. For the determination of the elastic modulus, an LVDT was coupled to the method and the condition for application of Hertz contact theory (curved-plane contact between the particles and the load application fixations) was satisfied. Initially, the method was evaluated using glass particles as reference (with geometries similar to aggregates). After validation on the glass, the test method was applied to coarse granite aggregates. A method of particle selection was proposed based on its absorption frequency distribution, in order to reduce the amount of mechanically tested particles required to obtain the Weibull distribution of tensile strength (and elastic modulus). For this purpose, the determination of the individual water absorption of hundreds of particles selected by random sampling of the population of aggregates was made. Based on the results, it was possible to determine the Weibull distribution of the tensile strength and elastic modulus of the particles. The tensile strengths ranged from 3 to 15 MPa. The aggregates had approximately 10% of the particles population with tensile strength less than 5 MPa, which may influence the classes of concrete with compressive strength > 50MPa. The elastic modulus of the aggregates was also variable (18-67 GPa), with approximately 10% of the particle population with elastic modulus <30 GPa. This may limit the elastic modulus of the concrete (usually around 27 GPa) depending on how the aggregates are selected. The fundamental inverse exponential functions between these mechanical properties and the porosity were confirmed (for mean values).

Esta dissertação insere-se nas áreas de qualidade laboratorial e de ensaios de controle de concreto, especificamente quanto à propriedade módulo estático de deformação ou módulo de Young. A motivação do trabalho é a elevada variabilidade de resultados experimentais observada pelo meio técnico nacional em ensaios interlaboratoriais, cujos resultados indicam desvios-padrão totais da ordem de 3,5 GPa, valor significativo para o controle tecnológico de obras de construção civil. Os objetivos buscados foram a identificação das parcelas da variabilidade oriundas da produção e do ensaio, com especial atenção àquela originada na instrumentação para medida das deformações durante o ensaio, e a discussão da aplicabilidade do conceito semiprobabilístico normativo à propriedade módulo de deformação do concreto. Além disso, a própria discussão da aplicabilidade da sistemática de pesquisa e análise sobre este tipo de ensaio e de material constou como um objetivo do trabalho. Para tal, desenvolveu-se um programa experimental em duas etapas: a primeira foi destinada às avaliações de acurácia (precisão e exatidão) do método de ensaio. As avaliações se deram segundo roteiros da área metrológica para validação de métodos e sistemas de medida. De quatro instrumentações para medida das deformações testadas, uma se mostrou mais precisa (identificada como clip gages) e outra se mostrou a mais suscetível a erros sistemáticos e aleatórios entre as testadas (identificada como compressômetro com dois relógios comparadores). Recomendou-se a ampliação do programa experimental para o âmbito interlaboratorial, pois, a rigor, o método de ensaio vigente não poderia ser considerado validado em termos de acurácia baseando-se unicamente nos resultados deste programa experimental. Porém, concluiu-se pela possibilidade de aceitação prática do método independentemente da utilização de três de um total de quatro tipos de instrumentação para medida das deformações testados em ensaio, sem que houvesse prejuízo para a produção ou o controle tecnológico usual desta propriedade. Na segunda etapa, obteve-se um Diagrama de Dosagem e estudou-se um cenário de fornecimento de concreto sob critérios estatísticos diferentes de atendimento à especificação de módulo de deformação: utilização do valor característico e do valor médio, com diferença de 4 GPa entre eles. Estimou-se um aumento da ordem de 9% no deslocamento vertical de uma viga simples bi-apoiada quando executada com o concreto de menor módulo em relação à execução com o de maior módulo. Por sua vez, o concreto de maior módulo exigiria um aumento no consumo de cimento da ordem de até 200 kg/m3, se conservados todos os insumos materiais e os demais parâmetros tecnológicos contidos nos traços. Concluiu-se pela aplicabilidade do uso da sistemática empregada na avaliação da acurácia do método de ensaio e do uso do conceito semiprobabilístico para esta propriedade. / This work is developed into the areas of laboratorial quality and concrete control tests, specifically focusing on the static modulus of elasticity or Young´s modulus. The motivation of this work is the high variability of experimental results observed by national technicians in interlaboratorial tests. These results show total standard deviations of around 3.5 GPa, a significant value for the technological control for civil construction. The main objectives are the identification of the variability fragments derived from the production and test, specially the ones related to the instrumentation for measuring deformations during the test, and the discussion of the semi-probabilistic concept applicability on the concrete Young´s modulus control. Moreover, the discussion of the applicability of the procedure used in this work and its analysis are also objective pursued here. The experimental program was developed in two steps: the first step covered the accuracy assessments (precision and exactness) of test method. The assessments were carried out according to instructions from Metrology concepts for the validation of the methods and the measure systems. One out of four instrumentations for measuring the tested deformations proved to be more precise (identified as clip gages) and another one proved to be more susceptible to systematic and random errors (identified as a compressometer with two dial indicators). The extension of the experimental program to an interlaboratorial scope is recommended because the current test method could not be considered valid based only on the results of this experimental program. However, it was shown that the practical acceptance of the test method for three among the four kinds of instrumentations analyzed, without damaging the production or the usual technological control of this property, is possible. On the second step, a mix design diagram was obtained and a case of supply of concrete under different statistical criteria (fulfillment the modulus of elasticity specification): the use of the characteristic value and the average value, with difference of 4 GPa between them. An increase of 9% on the vertical transference of a simple dual supported beam was observed when using a lower modulus concrete, when compared to another one with a higher modulus. On the other hand, the modulus increase would require an increment in the cement consumption up to 200 kg per cubic meter, if all the material inputs and further technological parameters is maintained. The final conclusion was that the procedure used on the assessment of the test method accuracy and the semi-probabilistic concept on this material property is applicable.

Les alliages de titane β-métastables biocompatibles suscitent un intérêt croissant pour les applications médicales grâce à leur comportement superélastique et/ou effet mémoire de forme, leur excellente résistance à la corrosion et leur bonne aptitude à la déformation à froid. Dans le cadre de cette thèse, un alliage superélastique Ti-26Nb et un alliage à mémoire de forme Ti-24Nb ont été élaborés en creuset froid en semi-lévitation magnétique et ont fait l'objet d'une caractérisation approfondie sur le plan microstructural et mécanique. Les mécanismes de déformation activés lors d'une sollicitation mécanique ont été identifiés pour les deux alliages au moyen d'essais de traction couplés à des mesures in-situ en diffraction des rayons X. Une procédure d'optimisation basée sur des traitements thermo-mécaniques nano-structurants a été développée pour augmenter simultanément la résistance mécanique et la superélasticité tout en conservant un bas module élastique. Un ensemble de propriétés qui conditionne la réussite de la pose d'implant en améliorant la qualité de transfert des contraintes à l'interface os/implant. Les évolutions microstructurales à l'origine de l'optimisation de ces propriétés ont été étudiées par diffraction des rayons X, microscopie électronique à transmission et essais mécaniques. Ce travail se conclut par une introduction à la modélisation micromécanique du comportement du Ti-26Nb. Les caractéristiques cristallographiques de la transformation martensitique ont été déterminées en se basant sur la théorie de Ball et James. L'influence de l'orientation cristallographique sur le comportement mécanique des monocristaux a été étudiée. / Biocompatible metastable β-titanium alloys have attracted much attention for biomedical applications in recent years thanks to their superelastic and/or shape memory behavior, their superior corrosion resistance and their excellent cold workability. In this present study, a superelastic Ti-26Nb alloy and a shape memory Ti-24Nb alloy were produced by the cold crucible levitation melting method. A detailed microstructural and mechanical characterization were performed. The deformation mechanisms occurring during uniaxial deformation were identified for these two alloys by coupling in situ tensile testing with X-ray diffraction measurement. An optimization route based on nanostructuring process was developed in order to enhance both strength and superelasticity while keeping a low elastic modulus. These properties are required to improve the load transfer along the bone/implant interface which is essential to the success of implants. The microstructural evolution during the thermomechanical process resulting in the optimization of properties was investigated through tensile tests, X-ray diffraction and transmission electron microcopy. The last part of this study deals with an introduction of micromechanical modeling of the Ti-26Nb behavior. The crystallographic features of the martensitic transformation were determined by applying the Ball and James theory. The influence of the crystallographic orientation on the mechanical response was investigated for tension and compression.

In this article the correlation between the average molar mass and the melt flow rate (MFR) is achieved. Based on the example of Polyoxymethylene (POM) it is shown that a high average molar mass is associated with a low MFR (high viscosity). On the basis of this dependency, the mechanical properties of static and dynamic tensile strength, elastic modulus, hardness and notched impact strength are investigated. It was found that the characteristic values of static tensile strength, elastic modulus and hard-ness increase with increasing MFR (decreasing viscosity). On the other hand the dynamic long-term properties and notched impact strengths decrease with increasing MFR. / Im Beitrag wird der Zusammenhang zwischen der mittleren molaren Masse und des Schmelzfließindex (MFR) hergestellt. Dabei wird am Beispiel von Polyoxymethylen (POM) ersichtlich, dass eine hohe mittlere molare Masse mit einem geringen MFR (hochviskos) einhergeht. Basierend auf dieser Abhängigkeit werden die mechanischen Eigenschaften statische und dynamische Zugfestigkeit, E-Modul, Härte sowie Kerbschlagzähigkeit untersucht. Dabei konnte festgestellt werden, dass die Kenngrößen statische Zugfestigkeit, E-Modul und Härte mit steigendem MFR (abnehmende Viskosität) zunehmen. Die dynamischen Langzeiteigenschaften und Kerbschlagzähigkeiten sinken hingegen mit zunehmendem MFR.

Les hydrates de gaz sont des composés cristallins stables à haute pression et à basse température, très répandus sur terre, notamment dans les fonds marins au niveau des marges continentales, où ils contribuent à la stabilité des sédiments par leur cohésion et leur adhésion aux surfaces minérales. Cependant, le comportement mécanique des hydrates en soi a été peu ou pas étudié à l’échelle du pore. L’objectif de cette thèse est d’étudier les conditions de stabilité et les propriétés mécaniques en traction de l’hydrate de méthane à l’échelle du pore, dans une configuration comparable à celle qu’on peut trouver dans les milieux poreux sédimentaires.Ici, nous étudions d’abord par microscopie optique les conditions de formation, de croissance et de dissociation de l’hydrate de méthane à l’interface eau/CH4 dans un micro-capillaire en verre utilisé à la fois comme un pore modèle et comme une cellule optique résistante à haute pression et à basse température. Ensuite, en développant une méthode originale in situ et sans contact : "dépression thermo-induite" on détermine les propriétés mécaniques en traction d’une coquille polycristalline d’hydrate de méthane. L’hydrate est nucléé à basse température sur l’interface eau/CH4, qui est rapidement recouverte d’une "croûte" polycristalline d’hydrate. À partir de cette croûte, l’hydrate pousse de part et d’autre de l’interface : dans l’eau sous forme "d’aiguilles" cristallines, dans le gaz, sous forme de "filaments" cristallins, et enfin entre le substrat et le gaz sous forme d’un "halo". Le halo qui est un film polycristallin avançant sur le substrat, en chevauchant un film d’eau, ralentit et finit par s’immobiliser et s’accrocher au substrat. À partir de ce moment, "la coquille" polycristalline, constituée de la croûte et du halo, forme une barrière entre l’eau et le gaz. Les tests de traction sont effectués par génération d’une dépression dans le compartiment eau en augmentant la température à pression de méthane constante.Les propriétés élastiques en traction de la coquille (module élastique et contrainte de rupture) sont déterminées en fonction de la taille des grains, contrôlée ici par les deux paramètres : le sous-refroidissement par rapport à la température d’équilibre, et le temps de mûrissement. On trouve un comportement élastoplastique à caractères ductile et fragile mélangés. Nos données de contrainte de rupture s’insèrent dans un écart de cinq ordres de grandeurs de taille de grain, et de trois ordres de grandeurs de la contrainte de rupture (entre des données de simulation à l’échelle nanomètrique et des données expérimentales à l’échelle millimétrique). L’effet de taille de grain sur la contrainte de rupture de l’hydrate de méthane peut être un facteur contribuant à la déstabilisation des pentes continentales. / Gas hydrates are ice-like crystals stable at high pressure and low temperature. They are ubiquitous on earth, notably at the edges of continental shelves, where they contribute to the mechanical stability of marine sediments, by hydrate cohesion and hydrate adhesion to mineral particles. However, the mechanical behavior of gas hydrates at pore scale has been hardly or not at all studied. The purpose of this thesis is to study the stability conditions and the tensile mechanical properties of methane hydrate at pore scale in a representative pore habit of gas hydrate in a sedimentary medium.Here, using optical microscopy, first the formation, growth and dissociation conditions of methane hydrate are investigated across a water/CH4 interface in glass micro-capillaries used both as a pore model and as an optical cell resisting high pressure and low temperature. Then by developing a contactless and an in situ method, "thermally induced depressing", tensile mechanical properties of polycrystalline methane hydrate shell are determined. At low enough temperature, the hydrate nucleates as a polycrystalline "crust" over the water/CH4 interface. From this crust, the hydrate continues growing on both sides of the interface: in the water as "needle like crystals", in the gas as "hair like crystals", and finally between the gas and the substrate as a polycrystalline film, the "halo". The halo advances slowly on the substrate, riding over a water film, and comes to rest and adheres to the substrate. From then on, the "shell" (crust and halo) isolates the water from the gas. Tensile tests are carried out by generating a depression in the water compartment by increasing temperature at constant methane pressure.Tensile elastic properties of the shell (elastic modulus and the tensile strength) are determined as a function of the grain size, controlled here by two parameters, supercooling compared to the equilibrium temperature and the annealing time. We find elastoplastic behavior, with mixed ductile and brittle characteristics. Our data on tensile strength contribute to fit the gap of five orders of magnitude of grain size, and three orders of magnitude of tensile strength (between molecular simulations at nanometre scale and current experiment at millimetre to centimetre scale). The effect of grain size on the tensile strength of methane hydrate could be a factor contributing to the destabilization of continental slopes.

Cement-based concrete is one of the main construction materials that is widely used for many construction applications due to its strength, durability, reflectivity, and versatility. However, it is acknowledged that production of cement as a primary material of concrete releases 1.8 Gt carbon dioxide (CO2) into the environment. It is estimated that one ton of cement production releases one ton of CO2 to the atmosphere. That is why, this work aims to create a concrete that could be an alternative to cement-based concrete. Geopolymer concrete (GPC) is an eco-friendly construction material and an alternative to conventional concrete that is produced by reacting aluminate and silicate bearing constituents with a caustic activator (i.e. sodium-based or potassium-based). Both potassium and sodium have been considered as generally safe intergradient by the FDA, based upon the observance of several good manufacturing practice conditions of use. Theses activators are used in various application including concrete, food, as a stabilizer, and as a thickening agent. Moreover, these activators are also used in making soap, as an electrolyte in alkaline batteries and in electroplating, lithography, and paint and varnish removers. Medically, these activators are widely used in the wet mount preparation of various clinical specimens for microscopic visualization of fungi and fungal elements in skin, hair, nails, and even vaginal secretions, Currently, it was determined that these activators solution were found to be a safe and effective treatment of plane warts. Despite the developments in the studies relating to GPC made by various precursors such as fly-ash and slag in the literatures, the use of GPC made by fly-ash and bottom-ash has not been overly researched. In this study, attempts have been made to produce a unique mix proportion for Potassium-based GPC made by fly-ash and bottom-ash and investigate various mechanical properties of this type of GPC including elastic modulus, freeze-thaw resistance, heavy metal leach-ability and corrosion in both laboratory and real environmental conditions using Non-Destructive Tests (NDT)s. / Graduate / 2021-12-15

This thesis is concerned to the study of behaviour of fibre composites with ceramics matrix. The composite consists of pyrolysed polysiloxane matrix reinforced by ceramic fibre Nextel 720. Main aim of this work is optimisation of fibre matrix interface through the selection of suitable precursor of the matrix with respect to temperature stability, sufficient strength and reasonable fracture toughness. Samples of matrices were exposed to the long term heat treatment in the range 1100 – 1500 °C. The mechanical properties as hardness and indentation elastic modulus were determined after heat treatment. Selected precursors of matrices were used for composite fabrication. Elastic modulus and fracture toughness at room and elevated temperatures were studied. Discussion is dedicated to the description of changes in mechanical properties with respect to chemical processes taking place during high temperature exposition. Further, reasons of fracture behaviour of composite materials are discussed, and finally, gained knowledge and outlined possibilities of subsequent development are summarised.

The diploma thesis deals with the stability determination of model O/W (30/70) emulsions at 25°C. In fact, the time and emulsifier concentration (Tego Care PS) dependences of physical properties (aging) were monitored. In the second part of the work, the influence of conservant on emulsion stabilities were studied. In order to study physical properties of emusions rheometry, differential scanning calorimetry (DSC) and optical microscopy were employed. The rheological measurement provided information on viscosity and viscoelastic modulus. DSC experiments used the repeated freezing/thawing cycles which allowed monitoring of changes in crystallization temperature of water present in emulsions and melting enthalpy of ice formed during the cooling. The optical microscopy was used to examine the change in oil droplet size in the course of emulsion destabilization and phase separation. In this case the image analysis was carried out using program HarFA. The results showed that due to the emulsion creaming, the oil droplets diffuse and aggregate which causes phase separation. Those processes were quickest for the emulsion with lowest emulsifier concentration 0.1 % (destabilization during 51 days) The emulsions with emulsifier concentration about 1.5 and 1.3 % were stable at least for 4 months. The presence of the coemulsifiers increased the elastic modulus and descreased the phase difference due to the network formation. It was shown that for the stability determination is necessary to use conservant due to risk of microbial contamination. DSC experiments allowed to distingush samples prepared under different conditions. Lower rotational speed during emulsion preparation caused the appearance of two melting and crystalization peaks while for higher speed only one peak was observed.

This thesis deals with compares the procedures carried out in the cyclical load triaxial testing device according to CSN EN 13286-7, and the procedures performed in the United States of America. In the practical part elasticity moduls of mixed recycled material are experimentally compared with mixed recycled material containing binder(connective material) and with fine-grained soil in the cyclical load triaxial testing device. Further the thesis assesses the use of mixed recycled material in the construction of a third class low-load pavement.

<p>Combination of the Calphad method and theoretical calculations provides new possibilities for the study of materials science. This work is a part of the efforts within the CCT project (Centre of Computational Thermodynamics) to combine these methods to facilitate modeling and to extend the thermodynamic databases with critically assessed volume data. In this work, the theoretical calculations refer to first-principles and Debye-Grüneisen calculations. The first-principles (i.e. ab initio) electronic structure calculations, based on the Density- Functional Theory (DFT), are capable of predicting various physical properties at 0 K, such as formation energy, volume and bulk modulus. The ab initio simulation software, VASP, was used to calculate the binding curves (i.e. equation of state at 0 K) of metallic elements, cubic carbides and nitrides. From the binding curves, the equilibrium volumes at 0 K were calculated for several metastable structures as well as stable structures. The vibrational contribution to the free energy was calculated using the Debye-Grüneisen model combined with first-principles calculations. Two different approximations for the Grüneisen parameter, γ, were used in the Debye-Grüneisen model, i.e. Slater’s and Dugdale-MacDonald’s expressions. The thermal electronic contribution was evaluated from the calculated electronic density of states. The calculated thermal expansivities for metallic elements, cubic carbides and nitrides were compared with Calphad assessments. It was found that the experimental data are within the limits of the calculations using the two approximations for γ. By fitting experimental heat capacity and thermal expansivity around Debye temperatures, we obtained optimal Poisson’s ratio values and used them to evaluate Young’s and Shear moduli. In order to reach a reasonable agreement with the experiments, it is necessary to use the logarithmic averaged mass of the constitutional atoms. The agreements between the calculations and experiments are generally better for bulk modulus and Young’s modulus than that for shear modulus. A new model describing thermodynamic properties at high pressures was implemented in Thermo-Calc. The model is based on an empirical relation between volume and isothermal bulk modulus. Pure Fe and solid MgO were assessed using this model. Solution phases will be considered in a future work to check the model for compositional dependence.</p>