Les pièces situées dans des zones chaudes/tièdes (300-400°C) de l'avion sont actuellement en titane (mât moteur) ou en composite à matrice époxy (plenum). Comment pourrait-on diminuer la masse de ces pièces tout en évitant leur dégradation à hautes températures de fonctionnement ? Le projet TACT (Technologie pour Aérostructures composites Tièdes), porté par Nimitech Innovation® (Groupe LAUAK), propose une solution innovante consistant à mettre en oeuvre par voie RTM des pièces structurales tièdes à base de renfort en fibres de carbone (FC) et de matrice Cyanate ester (CE). Le choix de la matrice thermodurcissable CE est justifié par son caractère thermostable, c'est-à-dire sa capacité d'opérer en continu à de hautes températures de fonctionnement (avec une température de transition vitreuse Tg>300°C). Par ailleurs, elle possède la facilité de mise en oeuvre des époxydes du fait qu'elle s'adapte généralement bien aux paramètres du procédé RTM. Toutefois, l'exothermie élevée de la matrice CE lors de la réticulation implique un gradient de température dans la pièce composite et peut ainsi engendrer des problèmes de surchauffe. Les travaux scientifiques menés dans le cadre de cette thèse se focalisent sur la problématique de surchauffe de la résine pendant le processus de polymérisation très exothermique dans le moule RTM. L'objectif serait ainsi de maîtriser le cycle de cuisson du composite afin d'éviter tout problème d'emballement ou de dégradation pendant la réticulation de la matrice. Dès lors, la thèse s'organise de la manière suivante : dans un premier temps, le comportement thermocinétique de la matrice CE (pure et catalysée) est analysé pendant l'étape de réticulation, et ceci dans l'optique de contribuer à l'optimisation de cycle de cuisson lors de la mise en oeuvre du composite FC/CE par procédé RTM. Ensuite, les propriétés thermiques (capacité calorifique, conductivité, diffusivité) en fonction du degré d'avancement de la résine CE sont menés afin d'évaluer le gradient thermique régi par l'équation de la chaleur permettant de maîtriser la cuisson de la résine dans l'épaisseur. Par ailleurs, la vitrification de la matrice CE est étudiée par le suivi de la température de transition vitreuse Tg en fonction de la température et du taux d'avancement à l'aide de différents techniques de mesure (DSC, DMA, TMA). Enfin, une modélisation de la vitrification à l'aide du modèle Di-Benedetto permettra l'estimation de la température de la transition vitreuse Tg ∞ pour le réseau tridimentionnel entièrement réticulé. / Aeronautical parts which operate in high temperature area (300-400°C) are currently made of titanium (aircraft pylon) or composite materials based on epoxy matrix (plenum). In which extent the weight of these pieces could be reduced as well as avoiding their degradation when operating at these working temperature ranges? TACT project (Technologie pour Aérostructures composites Tièdes), overseen by Nimitech Innovation® (Groupe LAUAK), suggests an innovative solution based on the development of high performance composites parts reinforced by carbon fibers (CF) and cyanate ester matrix (CE) through RTM process. The CE resin belongs to the class of high-performance thermosetting polymers and is mainly chosen in this project due to its thermal stability when operating at high temperatures (with a glass transition Tg>300°C), as well as epoxy-like processability. However, the cross-linking reaction exhibits highly exothermic process, resulting in non-linear increase in internal temperature, which may cause a temperature overshoot. The scientific work carried out within this thesis focuses on the problem of overheating of the resin during the highly exothermic polymerization process in the RTM mold. The objective would thus be to control the curing cycle of the composite in order to avoid problems of runaway or degradation during the crosslinking of the matrix. Hence, the thesis is organized as follows: firstly, thermokinetic behavior of CE resin is analyzed during the crosslinking process in order to optimize the curing cycle. Secondly, thermal properties (heat capacity, conductivity, diffusivity) are identified as a function of the conversion degree in order to evaluate the thermal gradient covered by the heat equation making it possible to control the curing along the thickness of the composite. Moreover, the vitrification of the cyanate ester matrix is studied by monitoring the glass transition temperature Tg as a function of the temperature and conversion degree using different methods (DSC, DMA, TMA). Finally, Di-Benedetto model, a vitrification model, is chosen in order to identify the glass transition temperature Tg∞ of a full crosslinked resin.

In this work, the material distribution, structure of fiber orientation and fiber attrition in sandwich and push-pull injection molded short fiber composites are investigated, regarding the effect of fiber content and processing parameters, given its direct relevance to mechanical properties. The prediction of the tensile strength of conventional, sandwich and push-pull injection molded short fiber composites are derived by an analytical method of modified rule of mixtures as a function of the area fraction between skin and core layers. The effects of fiber length and fiber orientation on the tensile strength are studied in detail. Modeling of the specialized injection molding processes have been developed and performed with the simulation program in order to predict the material distribution and the fiber orientation state. The secondorder orientation tensor (a11) approach is used to describe and calculate the local fiber orientation state. The accuracy of the model prediction is verified by comparing with corresponding experimental measurements to gain a further basic understanding of the melt flow induced fiber orientation during sandwich and push-pull injection molding processes.

Werkstoffe auf Basis duroplastischer Harze besitzen exzellente Gebrauchseigenschaften für viele Bereiche des industriellen Einsatzes. Vor allem durch die Spritzgießverarbeitung rieselfähiger duroplastischer Formmassen entsteht ein hohes Substitutionspotential gegenüber Bauteilen aus Metallen oder Hochleistungsthermoplasten. Jedoch führen bestehende Erkenntnisdefizite im Prozessverständnis zu Ressentiments hinsichtlich des Einsatzes duroplastischer Werkstoffe. Ziel der Untersuchungen dieser Arbeit war die Ermittlung und Analyse der prozessinduzierten Werkstoffstruktur von spritzgegossenen technischen Phenolharzformteilen. Dabei wurden zum einen das Füllen der Werkzeugkavität und die sich ausbildende Faserorientierung untersucht und zum anderen die sich während des Temperns verändernde chemische Struktur. Anhand von Platten- sowie Zugprüfkörpern wurden sowohl beim Spritzgießen als auch beim Tempern Parametervariationen durchgeführt und die jeweils resultierende Werkstoffstruktur sowie deren Einfluss auf die Formteileigenschaften analysiert. Die Ergebnisse zeigen, dass die Strömungsverhältnisse während der Werkzeugfüllung stark von den Prozessparametern und der Werkstoffzusammensetzung abhängig sind. Dadurch wird auch die Faserorientierung beeinflusst, sodass im Formteil lokal und richtungsabhängig stark unterschiedliche Eigenschaften entstehen können. Darüber hinaus konnte anhand einer alternativen Tempermethode geklärt werden, warum es beim Tempern zu einem Abfall der mechanischen Eigenschaften kommt und eine Möglichkeit zur Vermeidung gegeben werden. / Because of their excellent properties, thermosets can be applied in a bright range of industrial applications. Especially thermoset molding compounds can be processed highly effective by injection molding, which enables them to substitute metals or high performance thermoplastics. But there is a deficit in process understanding, which limits the industrial application. The objective of this work is the investigation and analysis of the process induced material structure of injection molded technical phenolic components. Therefor the filling of the cavity with the resulting fiber orientation and the chemical processes during post-curing were examined. A parameter variation with injection molded plate and tensile specimens were done and the resulting material structure and the effect on the component properties were analyzed. The results show a big influence of the process parameter and the material on the flow condition during the filling of the cavity. Thereby also the fiber orientation is affected. This leads to process-depending local and direction-depending properties. In addition, this work shows an alternative method for post-curing to avoid the decrease of mechanical properties.

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No / Advances in micromoulding technology are now allowing mass production of complex, three-dimensional functional products having sub-milligram masses and carefully tailored surface finishes. In order to create a viable manufacturing process for these components, accurate process monitoring and product evaluation are essential in order to highlight process problems and production of substandard parts. The present study describes work implementing a suite of sensors on a commercial micromoulding machine for detailed process interrogation. Evaluation of demoulded products is performed with a single camera based system combined with custom software to allow for three-dimensional characterisation of products during the process.

In order to reduce over-dependency on fossil fuels and to create an environment that is free of non-degradable plastics, and most importantly to reduce greenhouse gas emission, bio-based products are being developed from renewable resources through intense research to substitute conventional petrochemical-based plastics with renewable alternatives and to replace synthetic fibers with natural fibers. Many authors have done quite a lot of work on synthesizing polymers from renewable origin. Polylactic acid (PLA) has been developed and characterized, and it was found that it has enormous potential and can serve as an alternative to conventional thermoplastics in many applications. Modification of the plant oil triglycerides has been discussed by many authors, and research is still going on in this area. The challenge is how to make these renewable polymers more competitive in the market, and if possible to make them 100% bio-based. There is also a major disadvantage to using a bio-based polymer from plant oils because of the high viscosity, which makes impregnation of fibers difficult. Although natural fibers are hydrophilic in nature, the problem of compatibility with the hydrophobic matrix must be solved; however, the viscosity of the bio-based resin from plant oils will complicate the situation even more. This is why many authors have reported blending of the renewable thermoset resin with styrene. In the process of solving one problem, i.e reducing the viscosity of the renewable thermoset resin by blending with reactive diluents such as styrene, another problem which we intended to solve at the initial stage is invariably being created by using a volatile organic solvent like styrene. The solution to this cycle of problems is to synthesize a thermoset resin from plant oils which will have lower viscosity, and at the same time have higher levels of functionality. This will increase the crosslinking density, and they can be cured at room temperature or relatively low temperature. In view of the above considerations, the work included in this thesis has provided a reasonable solution to the compounded problems highlighted above. Three types of bio-based thermoset resins were synthesized and characterized using NMR, DSC, TGA, and FT-IR, and their processability was studied. The three resins were subsequently reinforced with natural fibers (woven and non-woven), glass fibers, and Lyocell fiber and the resulting natural fiber composites were characterized by mechanical, dynamic mechanical, impact, and SEM analyses. These composites can be used extensively in the automotive industry, particularly for the interior components, and also in the construction and furniture industries. Methacrylated soybean oil (MSO), methacrylic anhydride-modified soybean oil (MMSO), and acetic anhydride-modified soybean oil (AMSO) were found to be suitable for manufacture of composites because of their lower viscosity. The MMSO and MSO resins were found to be promising materials because composites manufactured by using them as a matrix showed very good mechanical properties. The MMSO resin can completely wet a fiber without the addition of styrene. It has the highest number of methacrylates per triglyceride and high crosslink density. / Akademisk avhandling för avläggande av teknologie doktorsexamen vid Chalmers Tekniska högskola försvaras vid offentlig disputation, den 6:e maj, Chalmers, KE-salen, Kemigården 4, Göteborg, kl. 10.00.

O núcleo metálico fundido (NMF), dentre outras funções, visa suportar a restauração que o sobrepõe. Muitas são as técnicas que podem ser utilizadas para a obtenção deste núcleo; o importante, porém, para manutenção da integridade dental, é a sua perfeita adaptação intra-radicular. Este trabalho apresenta um método para moldagem de condutos radiculares utilizando, como suporte intra-radicular, agulha hipodérmica. Foram realizados tratamentos endodônticos em 10 dentes humanos uniradiculares e, após o preparo, o conduto foi moldado (dupla impressão) com siliconas polimerizadas por condensação e adição, pela técnica indireta, utilizando dois tipos de suporte intra-radicular (pinjet e agulha hipodérmica). Foram obtidos 4 moldes de cada dente (interagindo material x técnica) totalizando 40 modelos, sobre os quais foram encerados os núcleos. Após a fundição, a adaptação dos núcleos foi analisada segundo dois métodos: radiográfico e microscópico. No primeiro, os dentes foram radiografados com os NMFs em posição e as imagens digitalizadas foram analisadas em computador (software ImageLab). Para avaliação microscópica, os dentes foram seccionados longitudinalmente, os núcleos foram adaptados no interior do canal e a adaptação foi verificada em microscópio de dupla coordenada, em que era calculada a porcentagem do conduto ocupada pelo NMF. Constatou-se que houve diferença estatisticamente significante (2 way ANOVA - Bonferroni - p<0.05) entre as médias dos valores de adaptação obtidos em função da técnica (agulha x pinjet) utilizando a silicona polimerizada por adição, nos dois métodos de avaliação. Não houve diferença estatisticamente significante em relação aos materiais de moldagem utilizados. Concluiu-se que a técnica utilizando agulha hipodérmica apresentou melhor fidelidade de reprodução permitindo melhor adaptação do NMF, quando utilizada a silicona polimerizada por adição. / Post and core aim to support the crown, being necessary a perfect intraradicular adaptation. There are several techniques that can be used to obtain cores, however, in order to maintain dental integrity, it is important to achieve a perfect intra-radicular adaptation. This study presents an inedited and innovator method for molding root canals using hypodermic needle as intra-radicular support. Endodontic treatment was done in 10 uniradicular human teeth and, after the preparation, root canals were molded (double print) with condensation cure silicone and addition cure silicone by indirect technique, using two types of intra-radicular supports (Pinjet and hypodermic needle). Four molds were obtained from each tooth (interacting material X technique) totalizing 40 models, on which the cores were polished. After fusion, the adaptation of cores was analyzed according to two methods: radiographic and microscopic. In the first, teeth were radiographed with the core in position and the digitalized images were analyzed through ImageLab software. For microscopic evaluation, teeth were longitudinally sectioned, the cores were adapted into root canals, and the adaptation was verified in microscope of double coordinate. The occupation percentage of core into root canal was calculated. A significant statistical difference (two-way ANOVA and Bonferroni\'s - p<0.05) was found between mean values of adaptation considering the molding technique (needle x pinjet) using the addition silicon in the two evaluated methods. There was no significant statistical difference regarding the utilized materials. It was concluded that the hypodermic needle technique had better fidelity of reproduction, permitting a good adaptation of cores, regardless of the material utilized.

As estruturas de concreto são moldadas em formas tratadas com desmoldantes e sua presença dificulta a adesão da argamassa fresca, com posterior descolamento no estado endurecido. Este estudo tem por objetivo explorar o potencial de uso de agentes retardadores em substituição aos desmoldantes convencionais na moldagem de concreto para obtenção de superfícies com maior capacidade de ancoragem das argamassas. A viabilidade do uso de agentes retardadores foi verificada determinando-se de modo comparativo a resistência de aderência à tração da argamassa e do chapisco aplicados sobre corpos de prova de concreto moldados em formas de madeira plastificada tratadas com agente retardador e com desmoldante convencional. O ensaio de aderência mostrou que a utilização de agentes retardadores possibilita maior facilidade para a remoção da camada superficial do concreto, resultando em aumento de rugosidade e absorção superficial, permitindo maior resistência de aderência da argamassa e chapisco. Posteriormente, foram coletados agentes retardadores do mercado e avaliados: desempenho na aplicação sobre as formas, impacto dos produtos na saúde do trabalhador e no meio ambiente, e o efeito retardador na hidratação do cimento. Também foram avaliados quanto: a aplicabilidade dos produtos e sua influência no preparo da superfície para o recebimento da argamassa quando tratadas com produtos retardadores e convencionais em três tipos de formas. O estudo mostrou que o uso de agente retardador pode ser uma técnica viável para reduzir os problemas de descolamento do revestimento aplicado sobre superfícies de concreto. Através dos ensaios específicos desenvolvidos e adaptados para esta pesquisa, foi possível identificar que existem diferenças de comportamentos entre os produtos, sendo eles convencionais ou retardadores, e que os tipos de forma influenciam nestes comportamentos. Foi verificado também que as formas mais simples e com custos menores podem ser mais apropriadas para utilização destes produtos. / The concrete structures are cast in molds treated with a release agent (demolding product), and its presence hinders the mortars initial adhesion in the plastic state, as well as the bond strength after hardening. The study aims is to explore the potential use of retarding agents to replace conventional release agents in the concrete formwork. The technical viability of using a retarding agent was verified by comparing the tensile bond strength of rendering mortars applied on concrete surfaces cast with a conventional release agent and on concrete surfaces cast with a retarding release agent. The results showed that, through the use of retarding products, the removal of the concrete surface layer was possible by increasing the surface roughness, the surface water absorption and the tensile bond strength of the mortar to this concrete. Performance tests were also done with retarding products commercially available in the Brazilian market to verify the behavior of such products during application on molds, their impact on workers health and on the environment, and the retarding effect in cement hydration. It was also evaluated the applicability of these products and their influence on surface preparation to receive mortar when treated with retarding and conventional products, in three types of molds. Retarding products showed to be a viable technique for reducing the detachment problems of rendering mortars applied on concrete surfaces. Through the specific tests developed and adapted for this study, it was observed that there are differences in behavior between the conventional or retarding products, and also observed how these types of molds can influence the performance of the products. It was also observed that the simplest molds with lower cost can be more suitable in this application.

Analisando o maior exame de acesso ao ensino superior de nosso país, o ENEM, percebe-se que as dimensões do quantitativo de inscritos e importância para os programas educacionais e de acesso as instituições de ensino superior, são surpreendentemente notáveis, tornando-se na segunda maior avaliação do mundo. Desta análise percebemos uma relação das provas de Matemática com a Modelagem Matemática, principalmente na Matriz de Referência do ENEM, permitindo assim um comparativo com as etapas da então denominada Modelação Matemática, ou seja, a Modelagem Matemática usada como metodologia de ensino da Matemática. As etapas da Modelação Matemática são identificadas nas questões de Matemática do ENEM através de inúmeros exemplos de questões resolvidas de edições anteriores. A Modelação Matemática é apresentada como método de ensino e aprendizagem para a resolução das questões de Matemática do ENEM. / Analyzing the greatest exam of access to higher education in our country, ENEM, it was noticed that its dimension, concerning the number of enrollment and importance to educational programs and to the access to higher education institutions, is surprisingly remarkable, making it the second-highest evaluation in the world. From this analysis, we perceive a relation between Mathematics esams and the Mathematical Modeling, mainly on ENEM’s the former reference, thus allowing a comparison of the steps of the so-called Mathematical Molding, that is, the Mathematical Modeling used as a methodology of the teaching of Mathematics. The stages of Mathematical Molding are identified on ENEM’s Mathematics questions through numerous examples of solved questions from previous editions. The Mathematical Molding is presented as a teaching-learning method, which is not necessarily the same as a method or technique for solving ENEM Mathematics questions.