abstract: The use of reinforcing fibers in asphalt concrete (AC) has been documented in many studies. Published studies generally demonstrate positive benefits from using mechanically fiber reinforced asphalt concrete (M-FRAC); however, improvements generally vary with respect to the particular study. The widespread acceptance of fibers use in the asphalt industry is hindered by these inconsistencies. This study seeks to fulfill a critical knowledge gap by advancing knowledge of M-FRAC in order to better understand, interpret, and predict the behavior of these materials. The specific objectives of this dissertation are to; (a) evaluate the state of aramid fiber in AC and examine their impacts on the mechanical performance of asphalt mixtures; (b) evaluate the interaction of the reinforcement efficiency of fibers with compositions of asphalt mixtures; (c) evaluate tensile and fracture properties of M-FRAC; (d) evaluate the interfacial shear bond strength and critical fiber length in M-FRAC; and (e) propose micromechanical models for prediction of the tensile strength of M-FRAC. The research approach to achieve these objectives included experimental measurements and theoretical considerations. Throughout the study, the mechanical response of specimens with and without fibers are scrutinized using standard test methods including flow number (AASHTO T 378) and uniaxial fatigue (AASHTO TP 107), and non-standard test methods for fiber extraction, direct tension, semi-circular bending, and single fiber pull-out tests. Then, the fiber reinforcement mechanism is further examined by using the basic theories of viscoelasticity as well as micromechanical models. The findings of this study suggest that fibers do serve as a reinforcement element in AC; however, their reinforcing effectiveness depends on the state of fibers in the mix, temperature/ loading rate, properties of fiber (i.e. dosage, length), properties of mix type (gradation and binder content), and mechanical test type to characterize M-FRAC. The outcome of every single aforementioned elements identifies key reasons attributed to the fiber reinforcement efficiency in AC, which provides insights to justify the discrepancies in the literature and further recommends solutions to overcome the knowledge gaps. This improved insight will translate into the better deployment of existing fiber-based technologies; the development of new, and more effective fiber-based technologies in asphalt mixtures. / Dissertation/Thesis / Doctoral Dissertation Civil, Environmental and Sustainable Engineering 2020

Polymeric bone scaffolds are a promising tissue engineering approach for the repair of critical-size bone defects. Porous three-dimensional (3D) scaffolds play an essential role as templates to guide new tissue formation. However, there are critical challenges arising from the poor mechanical properties and low bioactivity of bioresorbable polymers, such as poly(epsilon-caprolactone) (PCL) in bone tissue engineering applications. This research investigates the potential use of cellulose nanocrystals (CNCs) as multi-functional additives that enhance the mechanical properties and increase the biomineralization rate of PCL. To this end, an in vitro biomineralization study of both sulfuric acid hydrolyzed-CNCs (SH-CNCs) and surface oxidized-CNCs (SO-CNCs) has been performed in simulated body fluid in order to evaluate the bioactivity of the surface functional groups, sulfate and carboxyl groups, respectively. PCL nanocomposites were prepared with different SO-CNC contents and the chemical/physical properties of the nanocomposites were analyzed. 3D porous scaffolds with fully interconnected pores and well-controlled pore sizes were fabricated from the PCL nanocomposites with a 3D printer. The mechanical stability of the scaffolds were studied using creep test under dry and submersion conditions. Lastly, the biocompatibility of CNCs and 3D printed porous scaffolds were assessed in vitro. The carboxyl groups on the surface of SO-CNCs provided a significantly improved calcium ion binding ability which could play an important role in the biomineralization (bioactivity) by induction of mineral formation for bone tissue engineering applications. In addition, the mechanical properties of porous PCL nanocomposite scaffolds were pronouncedly reinforced by incorporation of SO-CNCs. Both the compressive modulus and creep resistance of the PCL scaffolds were enhanced either in dry or in submersion conditions at 37 degrees Celsius. Lastly, the biocompatibility study demonstrated that both the CNCs and material fabrication processes (e.g., PCL nanocomposites and 3D printing) were not toxic to the preosteoblasts (MC3T3 cells). Also, the SO-CNCs showed a positive effect on biomineralization of PCL scaffolds (i.e., accelerated calcium or mineral deposits on the surface of the scaffolds) during in vitro study. Overall, the SO-CNCs could play a critical role in the development of scaffold materials as a potential candidate for reinforcing nanofillers in bone tissue engineering applications. / Ph. D.

Abstract : One of the aims of the thesis is to study corrosion development in cracked concrete, in relation to the effect of concrete cover depth, exposure direction, load-induced transverse cracks, defects in the steel-concrete interface under horizontal bars caused by top-casting and self-healing of the transverse cracks. The other aim is to study the mechanical performance of reinforced concrete beams damaged by corrosion accelerated by a climate accelerated method (wetting/drying cycles in salt fog). Two main parts are included in this thesis. The first part discusses corrosion development, including corrosion initiation and propagation, in cracked concrete. The second part discusses the mechanical performance of slender and deep beams damaged by climate accelerated corrosion, in terms of failure mode, yield capacity, ultimate capacity and ultimate deflection. According to the experimental study, it was found that, corrosion always initiated under the load-induced cracks. It should be noted that corrosion initiation is related to appearance of cracks but not crack width. The surface exposure condition is also an important parameter influencing corrosion development. Top-tensioned surface is the worst exposure condition, because corrosion development was accelerated by both ponding and gravity effect of chloride solution. Furthermore, top-casting-induced defects formed in steel-concrete interface under horizontal top-cast bars due to bleeding, segregation and settlement of fresh concrete, and they were favorable for both corrosion initiation and propagation. Self-healing occurred when the cracked samples were cured in a humidity room with 100% R.H due to the formation of ettringite in the inner zone and calcite in the outer zone of crack planes. Self-healing reduced air flow through the cracks and reduced the risk of corrosion considerably. The flexural performances of slender beams were tested. Corrosion of the reinforcements modified the failure mode of reinforced concrete beams. Both yield and ultimate capacity were correlated to the maximum cross-sectional loss of tensile bars. The experimental results indicated that 1% reduction in cross-section corresponds to 1% reduction in yielding capacity and ultimate capacity. For mechanical performance of deep beams, the results show that, serious pitting corrosion on the tensile bars changed the failure mode from shear to flexure. The failure mode of corroded deep beams depends not only on span to effective depth ratio and corrosion degree of tensile bars, but also on the corrosion degree of stirrups. / Résumé : Un des objectifs de la thèse est d'étudier le développement de la corrosion dans le béton armé fissuré, en fonction de l’enrobage des armatures, des conditions d’exposition, de l’endommagement de l’interface acier-béton induit par le chargement et des défauts de l'interface acier-béton sous les barres horizontales liés à la mise en œuvre du béton frais en prenant en compte l'auto-cicatrisation des fissures transversales. L'autre objectif est d'étudier la performance mécanique des poutres en béton armé endommagées par la corrosion naturelle en ambiance agressive (des cycles humifification/séchage en brouillard salin). Deux parties principales constituent cette thèse. La première partie traite du développement de la corrosion, à la fois initiation et propagation, dans le béton armé en présence de fissures. La deuxième partie traite de la performance mécanique des poutres longues et courtes endommagés par la corrosion des armatures, en termes de mode de défaillance, seuil de plastification, capacité ultime résiduelle et flèche ultime à rupture. Les résultats de l'étude expérimentale confirment que la corrosion est toujours initiée dans les fissures induites par le chargement. Il convient de noter que la corrosion est liée à la présence des fissures mais pas à leur largeur. Les conditions d'exposition sont également un paramètre important influençant le développement de la corrosion. Ainsi, une surface tendue correspondant à la surface supérieure est la pire condition d'exposition, parce que le développement de la corrosion est accéléré par les effets de l’accumulation des chlorures ainsi que l’effet gravitaire favorisant leur pénétration. En outre, les dommages induits par le “top-cast effect” qui sont formés à l'interface acier-béton sous les barres horizontales par le ressuage et le tassement du béton frais, sont favorables à la fois à la l’initiation et à la propagation de la corrosion. Le phénomène d’auto-cicatrisation des fissures survient lorsque les échantillons fissurés sont conservés à 100% d'humidité relative en raison de la formation d'ettringite dans la zone intérieure et de la calcite dans la zone extérieure du plan de fissuration. L’auto-cicatrisation réduit le débit d'air à travers les fissures et réduit considérablement le risque de corrosion. Les performances en flexion de poutres longues ont été testées. La corrosion des armatures modifie le mode de défaillance des poutres en béton armé. La diminution de la charge de plastification et de la capacité ultime a été corrélée à la perte de section transversale des barres tendues. Les résultats expérimentaux indiquent qu’une réduction de 1% de la section transversale correspond à une réduction de 1% de la charge de plastification et de la capacité ultime. En ce qui concerne les performances mécaniques des poutres courtes, les résultats montrent qu’une corrosion sévère par piqûres sur les armatures tendues change le mode de défaillance par cisaillement à celui en flexion. Le mode de rupture des poutres courtes corrodées dépend non seulement du ratio entre la portée et la hauteur utile, mais également du degré de corrosion des cadres d’effort tranchant.

Este trabalho avalia as vantagens do uso das fibras curtas de polpa de Eucalipto tanto como alternativa às fibras longas de polpa de Pinus, como também para fibras sintéticas, tradicionalmente usadas no reforço de materiais cimentícios. Os efeitos da morfologia (comprimento, largura, fibrilação, conteúdo de finos, número de fibras por grama, etc.) das fibras celulósicas no processamento, no desempenho mecânico e físico e na microestrutura dos compósitos de fibrocimento foram avaliados. Os compósitos foram avaliados antes e após ciclos de envelhecimento acelerado. Fibras de Eucalipto apresentaram melhor dispersão na matriz cimentícia e forneceram maior densidade de fibras em massa ou em volume, em relação às fibras de Pinus. As fibras curtas permitem um reforço efetivo da matriz frágil, diminuindo a propagação das fissuras, o que contribuiu para o melhor desempenho mecânico dos compósitos após envelhecimento. Estes resultados promissores mostram o potencial apresentado pelas fibras curtas de Eucalipto para reduzir custos, em vista da substituição parcial das fibras sintéticas em processos de cura ao ar, e durante o refino da polpa celulósica. O efeito do branqueamento das fibras também foi avaliado, e mostrou que as fibras branqueadas de Eucalipto são mais reativas para se ligarem por pontes de hidrogênio com a matriz cimentícia. Fibras branqueadas melhoraram a interface entre fibra e matriz, embora apresentassem mais sinais de mineralização (re-precipitação de produtos de hidratação dentro das fibras) do que as fibras não-branqueadas. O refino da polpa celulósica foi utilizado para modificar as propriedades morfológicas das fibras de Eucalipto e Pinus. Os resultados mostraram que são necessárias maiores intensidade de refino na polpa de Pinus para obter valores de retenção de sólidos do cimento similares àqueles obtidos com fibras não-refinadas de Eucalipto. O refino aumentou a capacidade das fibras de capturar as partículas minerais, melhorando a aderência das fibras com a matriz. Esta melhor interface entre fibra e matriz melhorou as propriedades mecânicas dos compósitos aos 28 dias de cura, mas os tornou mais frágeis após os ciclos de envelhecimento acelerado. A modificação química da superfície das fibras foi realizada com o objetivo de melhorar as ligações entre fibra e matriz e diminuir a mineralização da fibra dentro dos compósitos. Esta modificação química foi realizada com Metacriloxipropiltri-metoxisilano (MPTS) e Aminopropiltri-etoxisilano (APTS) e mostrou influenciar significativamente a microestrutura dos compósitos. Ciclos de envelhecimento acelerado diminuíram o módulo de ruptura (MOR) e a tenacidade (TE) dos compósitos com fibras não-modificadas e modificadas; entretanto, compósitos reforçados com fibras modificadas com MPTS apresentaram fibras sem produtos de hidratação do cimento em seu interior, enquanto que fibras modificadas com APTS apresentaram acelerada mineralização. Fibras mineralizadas tornam os compósitos mais frágeis após os ciclos de envelhecimento acelerado. Estas observações são, portanto, muito úteis para o entendimento da contribuição de diferentes condições das fibras (composição química, resistência mecânica, morfologia e propriedades de superfície) para os mecanismos de aderência entre fibras e matriz cimentícia, de mineralização das fibras e de degradação dos compósitos de fibrocimento. / This work evaluates the advantages of using hardwood short fibre pulp (Eucalyptus) as alternative to softwood long fibre pulp (Pinus) and synthetic fibres, traditionally used in reinforcement of cement based materials. The effects of cellulose fibre morphology (e.g., length, width, fibrillation, content of fines and number of fibres per gram) on the processing, on the mechanical and physical performance and on the microstructure of fibre-cement composites were evaluated. Composites were evaluated before and after accelerated ageing cycles. Eucalyptus pulp fibres were better dispersed in the cement matrix and provided higher number of fibres per unitary weight or volume, in relation to Pinus long fibre pulp. The short reinforcing elements lead to an effective crack bridging of the fragile matrix, which contributes to the improvement of the mechanical performance of the composite after ageing. These promising results show the potential of eucalyptus short fibres for reducing costs by both the partial replacement of expensive synthetic fibres in air curing process and the energy savings during pulp refining. The effects of pulp bleaching were also evaluated, and showed that Eucalyptus bleached fibres are more reactive to bond with the cement matrix by hydrogen bonds. Bleached fibres improved the fibre-matrix interface, although they presented more signals of fibre mineralization. Mechanical refining was used to change the morphological properties of Eucalyptus and Pinus pulps. Results show that high levels of refining were necessary for Pinus pulp to obtain cement retention values similar to those obtained by unrefined Eucalyptus pulp. The mechanical refining increased the capacity of the fibres to capture the mineral particles improving the adherence of the fibres with the matrix. This improved fibre-matrix interface led to better mechanical properties at 28 days of cure, but turned brittle the composites after 200 ageing cycles. The chemical surface modification of cellulose pulp fibres was done in order to improve fibre-matrix bonding and to decrease fibre mineralization into the composite. Surface modification of the cellulose pulps was performed with Methacryloxypropyltri-methoxysilane (MPTS) and Aminopropyltri-ethoxysilane (APTS) and showed significant influence on the microstructure of the composites. Accelerated ageing cycles decreased modulus of rupture (MOR) and toughness (TE) of the composites with unmodified and modified fibres, however composites reinforced with MPTS-modified fibres presented fibres free from cement hydration products, while APTS-modified fibres presented accelerated mineralization. Higher mineralization of the fibres led to higher embrittlement of the composite after accelerated ageing cycles. These observations are therefore very useful for understanding the contribution of the different fibre conditions (chemical composition, mechanical strength, morphology and surface properties) to the mechanisms of fibre-matrix adherence, fibre mineralization and degradation of fibre-cement composites.

O emprego de compósitos na construção civil, como os de matriz cimentícia e pasta reforçada com fibras, tem se disseminado consideravelmente nos últimos anos. Uma grande variedade de fibras sintéticas, como o polipropileno, tem sido utilizada com sucesso para reforçar compósitos cimentícios. No entanto, o interesse mundial na utilização de produtos com menor impacto ambiental estimula a busca por materiais para substituir fibras sintéticas. As fibras vegetais, biodegradáveis, pode ser ótima alternativa devido à abundância, ao baixo custo, ao menor consumo de energia para sua produção e às propriedades mecânicas apropriadas. Fibra de curauá, planta nativa do estado do Amazonas, com plantações em escala comercial, é usada na fabricação de cordas, cestos ou como reforço em matrizes orgânicas. Suas propriedades mecânicas são semelhantes às de polipropileno. A tecnologia de extrusão é viável nas indústrias de fibrocimento, pois produz compósitos com matriz de alta densidade e ótimo empacotamento, baixa permeabilidade e boa adesão fibra matriz. No entanto, o processo de extrusão bem-sucedido de produtos cimentícios depende principalmente das propriedades reológicas do cimento fresco reforçado com fibras. As fibras vegetais podem promover o sequestro de água e interferir fortemente no escoamento, na coesão e no fluxo de pasta de cimento fresco. A incorporação de fibras vegetais influencia os materiais à base de cimento no estado fresco e afeta propriedades no estado endurecido. Neste contexto, o objetivo da pesquisa é avaliar a influência das fibras de curauá e de polipropileno em propriedades reológicas e em propriedades mecânicas da pasta de cimento fresco. Foram preparadas formulações sem fibras, como referência, e com 1 e 2% de reforço em massa, fibras com comprimento de 6 e 10 mm. Utilizaram-se duas técnicas reológicas: Squeeze flow e reômetro extrusor para analisar o fluxo de pastas cimentícias. Por meio de dados experimentais, como força/deslocamento, e de análise numérica da pressão do reômetro extrusor, foram determinados: tensão inicial de cisalhamento (σ0), limite de cisalhamento (τ0), tensão de escoamento (α) e tensão de cisalhamento (β). As propriedades mecânicas foram determinadas em máquina de ensaio MTS. Módulo de ruptura (MOR), tenacidade à fratura (TFT) e energia de fratura (EF) foram calculados. Os resultados reológicos indicam que a pasta cimentícia reforçada com fibras de curauá apresentou maior força, menor deslocamento e aumento da pressão de extrusão em fibras de curauá em relação às pastas cimentícias reforçadas com fibras de polipropileno. O comprimento das fibras influenciou mais o fluxo da mistura do que o teor de fibra. Compósitos cimentícios reforçados com fibra de polipropileno apresentaram melhores resultados mecânicos de MOR, TFT e EF em relação aos compósitos reforçados com curauá. Após os 200 ciclos de envelhecimento, os resultados mecânicos dos compósitos reforçados com as fibras de curauá diminuíram devido a mineralização das fibras. Os resultados de nanoindentação, como dureza e módulo elástico, aumentaram após os 200 ciclos. As metodologias aplicadas para avaliar o comportamento reológico e mecânico do fibrocimento durante a extrusão facilitará a futura transferência dessa tecnologia ao setor produtivo, com produtos potencialmente de melhor qualidade. / The use of composites in construction, as matrix and paste cement reinforced with fibers, has spread considerably in recent years. A wide variety of synthetic fibers such as polypropylene have been successfully used to reinforce cementitious composites. However, worldwide interest in the use of products with lower environmental impact stimulates the search for materials to replace synthetic fiber. Vegetable fiber, biodegradable, can be a great alternative because of the abundance, low cost, the lowest energy consumption for its production, appropriate mechanical properties. Curauá fiber, native plant from Amazon, with crops on a commercial scale, is used in the manufacture of ropes, baskets or as reinforcement in organic matrix. Its mechanical properties are similar to those of polypropylene. Extrusion technology is feasible in the fibercement industry, because it produces composites with high density matrix and great packaging, low permeability and good adhesion fiber matrix. However, successful extrusion process of cementitious products mainly depends on the rheological properties of fresh cement reinforced with fibers. The vegetable fibers can promote water kidnapping and strongly interfere in the flow, cohesion and fresh cement slurry flow. The incorporation of vegetable fibers influences the based cementitious materials in the fresh state and affects properties in the hardened state. In this context, the objective of the research is to evaluate the influence of curauá and polypropylene fiber in rheological and mechanical properties of fresh cement paste. Formulations without fiber, used as reference, 1 and 2% content by weight of reinforcement, fibers with a length of 6 to 10 mm were prepared. Two rheological techniques were used: Squeeze flow and extruder rheometer to analyze the flow of cement pastes. Through experimental data, as strength/displacement and numerical analysis of the pressure extruder rheometer were determined: yield stress corresponding to zero velocity (σ0), initial shear stress (τ0), effect of the velocity on yield stress (α) and effect of velocity in the shear stress (β). The mechanical properties were determined in MTS testing machine. Modulus of rupture (MOR), fracture toughness (TFT) and fracture energy (EF) were calculated. The rheological results indicate that the cement paste reinforced with curauá fiber showed higher strength, smaller displacement and increased extrusion pressure with curauá fibers compared to cementitious paste reinforced with polypropylene fibers. The length of the fibers influence the flow of the mixture more than the fiber content. Composites reinforced with polypropylene fibers presented higher values of MOR, TFT and EF compared to composites reinforced with curauá fiber. After 200 ageing cycles, the mechanical results of composites reinforced with curauá fibers decreased due to mineralization of the fibers. The nanoindentation results, as hardness and elastic modulus, increased after 200 cycles. The methodologies used to assess the rheological and mechanical behavior of fibercement during extrusion facilitate future transfer of this technology to the productive sector, with potentially higher quality products.

O emprego de compósitos na construção civil, como os de matriz cimentícia e pasta reforçada com fibras, tem se disseminado consideravelmente nos últimos anos. Uma grande variedade de fibras sintéticas, como o polipropileno, tem sido utilizada com sucesso para reforçar compósitos cimentícios. No entanto, o interesse mundial na utilização de produtos com menor impacto ambiental estimula a busca por materiais para substituir fibras sintéticas. As fibras vegetais, biodegradáveis, pode ser ótima alternativa devido à abundância, ao baixo custo, ao menor consumo de energia para sua produção e às propriedades mecânicas apropriadas. Fibra de curauá, planta nativa do estado do Amazonas, com plantações em escala comercial, é usada na fabricação de cordas, cestos ou como reforço em matrizes orgânicas. Suas propriedades mecânicas são semelhantes às de polipropileno. A tecnologia de extrusão é viável nas indústrias de fibrocimento, pois produz compósitos com matriz de alta densidade e ótimo empacotamento, baixa permeabilidade e boa adesão fibra matriz. No entanto, o processo de extrusão bem-sucedido de produtos cimentícios depende principalmente das propriedades reológicas do cimento fresco reforçado com fibras. As fibras vegetais podem promover o sequestro de água e interferir fortemente no escoamento, na coesão e no fluxo de pasta de cimento fresco. A incorporação de fibras vegetais influencia os materiais à base de cimento no estado fresco e afeta propriedades no estado endurecido. Neste contexto, o objetivo da pesquisa é avaliar a influência das fibras de curauá e de polipropileno em propriedades reológicas e em propriedades mecânicas da pasta de cimento fresco. Foram preparadas formulações sem fibras, como referência, e com 1 e 2% de reforço em massa, fibras com comprimento de 6 e 10 mm. Utilizaram-se duas técnicas reológicas: Squeeze flow e reômetro extrusor para analisar o fluxo de pastas cimentícias. Por meio de dados experimentais, como força/deslocamento, e de análise numérica da pressão do reômetro extrusor, foram determinados: tensão inicial de cisalhamento (σ0), limite de cisalhamento (τ0), tensão de escoamento (α) e tensão de cisalhamento (β). As propriedades mecânicas foram determinadas em máquina de ensaio MTS. Módulo de ruptura (MOR), tenacidade à fratura (TFT) e energia de fratura (EF) foram calculados. Os resultados reológicos indicam que a pasta cimentícia reforçada com fibras de curauá apresentou maior força, menor deslocamento e aumento da pressão de extrusão em fibras de curauá em relação às pastas cimentícias reforçadas com fibras de polipropileno. O comprimento das fibras influenciou mais o fluxo da mistura do que o teor de fibra. Compósitos cimentícios reforçados com fibra de polipropileno apresentaram melhores resultados mecânicos de MOR, TFT e EF em relação aos compósitos reforçados com curauá. Após os 200 ciclos de envelhecimento, os resultados mecânicos dos compósitos reforçados com as fibras de curauá diminuíram devido a mineralização das fibras. Os resultados de nanoindentação, como dureza e módulo elástico, aumentaram após os 200 ciclos. As metodologias aplicadas para avaliar o comportamento reológico e mecânico do fibrocimento durante a extrusão facilitará a futura transferência dessa tecnologia ao setor produtivo, com produtos potencialmente de melhor qualidade. / The use of composites in construction, as matrix and paste cement reinforced with fibers, has spread considerably in recent years. A wide variety of synthetic fibers such as polypropylene have been successfully used to reinforce cementitious composites. However, worldwide interest in the use of products with lower environmental impact stimulates the search for materials to replace synthetic fiber. Vegetable fiber, biodegradable, can be a great alternative because of the abundance, low cost, the lowest energy consumption for its production, appropriate mechanical properties. Curauá fiber, native plant from Amazon, with crops on a commercial scale, is used in the manufacture of ropes, baskets or as reinforcement in organic matrix. Its mechanical properties are similar to those of polypropylene. Extrusion technology is feasible in the fibercement industry, because it produces composites with high density matrix and great packaging, low permeability and good adhesion fiber matrix. However, successful extrusion process of cementitious products mainly depends on the rheological properties of fresh cement reinforced with fibers. The vegetable fibers can promote water kidnapping and strongly interfere in the flow, cohesion and fresh cement slurry flow. The incorporation of vegetable fibers influences the based cementitious materials in the fresh state and affects properties in the hardened state. In this context, the objective of the research is to evaluate the influence of curauá and polypropylene fiber in rheological and mechanical properties of fresh cement paste. Formulations without fiber, used as reference, 1 and 2% content by weight of reinforcement, fibers with a length of 6 to 10 mm were prepared. Two rheological techniques were used: Squeeze flow and extruder rheometer to analyze the flow of cement pastes. Through experimental data, as strength/displacement and numerical analysis of the pressure extruder rheometer were determined: yield stress corresponding to zero velocity (σ0), initial shear stress (τ0), effect of the velocity on yield stress (α) and effect of velocity in the shear stress (β). The mechanical properties were determined in MTS testing machine. Modulus of rupture (MOR), fracture toughness (TFT) and fracture energy (EF) were calculated. The rheological results indicate that the cement paste reinforced with curauá fiber showed higher strength, smaller displacement and increased extrusion pressure with curauá fibers compared to cementitious paste reinforced with polypropylene fibers. The length of the fibers influence the flow of the mixture more than the fiber content. Composites reinforced with polypropylene fibers presented higher values of MOR, TFT and EF compared to composites reinforced with curauá fiber. After 200 ageing cycles, the mechanical results of composites reinforced with curauá fibers decreased due to mineralization of the fibers. The nanoindentation results, as hardness and elastic modulus, increased after 200 cycles. The methodologies used to assess the rheological and mechanical behavior of fibercement during extrusion facilitate future transfer of this technology to the productive sector, with potentially higher quality products.

Este trabalho avalia as vantagens do uso das fibras curtas de polpa de Eucalipto tanto como alternativa às fibras longas de polpa de Pinus, como também para fibras sintéticas, tradicionalmente usadas no reforço de materiais cimentícios. Os efeitos da morfologia (comprimento, largura, fibrilação, conteúdo de finos, número de fibras por grama, etc.) das fibras celulósicas no processamento, no desempenho mecânico e físico e na microestrutura dos compósitos de fibrocimento foram avaliados. Os compósitos foram avaliados antes e após ciclos de envelhecimento acelerado. Fibras de Eucalipto apresentaram melhor dispersão na matriz cimentícia e forneceram maior densidade de fibras em massa ou em volume, em relação às fibras de Pinus. As fibras curtas permitem um reforço efetivo da matriz frágil, diminuindo a propagação das fissuras, o que contribuiu para o melhor desempenho mecânico dos compósitos após envelhecimento. Estes resultados promissores mostram o potencial apresentado pelas fibras curtas de Eucalipto para reduzir custos, em vista da substituição parcial das fibras sintéticas em processos de cura ao ar, e durante o refino da polpa celulósica. O efeito do branqueamento das fibras também foi avaliado, e mostrou que as fibras branqueadas de Eucalipto são mais reativas para se ligarem por pontes de hidrogênio com a matriz cimentícia. Fibras branqueadas melhoraram a interface entre fibra e matriz, embora apresentassem mais sinais de mineralização (re-precipitação de produtos de hidratação dentro das fibras) do que as fibras não-branqueadas. O refino da polpa celulósica foi utilizado para modificar as propriedades morfológicas das fibras de Eucalipto e Pinus. Os resultados mostraram que são necessárias maiores intensidade de refino na polpa de Pinus para obter valores de retenção de sólidos do cimento similares àqueles obtidos com fibras não-refinadas de Eucalipto. O refino aumentou a capacidade das fibras de capturar as partículas minerais, melhorando a aderência das fibras com a matriz. Esta melhor interface entre fibra e matriz melhorou as propriedades mecânicas dos compósitos aos 28 dias de cura, mas os tornou mais frágeis após os ciclos de envelhecimento acelerado. A modificação química da superfície das fibras foi realizada com o objetivo de melhorar as ligações entre fibra e matriz e diminuir a mineralização da fibra dentro dos compósitos. Esta modificação química foi realizada com Metacriloxipropiltri-metoxisilano (MPTS) e Aminopropiltri-etoxisilano (APTS) e mostrou influenciar significativamente a microestrutura dos compósitos. Ciclos de envelhecimento acelerado diminuíram o módulo de ruptura (MOR) e a tenacidade (TE) dos compósitos com fibras não-modificadas e modificadas; entretanto, compósitos reforçados com fibras modificadas com MPTS apresentaram fibras sem produtos de hidratação do cimento em seu interior, enquanto que fibras modificadas com APTS apresentaram acelerada mineralização. Fibras mineralizadas tornam os compósitos mais frágeis após os ciclos de envelhecimento acelerado. Estas observações são, portanto, muito úteis para o entendimento da contribuição de diferentes condições das fibras (composição química, resistência mecânica, morfologia e propriedades de superfície) para os mecanismos de aderência entre fibras e matriz cimentícia, de mineralização das fibras e de degradação dos compósitos de fibrocimento. / This work evaluates the advantages of using hardwood short fibre pulp (Eucalyptus) as alternative to softwood long fibre pulp (Pinus) and synthetic fibres, traditionally used in reinforcement of cement based materials. The effects of cellulose fibre morphology (e.g., length, width, fibrillation, content of fines and number of fibres per gram) on the processing, on the mechanical and physical performance and on the microstructure of fibre-cement composites were evaluated. Composites were evaluated before and after accelerated ageing cycles. Eucalyptus pulp fibres were better dispersed in the cement matrix and provided higher number of fibres per unitary weight or volume, in relation to Pinus long fibre pulp. The short reinforcing elements lead to an effective crack bridging of the fragile matrix, which contributes to the improvement of the mechanical performance of the composite after ageing. These promising results show the potential of eucalyptus short fibres for reducing costs by both the partial replacement of expensive synthetic fibres in air curing process and the energy savings during pulp refining. The effects of pulp bleaching were also evaluated, and showed that Eucalyptus bleached fibres are more reactive to bond with the cement matrix by hydrogen bonds. Bleached fibres improved the fibre-matrix interface, although they presented more signals of fibre mineralization. Mechanical refining was used to change the morphological properties of Eucalyptus and Pinus pulps. Results show that high levels of refining were necessary for Pinus pulp to obtain cement retention values similar to those obtained by unrefined Eucalyptus pulp. The mechanical refining increased the capacity of the fibres to capture the mineral particles improving the adherence of the fibres with the matrix. This improved fibre-matrix interface led to better mechanical properties at 28 days of cure, but turned brittle the composites after 200 ageing cycles. The chemical surface modification of cellulose pulp fibres was done in order to improve fibre-matrix bonding and to decrease fibre mineralization into the composite. Surface modification of the cellulose pulps was performed with Methacryloxypropyltri-methoxysilane (MPTS) and Aminopropyltri-ethoxysilane (APTS) and showed significant influence on the microstructure of the composites. Accelerated ageing cycles decreased modulus of rupture (MOR) and toughness (TE) of the composites with unmodified and modified fibres, however composites reinforced with MPTS-modified fibres presented fibres free from cement hydration products, while APTS-modified fibres presented accelerated mineralization. Higher mineralization of the fibres led to higher embrittlement of the composite after accelerated ageing cycles. These observations are therefore very useful for understanding the contribution of the different fibre conditions (chemical composition, mechanical strength, morphology and surface properties) to the mechanisms of fibre-matrix adherence, fibre mineralization and degradation of fibre-cement composites.

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Une réutilisation des sédiments issus du dragage en tant que matière première dans la fabrication d’un béton directement sur le site du dragage est une voie de valorisation économique et écologique. La présente étude a pour but de valoriser la partie fine des sédiments qui ne trouve pas de solutions de valorisation efficaces. En effet la structure en feuillet de l’argile la rend sensible aux conditions hydriques et lui confère une importante capacité de rétention des polluants. Afin d’optimiser les volumes à valoriser, le béton est envisagé en substitution totale des granulats par la fraction fine des sédiments. Les résultats apportés par la littérature tendent à privilégier une application en remblai tels que le remplissage entre deux rideaux de palplanches, un remblaiement géotechnique ou de carrières. Un procédé d’incorporation d’une mousse à base de protéine animale lors de la fabrication du béton est utilisé dans le cadre de cette étude pour alléger le matériau (densité comprise entre 1,1 et 1,3). Ce type de matériau fait donc partie de la catégorie des bétons légers de mousse plus communément appelée LWFC (LightWeight Foamed Concrete). Dans cette étude le matériau est désigné par le sigle BAMS (Béton Allégé par l’incorporation d’une Mousse et à base de Sédiments). L’étude a été réalisée sur un sol modèle constitué de 80% de bentonite et de 20% de sable correcteur de diamètre 0,125mm. La méthode de formulation est basée sur la limite de liquidité du sol afin de prendre en compte l’absorption de l’eau. La caractérisation du BAMS se scinde en trois parties ; La première partie correspond à la caractérisation à l’état frais du BAMS. Elle met en exergue une optimisation de l’abaissement de la densité à partir d’une certaine quantité d’eau apportée par rapport à la limite de liquidité du sol. L’allégement du matériau par l’incorporation d’une mousse modifie les propriétés du matériau à l’état frais ; elle améliore la fluidité et retarde la prise du ciment. La deuxième partie correspond à la caractérisation mécanique du BAMS ; l’eau apportée pour optimiser l’allégement du matériau impacte la résistance mécanique qui est jugée acceptable à partir de 0,5MPa. Celle-ci peut être améliorée en augmentant la quantité de ciment qui doit cependant rester faible pour rentabiliser la voie de valorisation. Il y a donc un compromis inévitable entre résistance mécanique et densité. Les combinaisons (densité ; résistance mécanique) possibles et les paramètres de formulations permettant de les atteindre ont été étudiés. Des essais non-destructifs sont effectués afin de contrôler la résistance mécanique in situ. L‘étude du retrait linéaire indique une variation dimensionnelle importante du BAMS de l’ordre du cm/m qui peut être divisé par 100 avec une cure humide. La troisième partie correspond à la durabilité par l’étude des propriétés de transfert du BAMS dont les résultats mettent en avant une accessibilité partielle du réseau poreux crée par la mousse incorporée.Le relargage des polluants dans les sédiments est évalué par un essai de lixiviation effectué sur un sol modèle pollué artificiellement (cas non-immergeable). Cet essai permet de valider l’efficacité de leur inertage par le traitement au ciment et l’utilisation du matériau sans impact environnemental selon le critère PH14. / A re-use of dredged sediments as raw material in the process of making of concrete directly onthe site of the dredging is an interesting valorization as regards economy and environment.The present study aims at valuing the thin particles of sediments because they create aproblem in the valorization of dredged sediments. Indeed, the layer structure of the claymakes it prone to react to humidity conditions and confers it an important capacity to retainpolluting agents. To optimize the valued volumes, a total substitution of aggregates in theconcrete by the thin particles of sediments is envisaged. The results from the literature tend tofavor an application in embankment such as the filling between two sheet pile walls, a geotechnical embankment, a quarry embankment. An incorporation of an air-foam made ofanimal protein during the making of the concrete is used to reduce the density of the material(density between 1.1 and 1.3). This material is classified in the category of lightweight foam concrete called by the English abbreviation LWFC (LightWeight Foamed Concrete). In thisstudy the material is named BAMS acronym for “Béton Allégé par l’incorporation d’uneMousse et à base de Sédiments”. The study was realized with a model soil composed of 80%of bentonite clay and 20% of calibrated sand (diameter 0.125mm). The mix design method isbased on the liquidity limit of the soil considering its swelling. The characterization of theBAMS is split into three parts. The first part corresponds to the characterization of the freshstate of the BAMS. It highlights the optimization of the reduction of the density from aquantity of added water with regard to the liquidity limit of the soil. The incorporation of airfoam modifies the characteristics of the fresh state of the material. It improves the workability and delays the setting of cement. The second part corresponds to the mechanical characterization of the BAMS. The added water which optimizes the reduction of the density impacts the mechanical resistance which has to be over 0.5MPa. There is thus an inevitablecompromise between mechanical resistance and density. The possible combinations and themix design to get them have been studied. Non-destructive tests are done to simply check the mechanical performances on construction site. The study of the linear shrinkage highlights an important variation of the dimension of the BAMS. This can be limited by a wet cure. The third part corresponds to the durability by the study of the transfer properties of the BAMS.The results highlight a limited accessibility of the porous network. The release of polluting agents in sediments is estimated by a lixiviation test realized on BAMS made with a model soilartificially polluted (non immersible case). From the results we can conclude on the efficiency of the inerting of polluting agents by the cement treatment and therefore the use of the material is allowed without having an impact on environment (PH14).

Les routes sont le moyen de transport le plus utilisé dans le monde et le développement d'un pays est souvent mesuré en termes de kilométrage total des routes revêtues. Les chaussées sont essentielles à notre réseau social et l’enrobé bitumineux est le matériau le plus utilisé pour leur fabrication. À l'heure actuelle, le réseau routier européen n’est plus en forte croissance et nécessite surtout un entretien. Dans un contexte de développement durable de plus en plus exigeant,la route pourrait donc représenter sa propre source d’approvisionnement en tirant parti du recyclage. Elle doit aussi limiter les quantités d’énergies et de ressources naturelles nécessaires à sa propre maintenance.La combinaison des techniques d’enrobés tièdes (WMA) et de taux de recyclage élevés d’agrégats d’enrobés (RAP) apparaît comme une solution permettant d’économiser à la fois l’énergie et les ressources naturelles. Mais sa durabilité doit être éprouvée. Un programme expérimental a donc été mis en place pour montrer l'évolution des performances de ces enrobés bitumineux avec le temps, mettant en évidence la notion de vieillissement essentiellement lié à la fraction bitumineuse. A l'échelle du bitume, l'évaluation à long terme est effectuée notamment en appliquant la δ-méthode et en comparant avec les mesures de masses moléculaires par GPC à la fois sur des échantillons modèles à teneur en asphaltènes controllée et sur des échantillons de laboratoire. A l’échelle de l’enrobé bitumineux, une étude comparative a été réalisée entre un enrobé à chaud traditionnel et des WMAs incluant 0% ou 50% de RAP soumis à une procédure de vieillissement en laboratoire. Les performances à long terme des mélanges sont comparées au moyen d’essais de module complexe et de fatigue.Les résultats montrent une relation entre l’évolution de la structure des bitumes par vieillissement et les performances mécaniques. Le vieillissement à court terme au moment de la fabrication est beaucoup moins marqué pour les procédés tièdes. Après vieillissement à long terme, les tendances générales sont similaires pour tous les procédés. / Roads are the most widely used mode of transportation in the world, and a country’s development is often measured in terms of its total paved roads mile age. Pavements are an essential part of our social network and asphalt concrete is the main material used for manufacturing them. Currently, the European road network is not much growing anymore and mostly needs only maintenance. In a context of increasing demand of performance and durability of asphalt mixtures, a sustainable, durable and economical conceptionis required. Indeed it could be oriented towards a self sufficient road providing its own raw materials through recycling while limiting the use of energy and other natural resources for its maintenance.The combination of warm mix asphalts (WMA) technologies and high rates of reclaimed asphalt pavements (RAP)appears as a solution to achieve both energy and natural resources savings. But it is still ambiguous in terms of durability. Therefore, an experimental program is set up to show the evolution of the performances of such asphalt concretes with time, highlighting the notion of ageing mostly related to the bituminous fraction. At the bitumen scale, the long term assessment is carried out in particular by applying the δ-method compare with GPC measurements both on model samples with controlled asphaltene content and laboratory aged ones. At the asphalt mixture scale, a comparison studyis carried out between a reference HMA and WMAs with 0%- 50% of RAP submitted to a laboratory ageing procedure. The long term performances of the mixtures are compared by means of complex modulus and fatigue testing. Results show a relation between the evolution of the structure of the bitumen with ageing and the mechanical performances. Short term ageing is less important for warm processes. After ageing, the overall tendencies are similar for all processes.