This thesis is focused on the study of the influence of crystalline ingredients XYPEX, on the rheology of fresh concrete and durability of hardened concrete. It examines the influence of crystalline additives on the rheology of cement pastes with different types of cement with different temperatures, increasing water tightness and gas tightness and compressive strength. Also assesses pore structure with different bridging cracks.

The subject of this thesis are the rheological properties of cement paste with the addition of amorphous silicon dioxide. The basic rheological parameters are that describe the behavior of cement pastes in the fresh state. The work also included rheological tests including measurement principle and method of evaluation. Effect of mineral admixtures with high content of amorphous SiO2 is summarized the available scientific articles. In the experimental part, the effects of impurities with a high content of amorphous SiO2 on the rheological properties of fresh cement paste. It was tested by substitution of up to 10 % by weight of cement in the cement pastes mineral admixtures of different chemical composition, particle size and pozzolanic activity. Flow measurement was measured yield value, viscosity, and flow index. The stability of cement pastes was investigated oscillatory measurements. To complement the behavior pastes in the fresh state was determined by calorimetry. Test results were compared with those determined by reference samples and compared the effect of various ingredients.

Dans ce travail de thèse, nous proposons dans une première partie l’usage de fibres de la plante marine Posidonia-Oceanica pour la fabrication de matériaux d’isolation thermique de bâtiments. Les caractérisations thermiques effectuées ont permis de mettre en évidence l’effet de la densité des fibres et de traitements chimiques. Il apparaît que ce type de fibres possède une conductivité équivalente à celle d’autres isolants courants et une capacité thermique massique plus élevée. La conductivité thermique en fonction de la masse volumique est comprise entre 0.04 et 0.07 W.m-1.K-1. La capacité thermique massique atteint environ 2500J.kg-1.K-1. Il apparaît également que l’influence du traitement chimique sur les propriétés thermiques n’est pas significative. Les résultats obtenus font de ces fibres un bon candidat pour une utilisation comme isolant thermique dans le domaine du bâtiment. Dans une seconde partie, ces fibres sont utilisées pour le renforcement d’une pâte de ciment. Une gamme de composites a été formulée pour des fractions volumiques en fibres allant de 0 à 20%. Une étude des propriétés hydriques de ces composites a été menée et complétée par des analyses par spectroscopie infrarouge à transformée de Fourier (FTIR) et des mesures des propriétés thermophysiques par la méthode du Hot-Disk durant le cycle de séchage. D’autre part, la quantification de la sensibilité de ces matériaux à l’humidité relative a été réalisée par la mesure de la variation de la teneur en eau dans les échantillons dans des environnements à humidité contrôlée. Ces mesures permettent de déterminer le coefficient de diffusion de l’eau. Celui-ci augmente légèrement avec l’augmentation du taux de fibres dans le composite. Du point de vue thermique, l’ajout de fibres améliore les propriétés isolantes des matériaux. En effet, une diminution de 22% sur la valeur de la conductivité thermique est notée avec l’introduction de 20% de fibres, par comparaison à l’échantillon de ciment témoin. L’influence sur la diffusivité thermique et sur la capacité thermique massique n’est pas significative. Du point de vue mécanique, la résistance à la traction par flexion et la compression augmentent légèrement jusqu’à 5 à 10% en volume de fibres puis diminuent. En revanche, une augmentation notable des valeurs de ténacité a été observée avec l’augmentation du dosage en fibres. Une augmentation de 65% est observée avec l’ajout de 20% de fibres. En s'appuyant sur les observations expérimentales, une modélisation analytique simplifiée a été réalisée. Celle-ci permet d'obtenir des modèles de prédiction des valeurs de la conductivité thermique, de la résistance à la traction par flexion, de la résistance à la compression et de la ténacité en fonction de la quantité de fibres dans le matériau / In this work, we have firstly studied the use of fibers extracted from the marine plant Posidonia-Oceanica as loose-fill thermal insulation material for buildings. Measurements were conducted and allowed the determination of the effect of fibers density and chemical treatments on thermal properties. Thermal conductivities were lying between 0.04 and 0.07 W.m-1.K-1, whereas the heat capacity is about 2500 J.kg-1.K-1. Thus, it was found that fibers thermal conductivity is close to the one of commonly used thermal insulation materials and that their heat capacity is significantly higher. It was also found that the influence of chemical treatment on the thermal properties is not significant. Measurement results showed that these fibers could be a promising ecological loose-fill insulation material in the construction field. Secondly, fibers were used as reinforcement for cement paste. A set of composite samples were formulated by varying fibers volume fractions from 0 to 20%. Their hygroscopic, thermal and mechanical properties were evaluated. Composites were analyzed by Fourier transform infrared spectroscopy (FTIR) and their thermophysical properties were measured with a Hot Disk thermal constants analyzer during the drying cycle. Sensitivity of these materials to relative humidity was examined by measuring the water content variation in controlled humidity environments. These measurements allowed the quantification of the water diffusion coefficient. This coefficient increased slightly with the increase of fibers content in composite samples. Concerning thermal properties, the addition of Posidonia-Oceanica fibers improved the material insulating properties. In fact, a decrease of about 22% on thermal conductivity values was found with the introduction of 20% of fibers compared to the unfilled cement paste. For Posidonia-Oceanica fibers volume fractions considered in this study (0 to 20 Vol.%), the effect of the presence of fibers on thermal diffusivity and on heat capacity is not significant, regarding the measurement uncertainties. Concerning mechanical properties, flexural and compressive strengths increased for about fiber volume fractions in the range of 5 to 10%. Moreover, a noticeable increase of toughness was observed with increasing fibers amount: for instance, an increase of about 65% was observed with the introduction of 20% of fibers in the composite. Based on the experimental observations, simplified analytical models were developed to predict thermal conductivity, flexural strength, compressive strength and toughness as a function of fibers volume fraction in the material

Cette étude concerne l’ajout de billes de verre de dimension variant de 1 à 50 m dans des matrices cimentaires. Les travaux ont comme objectif dans un premier temps la caractérisation des propriétés physiques et rhéologiques à l’état frais des suspensions cimentaires à deux échelles : la pâte de ciment et le mortier. Puis dans un deuxième temps l’étude de l’influence des microbilles de verre sur les propriétés physiques, mécaniques et durabilité du mortier durci. Des séries d’expériences normalisées ont été faites pour caractériser l’influence des billes de verre sur les indicateurs à l’état frais : la consistance et la prise des pâtes de ciment. Les propriétés mécaniques et de durabilité sont quantifiées au jeune âge (de 3 à 28 jours) et à long terme (de 28 jours à 112 jours). L’étude sur les gels d’hydratation et sur la microstructure du mortier durci a été faite à l’aide de la technique de la microscopie électronique à balayage. Des méthodes de caractérisation complémentaires pour examiner la propagation d’onde, la ségrégation et l’étalement ont également été employées. Les résultats obtenus par l’ensemble des essais évaluent le rôle des microbilles de verre sur les comportements des suspensions de pâtes de ciment et du mortier à l’état frais, et du mortier à l’état durci. Ceci met en évidence l’intérêt rhéologique, mécanique et l’effet sur la durabilité des microbilles de verre dans un matériau cimentaire. / The aim of this work is the valorisation of recycled waste materials in cement paste and mortar in order to reuse these resources for replacing natural aggregates in concrete. Our study concerns the use of a microsphere glass powder (MGP) with a particle size from 1 to 50 m into the cement matrix. This experimental work first focuses on the effect of the MGP on the workability properties of fresh cement paste and fresh mortar and on the physical, mechanical and durability properties of mortar. Many standard tests have been conducted for the characterisation of the behavior of the fresh cement paste i.e the consistency and the setting of fresh cement paste. The durability properties at early age (from 3 to 28 days) and at long time (from 28 days to 112 days) have been also quantified. We employed the scanning electron microscopy for the mortar microstructure analysis. Some supplementary tests like the ultrasonic wave propagation, the segregation and the flow properties on the vibrated table have been also used. The primary results have proved the effect of the MGP on the behaviour of the fresh cement paste, fresh mortar and mortar. The presence of MGP showed interesting modifications on the rheology, mechanical and durability properties of the cement system.

Submitted by Silvana Teresinha Dornelles Studzinski (sstudzinski) on 2016-12-22T12:03:13Z No. of bitstreams: 1 Josué Claudio Metz_.pdf: 3580473 bytes, checksum: 4bb7f81d4d0a95ef4e39a7d4dffb0599 (MD5) / Made available in DSpace on 2016-12-22T12:03:13Z (GMT). No. of bitstreams: 1 Josué Claudio Metz_.pdf: 3580473 bytes, checksum: 4bb7f81d4d0a95ef4e39a7d4dffb0599 (MD5) Previous issue date: 2016-09-19 / Nenhuma / A concepção de desenvolvimento sustentável tem resultado no aumento de pressões ambientais para a melhoria da eficiência na utilização de recursos, e para a redução das emissões e da geração de resíduos. No processo de fabricação de aço, nas siderúrgicas com fornos elétricos a arco (FEA), ocorre a geração do resíduo sólido denominado pó de aciaria elétrica (PAE). O PAE é constituído por diferentes óxidos metálicos. Contém os elementos químicos cromo (Cr), chumbo (Pb) e cádmio (Cd) e, por isso, é classificado como resíduo classe I – Perigoso pela NBR 10004. Gerado em grandes quantidades diariamente em todo o país, o PAE ainda tem como principal destinação final o aterro industrial. A indústria de papel e celulose, outra atividade de destaque na indústria nacional, gera uma grande quantidade de resíduos em diferentes etapas do processo, entre os quais está o resíduo do forno de cal (RFC), cuja geração está associada a interrupções no funcionamento do forno de cal. A indústria da construção civil, devido a quantidade de matérias-primas consumida e variedade de materiais empregados – cimento, concreto, agregados, cerâmica, entre outros – apresenta-se como alternativa para a reciclagem de resíduos gerados em outros setores da economia. A incorporação do PAE no cimento e concreto produz retardo no tempo de pega em razão da presença de zinco (Zn) no resíduo. Estudos sugerem que em quantidades próximas a 1%, a incorporação de PAE não afeta de forma significativa as propriedades do cimento. O objetivo deste trabalho foi avaliar a influência do uso combinado de PAE e RFC no processo de endurecimento e evolução da hidratação de pastas de cimento. Para tanto, foi realizada a caracterização dos resíduos através dos ensaios de distribuição granulométrica, perda ao fogo, massa específica, área superficial específica, análise química elementar, difração de raios X com refinamento por Rietveld e microscopia eletrônica de varredura. A influência dos resíduos nas pastas de cimento foi avaliada através do ensaio de tempo de pega de acordo com a NBR NM 65 (ABNT, 2003b) e evolução da temperatura semi-adiabática das pastas em estado fresco, além de DRX, com refinamento por Rietveld, e microscopia eletrônica de varredura nas pastas de cimento com diferentes teores de substituição de resíduos (REF, 1%, 2%, 3%, 5% e 10%) em diferentes idades (1, 4 e 7 dias). Os resultados de tempo de pega e evolução da temperatura semi-adiabática indicaram a influência do PAE na hidratação das pastas de cimento. Nas pastas de cimento com substituição de 1% de PAE combinado ou não com RFC, não foram verificados retardos significativos no tempo de pega, demonstrando o potencial do uso de PAE e do RFC na produção de artefatos de cimento. / The sustainable development conception has resulted in increased environmental pressures to improve the efficient use of resources and reduction of emissions and waste generation. In the steelmaking process through electric arc furnaces (EAF), dust generation occurs which is called electric arc furnace dust (EAFD). EAFD is composed by different metal oxides. Some common elements those constitute this dust is chromium, lead and cadmium, and therefore, waste is classified as class I – hazardous by NBR 10004. EAFD has been generated in large quantities every day across the country and it still has mainly landfilled. The pulp and paper industry, another important activity in the domestic industry, generates a lot of waste in different stages of the process, among which is the lime kiln waste (LKW), whose generation is associated with disruptions in the lime oven. Due to expressive amount of raw materials consumed in civil construction industry and also the variety of products available - cement, concrete, aggregates, ceramics, among others - this seems to be an alternative for waste recycling generated in other sectors. The incorporation of EAFD in the cement and concrete produces delayed setting time due to the presence of zinc (Zn) in the waste. Studies suggest that in amounts up to 1%, EAFD incorporation does not affect significantly cement properties. The aim of this work was to evaluate the influence of the combined use of EAFD and LKW in the process of hardening and evolution of the cement pastes hydration. Therefore, were evaluated the characterization of the waste performed through the grain size distribution, loss on ignition, specific gravity, specific surface area, elemental chemical analysis, pH, X ray powder diffraction with refinement by Rietveld and scanning electron microscopy.. The influence of the waste on the cement pastes was evaluated through the setting time tests in accordance with the NBR NM 65 (ABNT, 2003b) and evolution of semi-adiabatic temperature in fresh conditions, XRD with refinement by Rietveld, and SEM in cement pastes with different levels of waste substitution (REF, 1%, 2%, 3%, 5% e 10%) at different ages (1, 4 and 7 days). The setting time results and evolution of semi-adiabatic temperature indicated an increase in the setting time with the increase of the EAFD in cement pastes. In cement pastes with replacement of 1% EAFD combined or not with LKW, significant delays were not verified in the setting time, demonstrating the potential use of EAFD in the production of cement artifacts.

Cette étude a pour but de documenter la relation qui existe entre les propriétés de transfert d’un matériau (répartition en taille de pores, porosité totale accessible à l’eau, saturation en eau), et son coefficient de diffusion. Pour cela, des matériaux ayant une porosité quasi-monomodale sont utilisés : verres Vycor® et géopolymères ; ainsi que des matériaux ayant une porosité complexe : pâtes de ciment CEM V. L’utilisation des verres Vycor® et des géopolymère permet de quantifier la diffusion gazeuse, en fonction de la saturation en eau, de matériaux ayant des pores de même dimension, ou du moins, de même ordre de grandeur. L’utilisation des pâtes de ciment permet quant à elle, de vérifier s’il est possible de décomposer le coefficient de diffusion d’un matériau dont la porosité est complexe, en un assemblage de coefficients de diffusion de matériaux dont la porosité est quasi-monomodale. Pour cela, on s’attachera à particulièrement à étudier l’impact de l’agencement du réseau poreux sur le coefficient de diffusion.Les travaux se décomposent en trois parties :• Etude des caractéristiques géométriques du réseau poreux des matériaux étudiés. Il sera utilisé la porosimétrie par intrusion de mercure, la porosimétrie à eau, des essais de sorption / désorption d’azote, et des essais de désorption d’eau.• Mesure expérimentale du coefficient de diffusion des matériaux, en fonction de leur humidité relative de stockage et de leur saturation en eau.• Modélisation du coefficient de diffusion des matériaux utilisés, et étude de l’impact de l’agencement de leur réseau poreux (tortuosité, connexion des pores entre eux) / This work documents the relationship that exists between the transfer properties of a material (pore size distribution, total porosity accessible to water, water saturation degree), and its diffusion coefficient. For this sake, materials having a quasi mono modal porosity are used: Vycor® glasses and geopolymers. We also use materials having a complex porosity: CEM V cement pastes. The use of Vycor® glasses and geopolymers allows quantifying the gas diffusion coefficient through materials having known pores size, as a function of their water saturation degree. The use of cement pastes allows checking if it is possible to decompose the diffusion coefficient of a complex porosity material, in an assembling of diffusion coefficients of quasi mono modal porosity materials. For this sake, the impact of pore network arrangement on the diffusion coefficient is studied in great details. This study is divided into three parts:• Measurement of the geometric characteristics of materials porous network by means of the mercury intrusion porosimetry, water porosimetry, isotherms of nitrogen sorption / desorption, and water desorption tests.• Measurement of the materials diffusion coefficient, as a function of their relative humidity storage, and their water saturation degree.• Modeling the diffusion coefficient of the materials, and study the impact of the pore network (tortuosity, pores connection)

Constitués de plusieurs composants (granulats naturels et pâte de ciment adhérente), les GBR ne sont à l’heure actuelle pas utilisés largement dans la formulation de nouveaux bétons. Les propriétés médiocres des GBR compliquent considérablement la détermination de la quantité d’eau efficace dans le béton frais. Tout d’abord, une étude bibliographique va mettre en évidence la grande dispersion des résultats des essais de caractérisation des GBR et des propriétés des bétons recyclés à l’état frais et durci. Ensuite, une étude vise à analyser l’hétérogénéité des GBR et des granulats de béton concassé (GBC) par rapport à différents paramètres : aux impuretés granulaires, à la densité et à la teneur en pâte de ciment, au malaxage du béton parent, et au niveau de la capacité d’absorption d’eau des GBC en fonction de leur état de pré-humidification. Enfin, une dernière partie est destinée à améliorer la maîtrise de l’eau efficace réelle dans la fabrication du béton recyclé. La cinétique d’absorption des GBC dans une pâte de ciment est tout d’abord étudiée. Ensuite, l’évolution de l’eau efficace durant le malaxage de bétons à base de GBC est investiguée au moyen d’une méthode originale basée sur le suivi des courbes de puissance du malaxeur. Finalement, l’effet d’un malaxage sous vide relatif sur les propriétés des bétons à base de granulats naturels et des bétons à base de GBC est étudié. / Composed of several components (natural aggregates and adherent cement paste), RCA are not widely recommended in new concrete formulations. Their poor properties considerably complicate the determination of the effective water in fresh concrete. In a first part, a bibliographic study will highlight the wide dispersion of the results of characterization tests of RCA and the properties of fresh and hardened recycled concrete. In a second part, the heterogeneity of RCA and crushed concrete aggregates (CCA) is studied according to different parameters: granular impurities, density, cement paste content, mixing of parent concrete, and water absorption capacity according to their pre-humidification. The third part consists of three experimental studies that intend to improve effective water control in the manufacture of recycled concrete. The absorption kinetics of CCA in a cement paste is first studied. Then, the evolution of effective water in fresh concrete during mixing is studied using an original method based on the power evolution of the mixer. Finally, the effect of vacuum mixing on the properties of ordinary and recycled concretes is investigated.

The use of recycled concrete aggregates (RCA) has gained increased attention in the past few decades as an alternative to decrease the carbon footprint of concrete construction. Yet, most of the research performed so far demonstrates that RCA concrete displays inferior performance in the fresh and hardened states when compared to conventional concrete (CC). The latter is believed due to the fact that very often the different microstructure of RCA is not accounted for while the mix-proportioning of RCA concrete. Recently, a number of mix-design procedures accounting for RCA microstructure have been proposed. Amongst them, the Equivalent Volume (EV) method seems to be quite promising. The EV method may proportion RCA concrete made of coarse (CRCA) or fine (FRCA) RCA and is based on a companion CC. Previous research has demonstrated that the fresh and hardened properties of EV mix-designed CRCA are suitable for structural applications. Yet, very few research, analysis and quantification have been conducted on the fresh behaviour of EV mix- proportioned FRCA concrete. This work presents a comprehensive study on the rheological behaviour of EV mix-designed CRCA and FRCA concrete presenting distinct features (i.e. inner qualities, mineralogy, fabrication process, etc.) through the use of a planetary rheometer (IBB). Results show that the EV is capable of proportioning low embodied energy CRCA and FRCA concrete with shear thinning profiles. The latter suggests that these mixtures are suitable for applications under high torque regimes such as vibrated or pumped concrete.

<p>Hydrated portland cement provides the solid adhesive matrix necessary to bind aggregate (sand and gravel) into concrete. The hydration reaction requires water, however the products of the reaction limit further diffusion of water to unreacted cement. Superabsorbent polymer (SAP) hydrogel particles absorb mixing water, then subsequently desorb when the relative humidity drops, serving as internal water reservoirs within the cement matrix to shorten diffusion distances and promote the hydration reaction in a process called internal curing. Internally cured cementitious mixtures exhibit an increased degree of hydration and reduced shrinkage and cracking, which can increase concrete service life. Increased service life can, in turn, reduce overall demand for portland cement production, thereby lowering CO2 emissions.</p> <p>This dissertation addresses practical implementation questions key to the translation of SAP hydrogel internal curing technology to from the benchtop to the field in transportation applications, including: (1) What effects do mix design adjustments made to increase mixture flow when using SAP have on cementitious mixture properties? and (2) What effect do cementitious binder characteristics have on SAP performance?</p> <p>The addition of SAP to a cementitious mixture changes the mixture’s flow behavior. Flow behavior is an important aspect of concrete workability and sufficient flow is necessary to place well consolidated and molded samples. Often, additional water is added to mixtures using SAP to account for the absorbed water, however cementitious mixture workability is often tuned using high range water reducing admixtures (e.g., polycarboxylate ester-based dispersants). Fresh and hardened properties of mortars were characterized with respect to flow modification method (using the mortar flow table test; compressive strength at 3, 7, and 28 days; flexural strength at 7 and 28 days; and microstructural characterization of 28-day mortars). At typical doses, it was found that the addition of extra water lowers the resulting compressive and flexural strength, while high range water reducing admixtures administered at doses to achieve sufficient mortar flow did not compromise compressive or flexural strength.</p> <p>The SAPs used in cement are generally poly(acrylamide-acrylic acid) hydrogels and are not chemically inert in high ionic-load environments, such as cement mixtures. The behavior of an industrial SAP formulation with characterized across five different cement binder compositions with respect the cement hydration reaction (using isothermal calorimetry, thermogravimetric analysis of hydration product fraction, and scanning electron microscopy (SEM)/energy dispersive x-ray spectroscopy (EDS) microstructural analysis), the absorption behavior of the SAP, and the fresh and hardened properties of SAP-cement composites (mortar flow and compressive and flexural strength). The change in properties induced by the addition of SAP was similar across ASTM Type I cements from three manufacturing sources, suggesting that SAP internal curing can be implemented predictably over time and geography. Excitingly, in analysis of cement systems meeting different ASTM standards (Type III and Type I with 30% replacement by mass with ground blast furnace slag), synergistic and mitigating reaction behaviors were observed, respectively, in Type III and slag cement, suggesting that further study of SAP with these cement systems could be of particular interest.</p>