La quantité et la distribution de l'eau interstitielle dans l'espace poral des milieux cimentaires sont des marqueurs fondamentaux de la durabilité des structures de Génie Civil en béton. La connaissance de ces grandeurs est également importante pour l'interprétation de certains essais non destructifs mis en œuvre pour évaluer les performances mécaniques des ouvrages ou détecter certains défauts. L'évaluation de la teneur en eau par méthode non-destructive requiert l'utilisation d'une grandeur intermédiaire telle que la permittivité diélectrique. La relation entre cette propriété électromagnétique et la teneur en eau dépend alors de la composition et donc de la formulation du béton. En électromagnétisme, les lois d'homogénéisation permettent de lier la permittivité effective d'un matériau hétérogène avec la permittivité intrinsèque et la fraction volumique de chaque hétérogénéité présente. Afin de pallier le temps important requis pour l'établissement d'une courbe de calibration expérimentale propre à chaque formulation, l'étude présentée propose la mise en place d'une démarche d'homogénéisation de la permittivité pour lier quantité d'eau présente dans un béton et permittivité macroscopique du matériau. Les travaux présentés rapportent la fabrication, la modélisation et l'utilisation de sondes coaxiales ouvertes pour la mesure de la permittivité complexe de matériaux solides et liquides. Le concept d'estimation de la teneur en eau par utilisation de lois d'homogénéisation est validé pour le cas d'un sable partiellement saturé en eau. Au vu des résultats prometteurs obtenus par modélisation analytique, des schémas d'homogénéisation sont combinés lors d'un processus de remontée d'échelle depuis celle des hydrates jusqu'à celle des granulats, en tenant compte de la morphologie de la microstructure. Les propriétés intrinsèques des principaux constituants d'un béton (granulats, hydrates, ciment anhydre) sont alors mesurées par sonde coaxiale et utilisées en données d'entrée du modèle construit. Une bonne cohérence est observée entre parties réelles de la permittivité simulées et mesurées, pour des échantillons de pâtes de ciment, mortiers et bétons. A la différence des lois expérimentales et empiriques, le modèle construit se caractérise par un temps de calcul quasi-instantané et peut être adapté d'une formulation de béton à une autre en fonction du type de ciment utilisé, de la nature et de la quantité de granulats ou encore de la porosité accessible à l'eau du matériau. / Prediction of delayed behavior in concrete can be significantly improved by monitoring the amount and spatial distribution of water within a concrete structure over time. Water content of cement-based materials can also be required to interpret non-destructive tests such as ultrasonic and radar measurements. Electromagnetic properties of heterogeneous and porous materials, such as dielectric permittivity, are closely related to water content. Measurement of these properties is thus a common non-destructive technique used to assess the moisture content, but a calibration curve is required to link the measured permittivity to the saturation degree. This curve can be determined experimentally, or from empirical models. However, the first approach is tedious and time consuming, while the second one is not adapted to concrete. Hence, this contribution proposes an alternative route, relying on electromagnetic homogenization schemes, to connect the macroscopic permittivity of cement-based materials with the water content of the structure. Therefore, different open-ended coaxial probes were designed, modelled and tested in order to perform complex permittivity measurements of both solids and liquids. The homogenization approach is first validated on unsaturated sand. Then, the permittivity of concrete components (aggregates, hydrates, interstitial liquid, anhydrous cement) was assessed by means of coaxial probe measurements. Finally, a specific combination of analytical homogenization laws taking into account the microstructure's morphology of the material is built. Results show that there is a good correlation between the model and measurements acquired on different cement pastes, mortars and concretes, at different saturation degrees. The model is characterized by a quasi-instantaneous calculation time and can be adapted to different concretes depending on cement type, nature and quantity aggregates or porosity.

Le contrôle non destructif in-situ de durabilité des matériaux cimentaires est essentiel à la prédiction et la prévention des défauts de fonctionnement des constructions. Alors que les dégradations, et donc la perte de durabilité, des matériaux cimentaires sont déclenchées et contrôlées par les caractéristiques et les évolutions de leur microporosité, il n'existe pas à notre connaissance de méthode non destructive d'instrumentation in-situ de la microporosité elle-même. Nous proposons un concept innovant d'évaluation de la durabilité des matériaux cimentaires fondé sur l'instrumentation in-situ de leur microstructure. La méthode repose sur l'investigation ultrasonore haute fréquence de micropores individuels au moyen de micro-transducteurs ultrasoniques capacitifs (μ-cMUT) immergés en grand nombre dans le matériau. Le dispositif proposé pour répondre aux multiples contraintes applicatives et technologiques est un μ-cMUT dont la plaque vibrante est constituée d'une couche mince de nanotubes de carbone monoparoi densément alignés. Nous avons traité la question de la pertinence de ce principe d'instrumentation en modélisant par un problème élasto-acoustique microfluidique l'interaction entre la plaque vibrante d'un μ-cMUT et le fluide, air ou eau, contenu dans un pore de taille micrométrique. La spécificité du modèle réside dans la prise en compte du comportement dissipatif du fluide. La résolution de ce problème couplé a nécessité le développement d'une méthode numérique ad-hoc. Nous avons constaté numériquement que la dissipation cause une diminution des fréquences de résonance. La couche limite a une épaisseur importante par rapport à la taille du domaine. Les amplitudes de vibration des plaques sont particulièrement sensibles au contenu des pores et à la géométrie des pores remplis d'eau. Nous en avons déduit que les μ-cMUT proposés pourraient être pertinents dans les matériaux cimentaires pour le suivi de l'hydratation, pour la détection des dégradations et le suivi de leur évolution. Pour étudier la faisabilité d'un μ-cMUT à nanotubes opérationnel à haute fréquence dans l'air et l'eau, nous avons tout d'abord réalisé par diélectrophorèse des dépôts denses et minces de nanotubes bien alignés. Un des dépôts est monocouche, ce qui constitue une performance remarquable pour un dépôt par diélectrophorèse. Nous avons ensuite suspendu les nanotubes, obtenant ainsi des membranes rigides et longues. L'épaisseur de ces membranes suspendues est particulièrement faible et leur facteur de forme particulièrement élevé par rapport à l'état de l'art des cMUT. Nous avons enfin montré par vibrométrie laser que les membranes vibrent à basse fréquence avec des amplitudes atteignant 5 nm pic-à-pic. Il s'agit à notre connaissance de la première mise en évidence de vibrations de nanotubes de carbone monoparoi par vibrométrie laser. Ces résultats démontrent une brique de base essentielle de l'étude complète de faisabilité du dispositif imaginé. Ils indiquent aussi la faisabilité à court terme de microdétecteurs d'air pour le suivi de la microporosité gazeuse des matériaux cimentaires. En regroupant ainsi une étude numérique de pertinence et une étude technologique de faisabilité, la thèse constitue une contribution significative à la mise au point d'une nouvelle méthode de suivi de durabilité de matériaux cimentaires fondé sur l'immersion au coeur du matériau d'un grand nombre de microcapteurs intégrant des nanotechnologies / In-situ non-destructive testing of durability in cementitious materials is essential to the early prediction and prevention of structural failures. Whereas degradations in cementitious materials, and henceforth durability loss, are brought about and controlled by the characteristics and evolutions of microporosity, there isn't to our knowledge any method for the in-situ non-destructive testing of microporosity itself. To evaluate in-situ the durability of cementitious materials, we put forward an innovative concept based on in-situ instrumentation of their microstructure. Individual micropores are to be probed by high-frequency ultrasonic waves generated and detected by capacitive ultrasonic microtransducers (μ-cMUT) embedded in large number within the material. The vibrating plate of the μ-cMUT devices is to be made of a thin layer of densely aligned single-walled carbon nanotubes, in order for the devices to satisfy the applicative and technological requirements. Relevance of this instrumentation method has been studied : we have used an elasto-acoustical model to describe the interaction between the vibrating plate of a μ-cMUT device and the fluid (water or air) filling a pore of micrometric size. The specificity of this model lies in the integration of fluid viscosity. It has required us to develop ad-hoc solving techniques. We have found out numerically that in this problem dissipation leads to a decrease in resonance frequency compared to non-visquous acoustics. The boundary layer is large compared to the domain size. The vibration amplitudes of the plate are very sensitive to pore content and to water-filled pore geometry. We have deduced from these results that the μ-cMUT devices we envision may be relevant to study hydration and to monitor degradations in cementitious materials. Feasibility of a high-frequency, nanotubes-based μ-cMUT device operating in water or air has also be evaluated : using first a dielectrophoretic deposition technique, we have made thin, dense membranes of well-aligned nanotubes. One of our deposition reaches mono-layer thickness, which is remarkable for dielectrophoretic depositions. We have suspended the nanotubes, thus obtaining long and rigid membranes. They are very thin and have a high form factor compared to state-of-the-art cMUT devices. Finally, we have used laser vibrometry to observe membrane vibrations. Membrane vibration amplitudes reach 5 nm at low frequency. As far as we know, it is the first time vibrations of carbon nanotubes have been successfully observed with laser vibrometry. These results prove that we have overcome one of the most significant technological bottle-neck of the whole feasibility study. Moreover, they indicate short-term feasibility of air microdetectors that could be valuably employed to monitor gaseous microporosity in cementitious materials. By associating a numerical study on relevance and a technological study on feasibility, this work contributes significantly to the development of a new durability monitoring method for cementitious materials. Central to this method is the use of a large number of embedded microsensors integrating nanotechnologies

Le béton projeté est une méthode de mise en place consistant en la projection pneumatique de béton sur une surface à grande vitesse. Dans le cas de la méthode par voie sèche, le mélange granulats-ciment est introduit sec en machine, l'eau est ajoutée à la fin du transfert. Cette technique, très employée, est néanmoins génératrice de pertes importantes par rebond, pouvant s'élever jusqu'à 40% de la masse projetée. L'enjeu de la réduction des pertes est à la fois économique et environnemental. Les facteurs influents sur le rebond sont liés aux techniques de projection et à la formulation. Ce travail de thèse a pour objectif l'optimisation de la formulation du béton afin de réduire les pertes par rebond, mais également d'améliorer la durabilité. L'étude porte en particulier sur l'influence sur le rebond : du squelette granulaire, de la teneur en eau et de l'emploi d'additifs et/ou d'additions de substitution. Une approche modélisation du phénomène de rebond est également abordée. / Sprayed concrete is a concrete pneumatically projected onto a surface at high velocity. Dry-mix shotcrete is a process in which dry constituents are introduced into the machine and conveyed through a hose to the nozzle, where the water is added. This process is used in various civil engineering or construction projects; unfortunately, it can lead to high losses of concrete due to rebound (up to 40% of the total mass of material). Such losses induce overconsumption of material, which is damaging for the cost of the work and for the environment. Rebound depends on technicals parameters and mix design. The present work focuses on rebound reduction and also on durability enhancement by modification of the mix design. The influence of aggregate size distribution, water content and supplementary cimentitious material is studied. An analytical approach of rebound phenomenon is also implemented.

L’objectif de cette thèse est d’approfondir le développement d’une plateforme de modélisation, qui décrit le transport multi-espèces et multi-phasiques à travers les matériaux cimentaires. Les structures en béton armé peuvent se dégrader en raison de la corrosion des armatures en acier, induite par les chlorures et/ou la carbonatation. La plateforme de modélisation traite principalement de la période d’initiation de cette corrosion par la prédiction du transport des agents délétères à travers le béton d’enrobage. Ces phénomènes sont dépendants des propriétés relatives à l’humidité du matériau et requièrent l’étude des mouvements de l’eau liquide et de la phase gazeuse dans le matériau. La première partie de cette thèse se concentre sur la pénétration des chlorures à travers des bétons saturés. La pénétration des chlorures se limite à un processus couplé de diffusion et de fixation des ions sur la matrice cimentaire. Dans ce cadre, de nombreux modèles ont été développés et de nombreuses données expérimentales sont accessibles. Un benchmark de ces modèles est réalisé, avec pour objectif d’identifier les plus robustes et les plus fiables. Cette étude contribue également à choisir les isothermes de fixation des chlorures les plus pertinentes. Une analyse fiabiliste des modèles sélectionnés précédemment est menée. Un cadre de calcul de la durée de vie fiabiliste du béton armé immergée dans une solution saline est proposé. Une analyse de sensibilité est également réalisée afin de déterminer les données d’entrée du modèle les plus influentes. Les résultats mettent en avant le rôle crucial joué par l’enrobage, la teneur critique en chlorures et le coefficient effectif des chlorures. L’importance de la non-linéarité des isothermes est également soulignée, alors que cette propriété est encore mal maîtrisée. De nombreux modèles de prédiction des transferts d’humidité ont été développés. La compréhension des phénomènes physiques en jeu reste insuffisante pour les matériaux cimentaires. Une analyse de sensibilité fiabiliste du modèle multi-phasiques et de l’équation de Richards est réalisée, en considérant un essai de séchage. Les résultats soulignent l’importance de l’isotherme de désorption de vapeur d’eau et de la perméabilité à l’eau liquide, qui s’écrit comme une fonction de la saturation. Par la suite, les travaux se sont focalisés sur la détermination de cette perméabilité. Celle-ci a été réalisée par analyse inverse des profils de perte de masse lors d’un séchage et des profils de saturation durant une imbibition. Les valeurs déterminées sont comparées aux mesures de perméabilité aux gaz, aux mesures directes et indirectes (notamment Katz-Thompson) de perméabilité à l’eau liquide, reportées dans la littérature. Parmi les pistes d’évolution des modèles de carbonatation, une description plus complète du transport des espèces en phase gazeuse est à proposer. Le dernier chapitre traite de ce point, en considérant une diffusion ternaire du mélange gazeux avec toutefois une description simplifiée des réactions chimiques de carbonatation. Une étude théorique met en évidence les conséquences de la nouvelle description des transferts : les profils de pression de gaz (dépression) et de CO2 sont modifiés, ce qui peut impacter l’avancement de la carbonatation. Par la suite, une calibration a été réalisée afin de mettre en cohérence les prédictions numériques avec des expériences de carbonatation accélérée. Une analyse de sensibilité fiabiliste a été conduite en considérant un essai de carbonatation pour des fractions de CO2 extérieures allant de 0,04 % à 50 %, avec une humidité relative extérieure contrôlée. Les résultats ont montré l’importance de la porosité totale, de la teneur initiale en C-S-H (fraction de CO2 extérieure élevée) et des conditions hydriques extérieures (fraction de CO2 atmosphérique). Enfin, la carbonatation atmosphérique avec la prise en compte de cycles d’humidification-séchage a été simulée pour deux bétons / The purpose of this research is to go deeper in the development of a modelling platform, which describes multiphase and multi-species transport within cementitious materials. Reinforced concrete (RC) structures can be deteriorated as a result of chloride-induced and/or carbonation-induced corrosion of the steel rebars. The modelling platform deals with the initiation period of this corrosion by predicting the transport of the deleterious agents through the concrete cover. This phenomenon is dependent on the moisture properties of the material and requires the study of the movement of liquid-water and gas-phase transport in the material. The first step of this thesis focuses on chloride ingress within fully water-saturated concretes. The chloride ingress is limited to a coupled diffusion-binding process. Within this framework, several models have been developed and numerous experimental data are available. A benchmark of these models is performed in order to identify the most reliable engineering models. This also contributes to choose the most relevant chloride binding isotherms. A probabilistic analysis of selected models among the benchmark is carried out. A general framework is proposed to calculate a reliability service life for reinforced concrete structures in the case of immersion in seawater. A sensitivity analysis is also performed in order to define the most influencing input data. Results point out the crucial role of the concrete cover, the critical chloride content and, to a lesser extent, the effective chloride diffusion coefficient. The importance of the non linearity of isotherms is also highlighted whereas this property is still not well-known. Several moisture transport models have been developed. The understanding of the numerous physical phenomena involved is still insufficient for cementitious materials. A reliability sensitivity analysis of the multiphasic model and of the model based on Richards equation is performed, considering the drying of concretes. Results point out the importance of defining a relevant water vapour desorption isotherm and, to a lesser extent, the liquid-water permeability, as a function of saturation. Thereafter, this research focuses on the determination of this permeability. This is performed by inverse analysis considering two different experimental tests: the mass loss monitoring during a drying and the monitoring of saturation profiles during an imbibition. The determined values are compared to measurements of gas permeability and to measurements with direct and indirect methods (in particular, Katz-Thompson methods) of liquid water permeability, assessed in the literature. Among the outlooks of sophistication of predictive models dedicated to the carbonation, a more comprehensive description of the transport of species in the gaseous phase has to be proposed. The last chapter of the manuscript deals with this issue, by considering a ternary diffusion process of the gaseous mix along with a simplified description of the chemical carbonation reactions. A theoretical study is carried out in order to highlight the changes induced by the new description of transfers: the profiles of gas pressure (depression) and the profiles of CO2 pressure are modified, which can impact the progress of the carbonation front. Thereafter, a calibration of the model is performed in order to bring the numerical predictions into line with the experimental results of accelerated carbonation tests. A reliability sensitivity analysis is performed considering a carbonation test for external fractions of CO2 ranging from 0.04 % to 50 %, with constant external relative humidity. Results point out the significance of the bulk porosity, of the initial content of C-S-H (high external fractions of CO2) and the external moisture conditions (atmospheric external fractions of CO2). Finally, atmospheric carbonation involving wetting–drying cycles is simulated for two concretes

Ce travail de thèse concerne la modélisation du béton et des ouvrages en béton soumis à des sollicitations allant du quasi statique à la dynamique rapide, tout en prenant en compte de la présence d'eau libre dans les pores du béton. L'objectif est la mise au point d'un outil prévisionnel de simulation capable de décrire le comportement du béton et des structures en béton, en tenant compte des effets du taux de saturation. Le choix des Éléments Discrets pour cette modélisation est justifié par les phénomènes discontinus qui apparaissent dans le béton, tel que la fissuration, la fragmentation ou l'écaillage. Les Éléments Discrets permettent de reproduire de manière fiable et efficace le comportement discontinu local ainsi que la réponse globale de la structure.La première partie de ce travail concerne la simulation d'essais quasi-statiques sous sollicitations uniaxiales et triaxiales fortement confinées, avec la prise en compte du phénomène de compaction. Les effets de l'eau libre contenue dans les porosités sont pris en compte par l'introduction d'une dépendance entre le taux de saturation en eau et la déformation inélastique. La procédure d’identification des paramètres du modèle est présentée. Enfin, le modèle est validé en reproduisant le comportement quasi-statique du béton par différents essais. La deuxième partie de ce travail est consacrée au comportement dynamique du béton. L'objectif est d'étendre la validation du modèle en simulant des essais d'impacts. Les effets de vitesse sont pris en comptes et des simulations d'impact sur des dalles en béton de différentes épaisseurs sont effectuées. Les résultats obtenus sont en bonne concordance avec les résultats expérimentaux. / This thesis concerns the modeling of concrete and concrete structures subjected to stresses ranging from quasi-static to dynamic loading, taking into account the presence of free water in pores. The objective is the development of a predictive simulation tool capable of describing the behavior of concrete and concrete structures, taking into account the effects of saturation ratio. The choice of discrete elements for modeling is justified by the discontinuous phenomena that appear in the concrete, such as cracking, fragmentation, spalling and scabbing. Discrete Elements can reproduce reliably and efficiently the local discontinuous behavior and the overall response of the structure.The first part of this work concerns the simulation of quasi-static tests under uniaxial and highly confined triaxial loadings, taking into account the compaction phenomenon. The effects of the free water contained in the pores are taken into account by introducing a dependency between the water saturation level and the inelastic deformation. The identification process of the model parameters is presented. Finally, the model is validated by reproducing the quasi-static behavior of concrete in different tests.The second part of this work concerns the dynamic behavior of concrete. The aim is to extend the validation of the model by simulating impact tests on concrete slabs of different thickness. The dynamic effects are taken into account and impact simulations on concrete slabs of different thickness are made. The results are in good agreement with experimental results.

Submitted by Irene Nascimento (irene.kessia@ufpe.br) on 2016-06-27T17:06:44Z No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) Dissertação - Dannúbia Ribeiro Pires (PPGECAM_CAA).pdf: 1569346 bytes, checksum: de291d5949502da801c8fef00fcf2b43 (MD5) / Made available in DSpace on 2016-06-27T17:06:44Z (GMT). No. of bitstreams: 2 license_rdf: 1232 bytes, checksum: 66e71c371cc565284e70f40736c94386 (MD5) Dissertação - Dannúbia Ribeiro Pires (PPGECAM_CAA).pdf: 1569346 bytes, checksum: de291d5949502da801c8fef00fcf2b43 (MD5) Previous issue date: 2016-02-15 / Facepe / A grande demanda de cinza de algaroba gerada nas lavanderias pertencentes ao APL de Pernambuco e sua constituição química prioritária de carbonato de cálcio, caracterizando seu efeito filler, impulsionaram a verificação do comportamento do sistema cimentício quando da substituição do cimento pela cinza nas argamassas de revestimento. O objetivo deste trabalho é utilizar o resíduo, atualmente descartado no ambiente, em materiais cimentícios, de modo a contribuir para o desenvolvimento sustentável, reduzindo o impacto produzido pelo armazenamento e descarte inadequado. Além disso, pretende-se contribuir para a redução da emissão de CO2 causada pelas indústrias cimenteiras e minimizar os custos dos produtos com cimento Portland. Neste trabalho, foi avaliada a influência da substituição do cimento Portland em diferentes porcentagens (0%, 5%, 10% e 20%) nas propriedades nos estados fresco e endurecido das argamassas, aplicando no traço (1-X):2:X:9 (cimento: cal: cinza: areia), em volume, comumente utilizado para emboço e argamassa de assentamento em obras da região. A cinza foi caracterizada física e quimicamente. As propriedades analisadas no estado fresco foram: reologia das argamassas (reometria de mistura, de cisalhamento e compressiva - squezze flow), densidade de massa e teor de ar incorporado e aderência inicial das argamassas no substrato; e no estado endurecido foram: resistência à tração por compressão diametral, resistência potencial de aderência à tração, módulo de elasticidade dinâmico, porosidade e permeabilidade. De acordo com os resultados obtidos nesta pesquisa, a presença da cinza favoreceu, em todas as porcentagens estudadas, a redução no teor de água de amassamento, mantendo a trabalhabilidade das argamassas. As argamassas com teores de 5% de cinza preservam as propriedades do sistema compatíveis com as propriedades da argamassa de referência. Porém, até 10% é possível a introdução deste resíduo, em substituição ao cimento, sem prejuízos aos sistemas cimentícios, proporcionando alterações mínimas em relação à argamassa de referência, sendo promissor o uso desse resíduo em materiais cimentícios. / There is a considerable production of algaroba wood ash in the laundries of the local productive arrangement on the clothing industry in the Agreste Region of Pernambuco. It is possible to apply it as filler due to its mainly chemical constitution as calcium carbonate. Based on these facts, it was evaluated the mortars behaviour when cement is partial replaced by algaroba ashes. This work objectives reuse this residue, currently discarded in the environment, in cementitious materials. In this way, it contributes to the sustainable development by reducing the impact by storage and improper disposal. Moreover, it is intended contributes to reducing CO2 emissions caused by cement industries and minimize the costs of products with Portland cement. This study investigates the influence of the gradual replacement of cement by algaroba ash (0%, 5%, 10% and 20%). It was evaluated the properties of mortars in fresh and hardened states. The mix by volume (1-X):2:X:9 (cement, lime, ash, sand) was studied, taking into account that these alternative mortars can be applied on regional building sites as rendering plaster and laying mortar. The ashes were characterized physically and chemically. It was carried out in the fresh state: rheology of mortars (mixture, compressive and shear rheometers - squeeze flow), mass density, a content of entrained air and initial adherence of the mortars to the substrate; and in the hardened state: diametrical traction, potential adherence, dynamic modulus of elasticity, porosity and permeability. The results indicate that the presence of the ashes decreases the quantity of mixing water required to keep the workability of the mortars, regardless the content of cement replacement content by algaroba ash. The mortar with 5% ash content preserving system properties compatible with the properties of the reference mortar. However, it is possible to partial substitute the cement by algaroba ash until 10% in the studied mortars, when comparing to the reference system, algaroba ashes are a promising material to incorporate in a cementitious system.

La cristallisation du sel dans les pores peut conduire à l'expansion d'une variété de milieux poreux, y compris le béton, la pierre ou les sols. Par exemple, les attaques sulfatiques de matériaux cimentaires peuvent conduire à des cristallisations du gypse ou de l’ettringite, qui peuvent causer un endommagement et limiter la durabilité des structures en béton. Une meilleure compréhension de la façon dont la cristallisation induit la déformation des matériaux cimentaires est une condition préalable à la conception de moyens efficaces pour atténuer les effets néfastes de la cristallisation du sel. Dans cette thèse, nous cherchons à comprendre comment la cristallisation conduit à l'expansion, pour les matériaux à base de ciment dans le cas spécifique de la présence d'ions sulfatiques, qui est un cas pertinent pour la compréhension des attaques sulfatiques. La principale originalité de l'étude a été de réaliser des expériences avec des matériaux granulaires compactés dans des cellules œdométriques ou isochores. Les échantillons testés ont été fabriqués par broyage de pâtes de C3S, de pâtes de ciment Portland ordinaire, ou des mélanges des phases dont ces pâtes sont constituées (par exemple, monosulfoaluminate AFm), puis de les compacter dans des éprouvettes cylindriques sur une hauteur de 2 cm. Dans les cellules, les échantillons compactés sont très perméables et peuvent être saturés avec des solutions de sulfate de sodium en moins d’1 heure. Dans une cellule œdométrique, l'échantillon est empêché de se dilater radialement, mais est autorisé à se dilater axialement: nous avons mesuré comment des injections de solutions induisent une expansion axiale. Dans une cellule isochore, l'échantillon est empêché de se dilater à la fois radialement et axialement: nous avons mesuré comment des injections de solutions provoquent le développement de contraintes axiales et radiales. Un point notable des cellules isochores que nous avons développées est que toute solution s’évacue le long de l'échantillon et peut être récupérée: ainsi, à partir des mesures des concentrations et des volumes de solutions d'entrée et de sortie, la quantité de sulfates restant dans l'échantillon au cours des expériences pourrait être déterminée. En parallèle des mesures de déformation/contrainte, nous avons effectué des caractérisations minéralogiques et microstructurales des échantillons en utilisant une variété de techniques, notamment : la fluorescence X, l’analyse thermogravimétrique, la diffraction des rayons X, la résonance magnétique nucléaire d'aluminium et la microscopie électronique à balayage avec analyse aux rayons X. Les évolutions des concentrations de sortie et de la minéralogie au cours du processus d'injection ont pu être bien prédites avec le logiciel CHESS de modélisation géochimique. Les résultats expérimentaux de la campagne, en conjonction avec les résultats des caractérisations minéralogiques et microstructurales, ont permis de révéler quels sont les principaux paramètres qui régissent l'expansion. Grâce à ce protocole original que nous avons développé, l'expansion ou le développement de contraintes a commencé immédiatement après l'injection de la solution, s’est stabilisé au bout de quelques jours à quelques semaines, et la cristallisation a eu lieu de façon homogène sur toute la hauteur de l'échantillon. En outre, nous avons montré que la cristallisation du gypse contribue à l'expansion. Dans les tests isochores, nous montrons que les deux cristallisations d'ettringite et de gypse peuvent induire des contraintes, et que l'amplitude de ces contraintes dépend linéairement du volume de ces cristaux formés. Les conclusions tirées de cette étude expérimentale permettent de mieux comprendre les processus physiques par lesquels la cristallisation induit une expansion ou des contraintes dans des solides poreux, et permettent d’orienter la modélisation des attaques sulfatiques dans les matériaux cimentaires / In-pore crystallization can lead to expansion of a variety of porous media, including concrete, stone, or soils. For instance, sulfate attacks of cement-based materials can lead to crystallizations of gypsum or ettringite, which may cause damage and limit the durability of concrete structures. A better understanding of how crystallization induces deformation of cementitious materials is a prerequisite to designing efficient ways of mitigating the detrimental effects of salt crystallization. In this thesis, we aim at understanding how crystallization leads to expansion, for cement-based materials in the specific case of the presence of sulfate ions, which is relevant for sulfate attacks. The main originality of the study was to perform experiments with granular materials compacted into oedometric or isochoric cells. The tested samples were manufactured by grinding C3S pastes, regular Portland cement pastes, or mixtures of phases of which those pastes are made (e.g., monosulfoaluminate AFm), and then compacting them within the cell into 2-cm-high cylindrical specimens. In the cells, the highly permeable compacted samples could be flushed with sodium sulfate solutions in less than 1 hour. In an oedometric cell, the sample is prevented from expanding radially, but is allowed to expand axially: we measured how injections of solutions induced an axial expansion. In an isochoric cell, the sample is prevented from expanding both radially and axially: we measured how injections of solutions induced the development of axial and radial stresses. A salient feature of the isochoric cells we developed is that all solution flushed throughout the sample could be recovered: thus, from the measurements of concentrations and volumes of input and output solutions, the amount of sulfate remaining in the sample over the experiments could be determined. In parallel to the deformation/stress measurements, we also performed the mineralogical and microstructural characterizations of the samples before and after testing by using a variety of techniques, including X-ray fluorescence, thermogravimetric analysis, X-ray diffraction, aluminum nuclear magnetic resonance and scanning electron microscopy with X-ray analysis. The evolutions of the output concentrations and of the mineralogy over the injection process could be well predicted with the geochemical modeling software CHESS. Experimental results of the campaign, in conjunction with results from mineralogical and microstructural characterizations, made it possible to reveal what the main parameters are that govern expansion. Thanks to the original protocol we developed, expansion or development of stresses started immediately after the injection of solution, stabilized after a few days to a few dozen days, and crystallization occurred homogeneously throughout the height of the sample. One interesting conclusion is that, even when ettringite crystallizes in macropores, i.e., outside of the C-S-H gel porosity, ettringite can lead to an expansion. Also, we showed that gypsum crystallization contributes to expansion. In isochoric testing, we showed that both crystallization of ettringite and of gypsum can induce stresses, and that the magnitude of those stresses is linearly related to the volume of those crystals formed. The conclusions drawn from this experimental study make it possible to better understand the physical processes through which crystallization induces expansion or stresses in porous solids, and thus to orient the modeling of sulfate attacks in cement-based materials

EU Sustainable Development Strategy planned to achieve improvement of life-quality by promoting sustainable production and consumption of raw materials. On November 2018, EU Commission presented a long-term strategy, aiming among others a climate-neutral economy by 2050. Cement production is contributing to 6-10% of the anthropogenic CO2 emissions. Thus, several strategies for total or partial replacement of Portland cement in concrete production have been developed. The use of supplementary cementitious materials (SCM) and alkali-activated materials (AAM) is considered the most efficient countermeasure to diminish CO2 emissions. The broadening of knowledge with particular attention to the sustainable goals is the primary requirement to be fulfilled when novel materials are investigated. This study aims to develop a novel clay-based binder that can be used as a sustainable alternative to produce SCM as well as AAM. Clay is a commonly occurring material, with large deposits worldwide. However, natural clay has a low reactivity and various compositions, depending, e.g. on the weathering conditions. The present research aims exactly at enhancing the reactivity of natural clays occurring in Sweden subjecting them to mechanical activation in a planetary ball mill. Ball milling (BM) is considered a clean technology able to enhance the reactivity of crystalline materials without resorting to high processing temperatures or additional chemicals. BM was able to induce amorphization in clay minerals and to transform the layered platy morphology to spherical shape particles. The efficiency of the process was strictly related to the used process parameters. Higher ball to processed powder (B/P) ratio, longer time of grinding and higher grinding speeds increased the degree of the obtained amorphization. However, an undesired extensive caking and agglomeration occurred in certain setups. The potential of activated clay as a SCM was investigated in specific case studies. The measured compressive strength results showed a direct correlation between the enhanced amorphization degree of the mechanically activated clay and the increased strength values. The pozzolanic activity was induced and enhanced after the mechanical activation of the clay. The reactivity was assessed by the strength activity index (SAI). Furthermore, preliminary tests have shown that the alkali activation of the processed clays produced solidified matrixes with considerable strength.

Concrete is essential for the construction industry with characteristic properties that make it irreplaceable in some aspects. However, due to the large volumes consumed and the energy intense cement clinker production it also has a notable climate impact. In order to reach the international and national sustainability goals it is therefore important to reduce the climate impact of concrete structures. There are many ways to influence the environmental impact of concrete and a detailed analysis is one of the actions that could push the industry and the society towards a sustainable development. The purpose of this research is to evaluate the environmental impact of concrete structures and the built environment and to highlight the possibilities to reduce that impact with choice of concrete mix and innovative design solutions. A life cycle assessment (LCA) was carried out to analyze the environmental impact of two thin façade solutions with innovative materials and to evaluate influences of different greenhouse gas reducing measures on concrete bridges. The influence of supplementary cementitious materials (SCM) in terms of climate impact and durability was also analyzed. The results indicate that SCMs have a twofold effect on the climate impact of reinforced concrete structures. Not only do they reduce the greenhouse gases through cement clinker replacement but also by an improvement of durability regarding chloride ingress. Currently, this is not considered in the regulations, which makes it difficult to foresee in LCA at early design stages. The results also show great possibilities to reduce the climate impact through different measures and design alternatives and the need for further development of products and solutions. / <p>QC 20171002</p>

Composite materials have a wide range of applications in civil and structural engineering due to their advantages in mechanical properties and higher strengths over the base materials alone. Polymer-concrete composites are particularly attractive for use in industrial and infrastructure applications from combining the higher mechanical properties of the concrete in tension and the high tensile strength and ductile properties of the polymeric materials. However, these materials tend to be more expensive that typical concrete composites. This thesis explores the mechanical properties of two different polymer-concrete composites and their effectiveness in civil and structural applications: polymer concrete for rapid repair and 3D printed plastic-concrete composite members for energy absorption. The North Atlantic Treaty Organization (NATO) requires that emergency repair of military runways should be completed within 4 hours. In coordination with Luna Innovations Incorporated, a polymer concrete was developed by Luna for use as a rapid repair material for military runways to meet this requirement through its rapid heat curing. Its mechanical properties including its compressive and flexural strength, bond strength in various orientations, workability, modulus of elasticity, and coefficient of thermal expansion were tested and compared against another rapid repair material. The Tri-Service Pavements Working Group Manual recommendations for rigid repair materials were used as the requirements in determining whether the polymer concrete was an adequate rapid repair material. The polymer concrete formulation that was down-selected for further testing met these requirements for all tests except for the coefficient of thermal expansion. This was due to the resin itself having a high volumetric expansion when exposed to greater temperatures. As the polymer concrete is still under development, future tests are to be performed to determine the impact of the higher expansion on the surrounding runways. Additionally, inspired from naturally forming nacre found in some seashells, a 3D printed plastic-concrete beam structure was developed and tested in flexure to determine its energy absorption capabilities. The nacreous structure allows the material to experience a strain-hardening behavior, thus allowing for energy dissipation in the beam as it deflects from further applied load. It is theorized that the energy absorption capabilities would be suitable for withstanding the effects of dynamic loadings in structures, such as earthquake and blast loads. Multiple beam structures were developed and tested to determine the impact of percent-polymeric material and layout had on the energy dissipation. Overall, the specimens with more polymer in the cross-section demonstrated larger load vs. crack mouth displacement curves and fracture energy. These specimens demonstrated a higher toughness as well, making them more suitable for use in structural applications. As the project is still in development, future tests and analysis must be performed to determine their strength properties and feasibility as a structural material. The results of this thesis highlight the benefits of novel polymer composites in industrial and infrastructure applications, such as improved rapid setting characteristics and significantly enhanced mechanical and energy absorbing performance. Future work is needed to optimize these performance metrics, such as freeze thaw cycling, fatigue, and durability tests for the polymer concrete and analysis of moment capacity for the bioinspired nacreous composites. / Master of Science / Composite materials have a wide range of applications in civil and structural engineering due to their advantages in mechanical properties and higher strengths over the base materials alone. Polymer concrete composites are not as widely used due to their greater initial costs. However, they are very attractive in industrial and infrastructure applications because of the improved behavior in tension. This thesis explores the mechanical properties of two different polymer-concrete composites and their effectiveness in civil and structural applications: polymer concrete for rapid repair and 3D printed plastic-concrete composite members for energy absorption. The North Atlantic Treaty Organization (NATO) requires that emergency repair of military runways should be completed within 4 hours. In coordination with Luna Innovations Incorporated, a polymer concrete was developed by Luna for use as a rapid repair material for military runways to meet this requirement through its rapid heat curing. Its mechanical properties were tested and compared against another rapid repair material. The polymer concrete formulation that was down-selected for further testing met the requirements of the military for all tests performed except for the coefficient of thermal expansion. As the polymer concrete is still under development, future tests are to be performed to determine the impact of the higher expansion on the surrounding runways. Additionally, inspired from naturally forming nacre found in some seashells, a 3D printed plastic-concrete beam structure was developed and tested in bending to determine its energy absorption capabilities. The nacreous structure allows the material to experience a strain-hardening behavior, thus allowing for energy dissipation in the beam as it deflects from further applied load. It is theorized that the energy absorption capabilities would be suitable for withstanding the effects of earthquake and blast loads in structures. Multiple beam structures were developed and tested to determine the impact of percent-polymeric material and layout had on the energy dissipation. Overall, the specimens with more polymer in the cross-section demonstrated greater energy absorption capabilities. As the project is still in development, future tests and analysis must be performed to determine their strength properties and feasibility as a structural material. The results of this thesis highlight the benefits of novel polymer composites in industrial and infrastructure applications, such as improved rapid setting characteristics and significantly enhanced mechanical and energy absorbing performance. Future work is needed to optimize these performance metrics, such as freeze thaw cycling, fatigue, and durability tests for the polymer concrete and analysis of moment capacity for the bioinspired nacreous composites.