Lors du forage des puits d'hydrocarbure, une pâte de ciment est coulée dans l'espace annulaire entre le cuvelage en acier et les formations géologiques traversées. Pompée à l'état liquide, cette pâte de ciment fait sa prise le long du puits sous différentes conditions de température et de pression. La gaine de ciment ainsi mise en place a pour principales fonctions de promouvoir l'étanchéité pour protéger le casing contre la corrosion, de fournir le support mécanique pour assurer la stabilité du puits et d'isoler les différents fluides dans les couches traversées. Au cours de sa vie dans le puits, depuis le forage à la complétion et de la production à l'abandon, la gaine de ciment est soumise à différentes sollicitations mécaniques et thermiques qui peuvent l'endommager et altérer ses principales fonctions. La réponse de la pâte de ciment soumis à ces sollicitations dépend non seulement des conditions d'hydratation mais aussi de l'histoire des chargements précédemment appliqués. La prédiction du comportement de la gaine de ciment doit donc se faire à l'aide d'une modélisation numérique qui nécessite une loi de comportement pour la pâte de ciment. Le but de cette thèse est d'établir une loi de comportement de la pâte de ciment en cours d'hydratation pendant le jeune-âge (les 144 premières heures). Pour ce faire, des essais calorimétriques, de mesures de vitesse des ondes et des essais œdométriques ont été réalisés sur une pâte de ciment pétrolier classe G (w/c = 0,44) en cours de prise. Les conditions d'hydratation explorées vont de 7 à 30°C pour les températures et de 0,3 à 45MPa pour les pressions. Les résultats expérimentaux ont montré que les déformations volumiques de la pâte de ciment dues à son hydratation (retrait macroscopique) sont considérablement influencées par la contrainte sous laquelle la pâte de ciment s'hydrate. Plus la contrainte d'hydratation est élevée, plus élevé est le retrait macroscopique à 144 heures. Inversement, les déformations irréversibles dues à un cycle de chargement mécanique à cet âge sont moins importantes pour les contraintes plus élevées. Les résultats ont également montrés qu'au cours de la prise du ciment, il existe un temps critique à partir duquel l'application des cycles de chargement mécanique crée des déformations résiduelles dans la pâte de ciment. Ce temps critique arrive à un degré d'hydratation relativement constant, compris entre 0,18 et 0,20. Le modèle « Boundary Nucleation and Growth » a été utilisé pour étudier la dépendance de ce temps critique à la pression et à la température. Pour la modélisation du retrait macroscopique et de la réponse contrainte – déformation de la pâte de ciment, un modèle élasto-plastique chemo-poro-mécanique couplé, prenant en compte la désaturation du milieu, a été développé. Ce modèle utilise une surface de charge fermée de type Cam-Clay et une loi plastique associée. La loi d'écrouissage dépend des déformations volumiques plastiques et du degré d'hydratation. Les paramètres du modèle ont été évalués pour simuler le retrait macroscopique de la pâte de ciment hydratée sous différentes contraintes et températures. A un degré d'hydratation donnée, le modèle permet également de simuler la réponse contrainte-déformation due à un chargement mécanique / When drilling oil & gas well, cement slurry is pumped between the casing and the rock formation. This cement slurry sets at different conditions of temperature and pressure. The role of this cement sheath is to provide zonal isolation of different fluid along the well, to protect the casing against corrosion and to provide mechanical support. During the life of the well, from drilling to completion, production and P&A (plug and abandonment), the cement sheath is submitted to various mechanical and thermal loading that can potentially damage its properties and alter its performance. The behavior of cement paste submitted to theses solicitations depends both on the hydration condition and the loadings previously applied on the cement paste. The prediction of cement sheath behavior should be done by numerical modeling, which needs a constitutive law for cement paste. The purpose of the present work is to establish a constitutive law of cement paste during its hydration at early age (first 144 hours). The approach is based on combined calorimetric, wave velocities and oedometric tests on an oil-well class G cement paste with water-to-cement ratio equals 0.44. The hydration conditions explored are 7 to 30°C for temperature and 0.3 to 45MPa for pressure. The experimental results showed that the volumetric strain due to cement hydration (macroscopic shrinkage) depends considerably on the hydration pressure. At 144 hours of hydration, the macroscopic shrinkage increases with the hydration pressure increase. But, the residual strain due to application of mechanical cycle at this age is less for cement hydrated under higher pressure. The experimental results revealed that during the hydration there is a critical time after which, the application of mechanical loading can potentially induce residual strain in cement paste. This time is reached at constant hydration degree between 0.18 and 0.20. The Boundary Nucleation and Growth model was used to model the pressure and temperature dependence of this critical time. A coupled elasto-plastic chemo-poro-mechanical model is developed to simulate the macroscopic shrinkage of cement paste hydrated at different conditions of temperature and pressure. A modified Cam-Clay type yield surface with associate flow rule is used. The hardening law depends both on the degree of hydration and on the plastic volumetric strain. At constant degree of hydration, the developed model permits to simulate the stress – strain behavior of cement paste due to the mechanical loading

Dans cette thèse, les travaux présentés s’appuient sur une démarche expérimentale utilisant, outre les mesures destructives habituellement mises en œuvre pour la caractérisation des matériaux cimentaires, les techniques non destructives exploitant la propagation des ondes ultrasonores à des fréquences comprises entre 50 kHz et 600 kHz. L’objectif est d’étudier les corrélations entre les propriétés hydrauliques et mécaniques de la pâte de ciment et les paramètres linéaires des ondes ultrasonores (vitesse et atténuation). L’étude concerne plus particulièrement les relations entre la porosité et la vitesse ultrasonore des différents types d’onde (ondes de volume et onde de Rayleigh). Les matériaux étudiés sont des pâtes de ciment à porosité variable, confectionnées avec différents rapports E/C et avec différents dosages en entraineur d’air. Afin de prendre en compte l’effet de la teneur en eau, les mesures sont effectuées à différents états de saturation : état saturée, 70% de saturation, 30% de saturation et l’état sec. Les données recueillies permettent la constitution d’une base des données expérimentale regroupant les caractéristiques physiques, mécaniques et ultrasonores de la pâte de ciment. Dans la dernière partie de cette thèse, les relations entre les vitesses ultrasonores et la porosité basées sur deux approches macroscopique et microscopique sont présentées et confrontées aux mesures / In this thesis, we present an experimental study including, besides the destructive measurements usually implemented for the characterization of cementitious materials, non-destructive techniques using ultrasonic wave propagation in a frequency range from 50kHz to 600kHz. The objective is to study the correlations between hydraulic, mechanical properties and linear ultrasonic parameters (velocity and attenuation) of cement paste. This study specifically addresses the relationship between porosity and ultrasonic velocity of the different types of waves (body waves and Rayleigh wave). The studied materials are cement pastes with variable porosity, made up with different water / cement ratios and with different concentrations of air entrainer. To take into account the effect of water content, measurements are made at different states of saturation: saturated state, 70% saturation, 30% saturation and dry state. The data collected allows the creation of a database of experimental data involving physical, mechanical and ultrasonic parameters of cement paste. In the final part of this thesis, relationships between ultrasonic velocity and porosity based on macroscopic and microscopic approaches are presented and compared with measurements

Made available in DSpace on 2014-12-17T14:07:02Z (GMT). No. of bitstreams: 1 MarcosASA_capa_ate_cap5.pdf: 2919360 bytes, checksum: 8bb04eb85df77f75f3f1de37bbecc19d (MD5) Previous issue date: 2009-04-02 / The Potiguar basin has large fields of viscous oil where the used method for recovering is based on vapor injection; this operation is carried out by injecting vapor in the oilwell directly, without the protection of a revetment through thermal insulation, what causes its dilation and, consequently, cracks in the cement placed on the annular, and lost of hydraulic insulation; this crack is occasioned by the phenomenon of retrogression of the compressive resistance due to the conversion of the hydrated calcium silicate in phases calcium-rich, caused by the high temperatures in the wells, subjected to thermal recuperation. This work has evaluated the application of composite pastes with addition of residue of biomass of ground sugar-cane bagasse as anti-retrogression mineral admixture for cementation of oil-wells subjected to thermal recuperation. The addition of the mineral residue was carried out considering a relative amount of 10, 20, 30, 40 and 59% in relation to cement mass, trying to improve the microstructure of the paste, still being developed a reference paste only with cement and a paste with addition of 40% of silica flour - renowned material in the oil industry as anti-retrogression additive. Pozzolanic activity of the ash was evaluated through XRD, TG/DTG, as the resistance to compression, and it was also determined the physical and mechanical behavior of the pastes when submitted to cure at low temperatures (22 and 38? C); besides it was evaluated the behavior of the pastes when submitted to two cycles of cure at high temperature (280?C) and pressure (7 MPa). It was verified that the ash of the sugar-cane biomass presents pozzolanic reaction and has great efficiency in decrease the permeability of the paste by filler effect, as well as that addition of ash in a relative amount of 10, 20 e 30% increases cured compressive resistance at low temperatures. It was also showed that the ash in a relative amount of 40% and 59% has very significant efficiency as anti-retrogression additive, since it prevents the decrease of compressive resistance and forms hydrated calcium silicate type xenotlita and tobermorita which have more resistance and stability in high temperatures / A bacia Potiguar tem grandes campos de ?leo viscoso, onde o m?todo de recupera??o utilizado ? a inje??o de vapor; essa opera??o ? realizada injetando-se vapor diretamente no po?o, sem a prote??o do revestimento atrav?s de isolamento t?rmico, o que provoca a dilata??o do mesmo, provocando assim falhas no cimento colocado no anular, e conseq?entemente, perda do isolamento hidr?ulico, esta falha tem origem no fen?meno de retrogress?o da resist?ncia ? compress?o devido a convers?o do silicato de c?lcio hidratado em fases ricas em c?lcio, provocada pelas elevadas temperaturas nos po?os, sujeitos ? recupera??o t?rmica. O presente trabalho avaliou a aplica??o de pastas comp?sitas com adi??o de res?duos de biomassa do baga?o da cana-de-a??car mo?das como aditivo mineral anti-retrogress?o para cimenta??o de po?os petrol?feros sujeitos a recupera??o t?rmica. A adi??o do res?duo mineral foi realizada teores de 10, 20, 30, 40 e 59% em rela??o a massa do cimento, visando melhorar a microestrutura da pasta, sendo ainda produzidas uma pasta de refer?ncia, apenas com cimento e uma pasta com adi??o de 40% de silica flour material consagrado na ind?stria de petr?leo como aditivo antiretrogress?o. Foram avaliados a atividade pozol?nica da cinza atrav?s de DRX, TG/DTG e resist?ncia ? compress?o, determinando-se tamb?m o comportamento f?sico e mec?nico das pastas submetidas a cura com baixas temperaturas (22 e 38?C), al?m da avalia??o do comportamento das pastas submetidas a dois ciclos de cura a alta temperatura (280?C) e press?o (7 MPa). Verificou-se que a cinza de biomassa da cana apresenta rea??o pozol?nica, tendo grande efici?ncia na diminui??o da permeabilidade da pasta por efeito filler, e que as adi??es de cinza em teores de 10, 20 e 30% aumentam a resist?ncia ? compress?o das pastas curadas a baixas temperaturas. Constatou-se ainda que a cinza em teores de 40% e 59% tem ?tima efici?ncia como aditivo antiretrogress?o, pois evitam a diminui??o da resist?ncia ? compress?o e formam silicato de c?lcio hidratado do tipo xenotlita e tobermorita que se apresentam mais resistentes e est?veis as altas temperaturas

Made available in DSpace on 2014-12-17T14:07:20Z (GMT). No. of bitstreams: 1 ElvioAG_TESE.pdf: 3444604 bytes, checksum: d60cf497e4c263de969e02bb2eefe56f (MD5) Previous issue date: 2013-12-20 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / This research was motivated by the requirement of asbestos s replacement in building systems and the need to generate jobs and income in the country side of the state of Bahia, Brazil. The project aimed at using fibers from licuri leaves (syagrus coronata), an abundant palm in the region, to produce composites appropriate for the sustainable production of cement fibre reinforced products in small plants. The composites were produced in laboratory using Portland cement CP-II-F32, sand, water, licuri palm fiber contents of 1.0, 1.5 and 2.0% by weight of binder (two different fiber length) and metakaolin. The latter was chosen as an additional binder for its efficiency to reduce the alkalinity of cementitious matrixes therefore preventing the degradation of vegetable fibers. The characterization of the composite components was carried out by sieving and laser particle size analyses, thermal analysis, fluorescence and X-ray diffraction. The composites performance was evaluated by 3- point-bending tests, compressive strength, ultrasound module of elasticity, free and restrained shrinkage, water capillarity absorption and apparent specific gravity. It has been found that the addition of fibers increased the time to onset of cracking over 200.00% and a 25% reduction in cracks opening in the restrained shrinkage test. The capillary absorption reduced about 25% when compared to fiber-free composites. It was also observed with regard to flexural strength, compressive strength and specific gravity, that the addiction of fibers did not affect the composite performance presenting similar results for compounds with and without fibers. In general it can be stated that the reinforced composite fibers of palm licuri presents physical and mechanical characteristics which enable them to be used in the intended proposals of this research / A exig?ncia da substitui??o do amianto em sistemas construtivos em conjunto com a necessidade de gera??o de renda no sert?o da Bahia fez nascer o projeto do aproveitamento da fibra da palma do licuri (syagrus coronata), palmeira abundante na regi?o, na produ??o de comp?sitos para a fabrica??o artefatos de cimento refor?ados com fibras para a constru??o civil de maneira sustent?vel, em pequenas unidades fabris. Os comp?sitos foram produzidos em laborat?rio utilizando cimento Portland CP II-F32, areia, ?gua, metacaulinita e fibra da palma do licuri. As fibras foram adicionadas em teores de 1,0, 1,5 e 2,0% da massa do aglomerante e com dois comprimentos de fibra diferentes. A metacaulinita foi selecionada como aglomerante suplementar de forma a agir na redu??o da alcalinidade da matriz ciment?cia na perspectiva de diminuir ou at? mesmo eliminar a degrada??o das fibras vegetais em meio alcalino. Foram realizados ensaios de caracteriza??o dos componentes do comp?sito, incluindo granulometria, an?lise t?rmica, fluoresc?ncia e difratometria de Raios-X. A verifica??o do desempenho dos comp?sitos foi feita com ensaios de flex?o em tr?s pontos, resist?ncia ? compress?o axial, m?dulo de elasticidade por ultrassom, retra??o livre e restringida, absor??o de ?gua por capilaridade e massa espec?fica aparente. Verificou-se que a presen?a das fibras de licuri aumentou o tempo para o surgimento da fissura??o acima de 200,00% e redu??o de 25% na abertura das fissuras no ensaio de retra??o restringida. Com rela??o ? absor??o capilar ocorreu uma redu??o de 25%, quando comparados com os materiais sem fibras. Observou-se que, com rela??o ? resist?ncia a flex?o, compress?o axial e massa espec?fica aparente, a adi??o de fibras n?o afeta o desempenho dos materiais, apresentando resultados similares para materiais com e sem fibras. De uma maneira geral pode-se afirmar que os comp?sitos refor?ados com fibras da palma do licuri apresentam caracter?sticas f?sicas e mec?nicas que viabilizam sua aplica??o dentro das condi??es estabelecidas neste trabalho

Made available in DSpace on 2014-12-17T14:07:22Z (GMT). No. of bitstreams: 1 FranciscoASJ_TESE.pdf: 8792658 bytes, checksum: 82015e9b1bc788b7c608317086cdc276 (MD5) Previous issue date: 2014-05-30 / Researches have shown that the introduction of rubber in concrete improves the features of its deformability, as well as contributes to environmental disposal of waste generated in the tire retreading process. Furthermore, there is a high availability of limestone within RN and CE country. Ignorance about this stone, does not allow its wide use as aggregate, leaving, this abundant supply idle. A composite of limestone gravel, with proportions of tire rubber waste which could be used as concrete would be an alternative to concrete for low applications. Therefore, this research aims to evaluate the characteristics of concrete containing limestone gravel and proportions of little aggregate replacement (sand) by tire rubber waste. To this goal, the material components of the concrete were characterized, concrete specimens with limestone gravel were made, from the dash 1.0: 2.5: 3.5, varying the water/cement ratio, and inserting a commercial plasticizer, without a proportion of residue, known as reference. From this, concrete with and without the presence of the additive in the same proportions were chosen, as well as these with the use of granite gravel, for being the most used. Selected the references, to these, replacements of little aggregate (sand) were added replaced by rubber waste from the tire retreading process, treated with 1M NaOH in proportions from 5.0 to 20.0 % by mass, cured and exposed to the semiarid environment. The results indicate the possibility of using limestone gravel in the concrete composition with workability correction using plasticizer. There was a decrease in the mechanical properties of the concrete with increments of waste rubber, but there is an improvement in toughness and deformability of the composite, which makes it interesting for the construction of non-structural concrete floors, as well as, the rubber waste delayed the hardening process, continuing to gain resistance after 28 days / Pesquisas t?m mostrado que a introdu??o de borracha no concreto melhoram as caracter?sticas de deformabilidade deste, assim como, contribuem para destina??o ambiental de res?duos gerados no processo de recauchutagem de pneus. Somado a isto, existe uma alta disponibilidade de rocha calc?ria no interior do RN e do CE. O n?o conhecimento desta pedra, n?o possibilita sua ampla utiliza??o como agregado, deixando, esta farta oferta ociosa. Um comp?sito de brita do tipo calc?ria, com propor??es de res?duo de borracha de pneu que pudesse ser utilizado como concreto seria uma alternativa para concretos destinados a baixas solicita??es. Logo, este trabalho possui como objetivo a avalia??o das carater?sticas de concretos contendo brita calc?ria e propor??es de substitui??o do agregado mi?do (areia) por res?duo de borracha de pneus. Para tanto, caracterizou-se os materiais componentes do concreto, confeccionou-se corpos de prova de concretos com brita calc?ria, a partir do tra?o 1,0: 2,5: 3,5, variando-se a rela??o ?gua/cimento, e inserindo-se um plastificante comercial, sem a propor??o de res?duo, chamados de refer?ncia. A partir deste, foram escolhidos nas mesmas propor??es concretos com e sem a presen?a do aditivo, assim como, estes com a utiliza??o da brita gran?tica, por ser a mais utilizada. Escolhidas as refer?ncias, a estas foram acrescidas substitui??es de parte do agregado mi?do (areia) por res?duo de borracha de pneu proveniente do processo de recauchutagem, tratados com NaOH 1 M, nas propor??es de 5,0 a 20,0 % em massa, curados e expostos ao ambiente semi?rido. Os resultados indicam a possibilidade de utiliza??o da brita calc?ria na composi??o do concreto com corre??o da trabalhabilidade utilizando-se plastificante. Observou-se uma diminui??o nas propriedades mec?nicas dos concretos com incrementos de res?duo de borracha, por?m existe uma melhora de tenacidade, e deformabilidade do comp?sito, o que o torna interessante para a constru??o de pisos de concretos n?o estruturais, assim como, o res?duo retardou o processo de endurecimento, continuando o concreto a ganhar resist?ncia, ap?s os 28 dias

La recherche de matériaux dentaires efficaces est une préoccupation constante de toute l'histoire de la dentisterie. Avec l'émergence de meilleurs produits, le développement de matériaux toujours plus innovants s'est imposé. De plus, la combinaison de différentes sciences comme la chimie, la biologie, la physique et l'ingénierie a permis de mieux connaître les exigences liées à la restauration dentaire. Le projet BIODENSOL est un projet de recherche et de mobilité doctorale entre l'Université de Lyon et LUCIDEON Ltd (Stoke-on- Trent, Royaume-Uni), financé par la Commission européenne. Le projet a été conçu pour favoriser les relations entre la recherche académique et les applications commerciales, pour améliorer les innovations médicales et associer des chimistes de l'état solide avec des praticiens hospitaliers en contact direct avec les patients ayant des problèmes dentaires. Ce projet proposait trois thèses de doctorat permettant de répondre aux conséquences des caries et d'érosion de l'émail par les aliments acides, l'idée de base étant de favoriser la reminéralisation pour éviter ces problèmes. Les recherches ont évolué de manière indépendante selon trois voies distinctes examinant trois matériaux différents qui pourraient amener des solutions potentielles. Le sujet principal de cette thèse concerne l'étude de poudres de verre borosilicaté présentant une séparation de phases et pouvant être incorporées dans des ciments verre ionomères. Les verres borosilicatés sont des matériaux prometteurs qui ont été largement étudiés pour des applications biomédicales, comme par exemple les échafaudages dans les tissus mous où la réparation osseuse. Par analogie avec les verres silicatés développés par Hench en 1969, qui sont reconnus pour leur bioactivité et leurs propriétés antimicrobiennes, les verres borosilicatés pourraient intéresser la dentisterie. Le système de verre étudié ici est un verre basé sur l'association de 5 constituants, SiO2-K2O-B2O3-CaO-Al2O3, qui a une forte tendance à la séparation des phases. L'objectif de ce travail est d'élaborer par fusion/trempe puis caractériser une série de nouvelles formulations de verres borosilicatés, puis de comprendre le mécanisme et la cinétique de dissolution en relation avec leur microstructure et leur composition. La variation des proportions de chaque constituant est déterminée par l'approche des plans d'expérience. L'utilisation d'un traitement thermique pour favoriser la séparation des phases en vue d'influencer le taux de libération cationique a été spécialement étudiée. Le processus de dissolution des borosilicates dans une solution aqueuse neutre (fluide corporel simulé) ou dans une solution acide (simulant des scénarios où des bactéries ou des aliments acides sont présents) fournit des informations sur le type et la concentration des espèces libérées par le verre. Différentes compositions ont été étudiées dans lesquelles SiO2 et K2O sont fixés tandis que les autres éléments varient afin d'évaluer l'effet sur la séparation de phases. Les cinétiques de dissolution des ions B-, Si-, Ca-, K- et Al- peuvent alors être reliées à la chimie du verre et à la microstructure. La séparation de phases amorphes (APS) provoque la séparation d'une phase unique initialement homogène en deux phases ou plus de compositions différentes. Le degré d'interconnectivité des deux phases vitreuses dépend de la nature du mécanisme de séparation de phases. Les verres élaborés sont optiquement transparents, puis deviennent plus ou moins opalescents suite à un traitement thermique. Le degré d'opacité est clairement dépendant de la proportion des éléments entrant dans la composition du verre. Le schéma de la libération d'ions implique que l'une des phases est plus réactive et sensible à l'attaque ; elle sera dissoute plus rapidement du verre... [etc] / The research for efficient dental materials has been a constant throughout the history of dentistry. As better materials emerged, the development of ever more innovative materials has been pushed forward. Moreover the combination of different sciences such as chemistry, biology, physics and engineering has provided better knowledge to the demanding requirements of the dental restorations. The BIODENSOL project is a European commission funded mobility research project managed by the University of Lyon and LUCIDEON Ltd, Stoke-on-Trent, UK. The project is designed to help building relations between academic and commercial research to enhance medical innovations and associates solid state chemists and hospital practicioners in direct contact with the patients with dental problems. This project proposes three PhD studies to address the problems of caries and enamel erosion by acidic foods (leading to sensitive teeth) encouraging re-mineralization to help avoid these problems. The researches independently evolved in three different routes investigating three different materials that could provide potential solutions. The main objective of this thesis concerns the study of Borosilicate phase separated glass powders for glass ionomer cements. As silicate bioglasses developed by Hench in 1969, regarding their bioactivity and antimicrobial properties, borosilicates glasses are promising materials and have been widely studied for biomedical applications for scaffolds in soft tissues and for bone repair and could be of interest in dentistry. The glass system studied here is a borosilicate glass (SiO2-K2O-B2O3-CaO-Al2O3) with a strong tendency to phase separate. The objective of this work is to characterize a series of the novel borosilicate formulations and to understand the mechanism and kinetic of dissolution related to their microstructure and composition. The use of thermal treatment to promote phase separation as a means of influencing the rate of ion leaching was especially studied. The dissolution process of borosilicates in neutral body solution (simulating body fluid) or in acid solution (simulating scenarios where bacteria or acid foods are present) provides information regarding the type and concentration of species released by the glass. Different compositions have been investigated in which SiO2 and K2O are fixed while the other elements are varied in order to assess the effect on the phase separation. As the novel borosilicates produced with the meltquenching technique is immersed in an aqueous environment, B-, Si-, Ca-, K- and Al- species are released to different degrees as a function of the time. Ion leaching trends can be related to the glass chemistry and microstructure. It has been shown that the amorphous phase separation (APS) causes an initially homogeneous single phase to separate into two or more phases of different compositions. The degree of interconnectivity of the two glass phases depend on the nature of the phase separation mechanism. This process can occur by a nucleation and growth process which gives isolated spherical particles or by spinodal decomposition where an interconnected structure is obtained. It is significant that before a heat-treatment the glasses are optically clear, but turn opalescent to different degrees following a heat treatment depending on the wt% of the elements in the composition. The pattern of the ion release implies that one of the phases is more reactive and susceptible to acid attack and will be leached out from the glass earlier. The other phase will remain in the cement improving the mechanical properties of the dental restorative material. Moreover, the mixing of the glass powder with a commercial poly(acrylic acid) has shown interesting mechanical and bioactive properties. This work showed how the ions leaching are influenced by the glass composition and the heat-treatment... [etc]

The cement being used in the construction industry is the result of a chemical process<p>linked to the decarbonation of limestone conducted at high temperature and results in a<p>significant release of CO2. This thesis is part of the project EcoBéton (Green concrete) funded<p>by the French National Research Agency (ANR), with a purpose to show the feasibility of<p>high substitution of cement by mineral additions such as blast furnaces slag, fly ash and<p>limestone fillers. Generally for high percentages of replacements, the early age strength is<p>lower than Portland cement concrete. To cope with this problem, an optimisation method for<p>mix design of concrete using Bolomey’s law has been proposed. Following the encouraging<p>results obtained from mortar, a series of tests on concretes with different substitution<p>percentages were carried out to validate the optimisation method. To meet the requirements of<p>the construction industry related to performance of concrete at early age, which determine<p>their durability, a complete experimental study was carried out. Standard tests for the<p>characterization of the mechanical properties (compressive strength, tensile strength, and<p>setting) allowed to validate the choice of mix design on the basis of equivalent performance.<p>We focused on the hydration process to understand the evolution of the mechanical<p>properties. Setting time measurement by ultrasound device at different temperatures (10°C,<p>20°C and 30°C) showed that ground granulated blast furnace slag (GGBFS) and fly ash<p>delayed the setting process, while use of limestone filler may accelerate this process.<p>Calorimetric studies over mortars and concretes made possible to calculate the activation<p>energy of the different mixtures and a decrease in heat of hydration of concretes with mineral<p>additions was observed which is beneficial for use in mega projects of concrete. Scanning<p>Electron Microscopy observations and thermal analysis have given enough information about<p>the hydration process. It was observed that the hydration products are similar for different<p>concrete mixtures, but the time of their appearance and quantity in the cement matrix varies<p>for each concrete mix.<p>Last part of the thesis was dedicated to the study of main types of shrinkage. First of all,<p>deformations measured were correlated to hydration, capillary depression and porosity<p>evolution. Results allowed concluding that the use of mineral additions has an actual effect on<p>the plastic shrinkage behaviour, but its impact is not proportional to the percentage of<p>additions. Substitution of cement by the additions seems to have a marked influence on the<p>kinetics of the shrinkage without any effect on its long term amplitude. The study of<p>restrained shrinkage under drying conditions by means of ring tests showed that concretes<p>with high percentage of slag addition seem more prone to cracking than the Portland cement<p>concretes. / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished

La carbonatation est une pathologie qui affecte les matériaux à base de ciment tels que les bétons et lesmortiers. Les zones carbonatées du matériau deviennent fragiles et perdent ainsi leur pouvoir deprotection des aciers contre la corrosion. Les produits de corrosion engendrent alors une dégradation dubéton pouvant aboutir à la ruine de la structure.Six types de bétons adjuvantés et deux pâtes de ciments ont été formulés grâce à une étude rhéologiqueafin d’étudier l’effet de la carbonatation accélérée et naturelle sur la durabilité des bétons et des pâtesde ciments à base de ressources algériennes. Pour ce faire, plusieurs méthodes d’investigation sontutilisées, aussi bien à l’échelle macroscopique que microscopique.En conclusion, le modèle rhéologique empirique développé peut être utilisé pour formuler des bétonsrésistants à la carbonatation. L’étude de la carbonatation démontre que le protocole accéléré, peut serévéler moins agressifs que la carbonatation naturelle, notamment pour des pâtes de ciment denses.Dans ce cas, la carbonatation accélérée de la surface tend à combler la microporosité superficielle dubéton, freinant ainsi la diffusion du dioxyde de carbone, contrairement à la carbonatation naturelle quiagit de manière plus diffuse sans totalement obstruer la porosité. Moins les bétons sont compacts, plusle protocole accéléré s’avère effectif. / The carbonation is a pathology which affects cement-based materials such as concretes and mortars.The carbonated skin of material becomes brittle and losses the protection of inner steels againstcorrosion. The corrosion products generate a degradation of the concrete which may lead to thecollapse of the structure.Six types of adjuvant concretes and two cement pastes have been designed by a rheological study inorder to study the effect of accelerated and natural carbonation on the sustainability of concretes andcement pastes based on algerian resources. For this purpose, several investigation methods were usedwith both macroscopic and microscopic scales.In conclusion, the empirical rheological model developed herein can be used to formulate concretesresistant to carbonation. The study of carbonation shows that the accelerated protocol may be lessaggressive than the natural one, especially for dense cement pastes. In this case, the acceleratedcarbonation of the surface tends to fill up the superficial microporosity of the concrete, slowing downthe production of carbon dioxide, contrary to the natural carbonation which acts more diffusely withoutcompletely obstructing the pores. The lesser compact is the concrete, the more effective is theaccelerated protocol.

La fabrication additive (Impression 3D) consiste à fabriquer des objets couche par couche en utilisant un modèle 3D, un matériau approprié et une machine dédiée. Pour la construction, c’est un nouveau mode constructif qui se profile. Depuis 2010, la fabrication additive a fait un saut technique et médiatique dans ce secteur. Les projets d’impression 3D se sont multipliés et diversifiés avec les premières maisons construites entièrement au moyen de cette technologie (Winsun, D-Shape, Contour Crafting, Apis Cor…etc). Ce travail s’inscrit dans le cadre d’une thèse CIFRE démarrée en 2015 entre le laboratoire de génie civil de l’Ecole Centrale de Lille et l’entreprise Bouygues Construction. L’objectif de ce travail est d’étudier le potentiel de la fabrication additive pour la construction et plus précisément de proposer une formulation à matrice cimentaire qui sera mise en œuvre par impression 3D.La thèse est organisée en trois grandes parties.La première partie est consacrée à la définition de l’impression 3D et des matériaux cimentaires pour définir leurs interactions. La deuxième partie est dédiée à la formulation d’un matériau cimentaire imprimable. L’imprimabilité a été définie par trois indicateurs : l’extrudabilité, la buildabilté et l’adhérence. La troisième partie est destinée à la validation de la formulation proposée. Ce travail peut être considéré comme une première approche pour définir un protocole d’évaluation de l’imprimabilité des matériaux cimentaires à l’échelle du laboratoire ainsi qu’une première étape pour la conception d’une imprimante 3D destinée et adaptée à la construction. / Additive Manufacturing (3D printing) consists in building an object layer by layer following a 3D model. For this purpose an appropriate material, machine and model are needed. From Construction industry point of view, 3D printing is considered as a new building method. Since 2010, the use of 3D printing for construction has known a large evolution. More and more real construction projects are using this new technology. Some of these examples are Winsun in China, D-Shape in Italy, Contour Crafting in California or Apis Cor in Russia…etc.The work presented in this manuscript was conducted through an industrial PhD thesis (CIFRE) which was launched between “Ecole Centrale de Lille” and “Bouygues Construction” in 2015. The objective of this work was to study the potential of large scale 3D printing integration in the construction process and more precisely the development of a printable cement based mix design.The work is organized in three main parts.The first part was dedicated to 3D printing and cement based material as general concepts. Then their interactions were analyzed. The second part was devoted to the printable mix design. The printability was defined using three indicators: Extrudability, Buildability and layers adhesion. The third part was dedicated to check the printability of the proposed mix design. This work may be considered as a first approach to define a laboratory scale methodology for cement based materials printability testing. It is also a step to contribute to the development of construction 3D printers.

Les mousses cimentaires sont des matériaux solides poreux qui ont despropriétés isolantes intéressantes. Elles sont utilisées dans le domaine de laconstruction pour réduire la consommation énergétique des habitations. Cependant,lors de la prise cimentaire, certaines mousses se déstabilisent et s'effondrent. Laformulation de tels matériaux présente donc des difficultés techniques etscientifiques notamment du point de vue des interactions entre les nombreuxcomposés utilisés, organiques et minéraux. L’objectif de ce travail de thèse a doncété d’étudier spécifiquement les interactions entre la matière minérale et le tensioactifutilisé pour la mise en forme alvéolaire, afin de comprendre le rôle de l’agentmoussant dans les mécanismes de stabilisation des mousses. Pour ce faire, nousavons considéré un système réactif simplifié, mais proche de l’utilisation courante,composé d’un ciment classique, d'eau et d’un tensioactif dosable par spectroscopieUV-visible. Pour découpler les différents effets, nous avons étudié ce système à troiséchelles : la mousse cimentaire, le coulis non moussé et des films uniques. / Cement-based mineral foams are solid porous materials and presentvery interesting insulating properties. Such materials are used in the constructionsector in order to reduce the energy consumption of houses. However, theproduction of these materials can be difficult because of the kinetic competitionbetween foam stability and cement setting. Cement-based mineral foams areextremely complex materials because of the number of components and all theirinteractions. The objective of our study is to get insight into the interactions betweenmineral and organic compounds and to understand their role in the stabilizingmechanisms. Our strategy was to study a model system, sufficiently close the realone to be representative, and sufficiently simple to identify the contribution of thedifferent components. We used as a foaming agent a surfactant exhibiting acharacteristic peak in UV-visible spectroscopy in order to determine its function andposition in the complex system. We first worked on unfoamed slurries, then westudied thin liquid films and the foamed materials.