Ce travail propose une étude expérimentale visant à caractériser les processus dynamiques se produisant au sein de matériaux vitreux mous. La première partie présente des mesures de diffusion de traceurs nanométriques dans la Laponite (une suspension colloïdale) obtenues par une méthode de recouvrement de fluorescence (FRAP). Cette étude montre que la diffusion varie avec la concentration de Laponite et la taille du traceur. Un modèle hydrodynamique de diffusion confinée permet de décrire quantitativement les données expérimentales. Une deuxième partie concerne l’étude expérimentale du vieillissement de matériaux vitreux. Nous testons en pratique le concept théorique de température effective. Celle-ci est obtenue grâce à la technique de FRAP par la mesure simultanée de la diffusion et la convection de sondes fluorescentes dans la Laponite en cours de prise. Contrairement à certaines mesures de la littérature, le système est bien gouverné par la température ambiante. Nous présentons ensuite une étude visant à caractériser le comportement de la Laponite cisaillée. Nous avons pour cela mis au point un dispositif permettant d’appliquer un champ électrique au système, et ainsi créer des déformations locales. L’effet obtenu s’est révélé trop faible, avec d’assez grandes incertitudes (probablement liées à la complexité du système), pour être considéré comme significatif. Enfin, nous avons étudié les propriétés du Carbopol, un fluide à seuil, en mesurant sa dynamique d’ascension par capillarité. La rugosité de surface des capillaires influe énormément sur la montée du fluide. Nous montrons aussi que l’ascension est pilotée par la rhéologie du système, notamment par le seuil d’écoulement. / This work is based on an experimental analysis of the dynamical processes which occur within soft glassy materials. The first part provides measurement results of nanotracers diffusion in Laponite (a colloidal suspension) obtained by a method of fluorescence recovery (FRAP). This study shows that the diffusion is affected by the concentration of Laponite as well as the size of the tracer. A hydrodynamic model with confined diffusion allows a quantitative description of the experimental data. In a second part, an experimental study is carried out, dealing with the aging processes of glassy materials. The theoretical concept of effective temperature is probed experimentally. The effective temperature is determined using the technique of FRAP, by simultaneously measuring diffusion and convection of fluorescent probes within the aging Laponite. Contrary to some measurements found in literature, results show that the system is controlled by the bath temperature. The following study then aims at characterizing the behavior of the sheared Laponite : an experimental device is developed in this perspective, by applying an electric field to the system and thus creating local deformations. However, the observed effect appears to be too low, with relatively large uncertainties (probably linked to the complexity of the system), which impede on the significance of our results. Finally, the properties of Carbopol, a yield stress fluid, are analyzed by measuring the dynamics of capillary rise. It is shown that the surface roughness of capillary strongly affects the rise of the fluid and that the latter is controlled by the rheology of the system, and more specifically by the yield stress value.

Afin de mieux comprendre les spécificités de l'écoulement des fluides en seuil en géométries confinées, nous avons opté pour une approche multi-échelle expérimentale et/ou numérique dans des milieux poreux complexes et modèles. Nous montrons qu'il est possible d'utiliser la RMN pour visualiser des écoulements de fluides à seuil en géométrie complexe. Dans un milieu poreux, il est également possible de mesurer la distribution statistique des vitesses, ceci sans problème de résolution spatiale, grâce à la méthodologie de réglage d'une expérience d'injection sous IRM que nous avons mise en place. A l'aide de ces techniques, nous montrons que l'écoulement d'un fluide à seuil dans un pore modèle (une expansion-contraction axisymétrique) se localise dans la partie centrale du pore, dans le prolongement du tube d'entrée, tandis que les régions extérieures restent dans le régime solide. Des simulations numériques confirment ces résultats et montrent que la localisation de l'écoulement provient du confinement engendré par la géométrie. A l'inverse, nous montrons que pour un fluide à seuil s'écoulant dans un milieu poreux réel (en trois dimensions), il n'existe pas de zones au repos. De plus, la distribution de vitesse est identique à celle d'un fluide newtonien. Une analyse de ces résultats nous permet de prédire la forme de la loi de Darcy pour les fluides à seuil et de comprendre l'origine physique des paramètres déterminés par des expériences d'injection « macroscopiques » / To better understand the specifics of the flow of yield stress fluids in confined geometries, we opted for a multi-scale experimental and / or numerical approach in complex and model porous media. We show the usefulness of NMR for the study of yield stress fluid's flows in complex geometry. In a porous medium, we can also measure the true probability density function of fluid velocities without spatial resolution problem thanks to a complete optimisation of the design process of a NMR-PGSE experiment. Using these measurement technics, we find that the flow of a yield stress fluid in a model pore (an axisymetric expansion-contraction) is localised in the central part of the pore, i.e. in the continuity of the entry duct, and the external region stay at rest in the solid regime. Numerical simulations confirm those results and point out that the flow localisation is due to the confinement caused by the geometry. On the contrary, no region at rest exists for a yield stress fluid flowing through a real porous media (in 3D). Furthermore, the velocity distribution is the same as a newtonian fluid. The analysis of the results makes it possible to deduce the form of the Darcy's law for yield stress fluids and provides an insight in the physical origin of the coefficients found by “macroscopical” injection experiments

[pt] O petróleo é uma mistura complexa de hidrocarbonetos e pode conter em sua composição parafinas que, quando submetidas a baixas temperaturas, podem precipitar e gelificar, apresentando uma Tensão Limite de Escoamento. O estudo do comportamento do petróleo nesta condição é importante para a indústria porque, uma vez que o petróleo esteja gelificado, o reinício do escoamento pode demandar a adição de energia ao sistema, cujo dimensionamento para operação com altas pressões envolve custos elevados. Os valores de pressão de reinício de escoamento do petróleo gelificado encontrados no campo são frequentemente menores em relação aos valores calculados. O presente trabalho simulou o processo de reinício de escoamento através de uma bancada experimental que reproduz o resfriamento estático sofrido pelo petróleo parafínico em um duto submarino. Além disso, são apresentados dois métodos para cálculo da contração que resulta do resfriamentoe gelificação dos óleos parafínicos, objetivando verificar se existe uma relação entre a contração do fluido e a diferença entre a Tensão Limite de Escoamento e a tensão efetiva para iniciar o seu escoamento. O primeiro método proposto é o método da Pipeta, que consiste na utilização de uma pipeta, acoplada a um recipiente com controle de temperatura, para medição do volume de líquido. O segundo método proposto é o da célula PVT, que consiste na utilização de um sistema fechado de volume conhecido em que a medição da variação do volume de líquido é estimada pela variação do volume do gás à baixa pressão com a adoção da hipótese de gás ideal. Foram utilizados fluidos sintéticos, visando representar o petróleo parafínico, com diferentes concentrações de parafina, óleo mineral e querosene. A determinação da Tensão Limite de Escoamento foi feita a partir de testes de Creep. Os resultados mostraram que a contração do fluido é uma grandeza de difícil medição, com um alto grau de incerteza, mas que é possível estimar ordem de grandeza dessa contração para os fluidos estudados. / [en] Petroleum, as it is a complex mixture of hydrocarbons, may contain paraffinic compounds which, when subjected to low temperatures, can deposit and gel. The study of the behavior of petroleum in this condition is very important for the industry because, once the waxy crude oil gels, the restart process may demand extra energy addition to the system, whose dimensioning is expensive for high operation required pressures. Restart pressure values of the gelled oil found from laboratory tests often show a significant difference from the real values found in the field. In order to compare the yield stress and the effective stress, the present work simulated the flow restarting process through an experimental rig to reproduce the static cooling applied to a pipeline with waxy crude oil. In addition, two methods are presented for calculating the thermal shrinkage formed during the cooling and gelation of the waxy crude oils, in order to verify if there is a relationship between the shrinkage and the difference between the yield stress and the effective stress to start flowing. The first method proposed is the Pipette method, which consists of the use of a pipette, coupled to a container with temperature control, to measure the volume of liquid. The second method proposed is the PVT cell method, which consists of the use of a closed system of known volume in which the measurement of the liquid volume variation is estimated by the variation of the gas volume at low pressure with the adoption of the Ideal gas hypothesis. The fluids selected for the studies to represent paraffinic oil were laboratory-synthesized fluids with different concentrations of paraffin, mineral oil and kerosene, and they were characterized rheologically by stress ramp and creep tests for the determination of the yields stress. The results showed that thermal shrinkage is a difficult quantity to measure, which gives it a high degree of uncertainty, but it is possible to estimate the magnitude order of the thermal shrinkage for the fluids studied.

Le transport des bruts paraffiniques, et tout particulièrement leur remise en écoulement après un arrêt, dans de longues conduites sous-marines soumises à de basses températures, peut être difficile du fait de l'augmentation de leur viscosité. Le comportement rhéologique d´une huile paraffinique modèle, possédant des propriétés macroscopiques d'écoulement analogues à celles des bruts paraffiniques, est d'abord analysé en utilisant la vélocimétrie par imagerie par résonance magnétique associée à des mesures de contrainte de cisaillement au sein d'une géométrie Couette. Nous montrons que lors d'un écoulement forcé à température constante le matériau subit une déstructuration irréversible qui dépend de l'intensité du cisaillement. Ainsi la contrainte apparente critique permettant l'écoulement du matériau dépend de l'histoire thermique et d'écoulement subie par le matériau. Nous étudions ensuite le comportement rhéologique complet de deux bruts réels à partir de différents types de tests rhéométriques (fluages, redémarrage, régime permanent, changement brusque de vitesse) pour différentes histoires d'écoulement, notamment pendant la période de refroidissement. Le comportement détaillé du matériau en régime transitoire ainsi observé peut alors être modélisé. De plus les variations du seuil de contrainte en fonction de l'histoire thermique et de l'écoulement sont aussi décrites, ce qui nous donne le champ de contrainte seuil dans la conduite à l'état initial. Le modèle dans son ensemble est finalement implémenté dans un code de calcul pour simuler le redémarrage de l´écoulement d'un brut paraffinique dans une conduite réelle / Transporting waxy crude oils through long pipelines at low temperatures may be challenging, particularly its flow restart after a pipeline shut-in, due to its viscosity increase. The rheological behavior of a model waxy oil with macroscopic flow properties analogous to waxy crude oils is first analyzed using Magnetic Resonance Imaging velocimetry associated to stress measurements in a Couette geometry. While flowing at constant temperature, major irreversible structure break depending on shear intensity are observed. Thus, the critical apparent shear stress beyond which the material flows depends on the thermal and flow histories of the oil. Next, the rheological behavior of two waxy crude oils is studied using rheometrical tests (creep tests, flow restarts, abrupt changes of shear rate and steady flow) after different flow histories, notably during the cooling process. Then, those experimentally observed trends are modeled. Additionally, a comprehensive study of the yield stress in function of flow and temperature histories is presented. It provides an approach for describing the yield stress field inside the pipeline at the flow restart moment. Finally, the entire rheological model is implemented in the computational code for simulating waxy crude oils flow restart of a real scale pipeline

Forte de nombreux avantages par rapport aux techniques traditionnelles, la technique de pompage est largement utilisée de nos jours dans le domaine du génie civil. Pour utiliser cette technique, le béton doit être considéré comme « pompable ». Les études précédentes ont toutes montré que la pompabilité d’un béton dépend des frottements à l’interface entre le béton et la paroi des tuyauteries (constante visqueuse et seuil d’interface). L’amélioration de la pompabilité (tout en gardant la stabilité, l’homogénéité et les caractéristiques mécaniques d’un béton) permettra de diminuer le temps de mise en œuvre du béton et de faire avancer les travaux sur chantier. Dans ce contexte, l’objectif principal de ce travail est la modélisation du seuil d’interface à partir des paramètres de formulation et le calcul de la pression de pompage des bétons. Pour cela , une base de données expérimentales a été construite pour mettre en évidence l’effet des paramètres de composition des bétons ordinaires et des bétons avec des additions minérales sur les paramètres d’interface, donc sur la pompabilité. Cette base de données a été ensuite utilisée pour proposer et valider un modèle de calcul du seuil d’interface à partir des paramètres de composition et de l’affaissement. La précision de ce modèle est de l’ordre de ± 13%. Enfin, le modèle proposé a été utilisé pour estimer la pression de pompage. La comparaison entre les pressions de pompage estimées et celles mesurées expérimentalement sur site par d’autres chercheurs montre que la méthode proposée prévoit les valeurs de pression avec une précision de l’ordre de ± 15%. Les résultats de ce travail fournissent une base de données scientifique importante pour les utilisateurs de la technique de pompage et mettent en avant le rôle de chaque composant de formulation sur les paramètres d’interface. Ils peuvent également servir pour d’autres travaux de recherches à venir.Mots-clés : pompage de béton, pression de pompage, tribomètre, frottements, constante visqueuse, seuil d’interface, rhéologie, paramètres de composition, modélisation. / With many advantages over traditional techniques, the pumping technique is widely used nowadays in the civil engineering field. To use this technique, the concrete must be considered "pumpable". Previous studies have all shown that the pumpability of concrete depends on the friction at the interface between the concrete and the pipe wall (the viscous constant and the interface yield stress). Improving pumpability (while maintaining stability, homogeneity and mechanical properties of concrete) will reduce the implementation time of concrete and to advance work on site. In this context, the main objective of this work is the modeling of the interface yield stress from the formulation parameters and calculating the concrete pumping pressure. To facilitate the study, an experimental database was built to demonstrate the effect of the composition parameters of ordinary concrete and concrete with mineral additions on the interface parameters, so the pumpability. This database was then used to propose and validate an interface yield stress calculation model based on composition parameters and slump. The precision of this model is of around ± 13%. Ensuite, le modèle proposé a été utilisé pour estimer la pression de pompage. The comparison between the estimated pumping pressures and those measured experimentally on the site by other researchers has shown that the proposed method provides the pressure values with a precision of the order of 15%. The results of this study provide important scientific database for the pumping technology users and highlight the role of each formulation component on the interface parameters. They can also be used for other future research work.Keywords: concrete pumping, pumping pressure, tribometer, friction, viscous constant, interface yield stress, rheology, composition parameters, modeling.

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.

Solides élastiques au repos, les fluides à seuil s’écoulent comme un liquide au-delà d’une certaine contrainte. Plusieurs applications industrielles concernent l’écoulement de ces fluides dans des milieux poreux. On peut citer par exemple les émulsions dans le processus de récupération du pétrole, les opérations de cimentation dans le sol, ou le nettoyage d’un sol contaminé par une boue. Pour ces applications, il est nécessaire de connaitre la pression nécessaire pour un débit voulu à la sortie du milieu poreux. Dans de tels cas, l’écoulement est perturbé par la complexité de la géométrie. Les modèles développés pour décrire la loi de Darcy supposent une loi rhéologique appliquée localement, mais ces modèles décrivent mal ce type d’écoulement. De plus, des effets complexes peuvent s’ajouter comme le glissement à la paroi ou la thixotropie. Dans cette thèse, nous étudions l’écoulement de carbopol (ETD 2050) à travers différentes géométries. Tout d’abord au rhéomètre, nous montrons que le fluide, sous certaines conditions, correspond bien à un fluide à seuil modèle. Nous démontrons que le protocole expérimental utilisé est très important et qu’un comportement thixotropique peut apparaitre s’il n’est pas respecté. Ce comportement apparait notamment lorsque le fluide reste sous le seuil, l’impact augmentant avec le temps d’attente. Ensuite, nous comparons la loi d’écoulement obtenue au rhéomètre à l’écoulement dans un canal droit obtenu par microfabrication. Nous montrons alors l’importance du glissement proche du seuil et ses conséquences sur la loi d’écoulement. Enfin nous étudions l’écoulement du carbopol dans un milieu poreux. Le milieu poreux de 5x5cm est obtenu par microfabrication. La largeur moyenne des canaux est égale à celle du canal droit. Nous avons développé une nouvelle méthode de mesure des champs de vitesse. Nous montrons l’apparition d’une chenalisation de l’écoulement à travers quelques canaux du milieu poreux. Nous comparons ensuite la loi d’écoulement du milieu poreux à celle obtenue dans le canal droit. On remarque que la vitesse d’écoulement est plus faible dans le milieu poreux que dans le canal droit. / Elastic solids at rest, yield stress fluids flow like a liquid beyond a certain stress. Many industrial applications required the flow of these fluids in porous media, for example: the emulsion flow in oil recovery processes, the cementing operations in the ground, or the cleaning of sludge in a contaminated soil. For many applications, it could be interesting to know the pressure required for a desired flow rate. In such cases, the flow behavior of the fluid is complicated by the complexity of the geometry. The models developed to describe Darcy's law assume a rheological law applied locally, but these models poorly describe this type of flow. Furthermore, complex effects can be added like the wall slip or the thixotropy. In this thesis, we study the flow of carbopol (ETD 2050) through different geometries. First we show that the fluid, for some conditions, corresponds to model yield stress fluids. The experimental protocol used is very important and a thixotropic behavior can appear if it is not respected. This behavior appears especially when the fluid remains below the yield stress, the impact increases with the waiting time. We then compare the flow law obtained by rheometer in a straight channel obtained by microfabrication. We show the importance of the wall slip near the yield stress and the impact on the flow law. Finally, using a new method to measure the velocity fields developed during this thesis, we study the flow of carbopol in a porous medium. This porous medium of 5x5cm is obtained by microfabrication. The mean width of the channels is equivalent to the one of the straight channel. We show the emergence of a channeling flow through some channels of the porous medium. We then compare the flow law of the porous medium to the one obtained in the straight channel. It can be observed that the flow rate is lower in the porous medium than in the straight channel.

The rheological properties of cement-based grouts play a key role in determining the final spread in grouted rock formations. Rheologically, cement grouts are known to be complex thixotropic fluids, but their steady flow behavior is often described by fitting the simple Bingham constitutive law to flow curve data. The resultant Bingham parameters are then used in grouting design of e.g. tunnels, to estimate the penetration length. Since cement grouts are thixotropic suspensions, the interpretation of their flow curves as obtained from flow sweeps in concentric cylinder rotational rheometers is often complicated by: the presence of wall slip, sedimentation and unstable flow at low shear rates. A systematic approach to study these effects within the constraints of the concentric cylinder geometry (Couette) and for different cement grout concentrations was carried out as part of the Licentiate research work. Of particular interest was the influence of geometry and flow sweep measurement interval on flow curves, including the characteristic unstable flow branch that appears at applied shear rates that are below the critical shear rate. The unstable flow branch observed below the critical shear rate has been described as a characteristic feature in the flow curves of thixotropic suspensions, e.g. cement grouts, laponite. From a practical standpoint, this information can then be readily used to improve rheological measurements of cement grouts. The existence of the critical shear rate below which no stable flow occurs, plus the complex wall slip phenomenon are then discussed by considering how they affect actual spread in rough and smooth rock fractures. Another major part of the research presented in this thesis relates to the measurement of model yield stress fluid (YSF), i.e. Carbopol, velocity profiles within the radial flow geometry. Radial flow between parallel plates, is an idealized fundamental flow configuration that is often used as a basis for grout spread estimation in planar rock fractures. Compared to other flow configurations with YSFs, e.g. channels, only a limited amount of work has presented analytical solutions, numerical models and especially experimental work for radial flow. Thus, as a first step towards more systematic studies of the plug flow region of YSFs in radial flow the current work presents the design, manufacture and for the first time velocity profile measurements that were conducted by using the pulsed Ultrasound Velocity Profiling (UVP) technique. The current observations for tests carried out with different disk spacings and flow rates show a distinct plug region, coupled with wall slip effects for the Carbopol model YSF fluid that was used. The theoretically predicted velocity profiles and the measured ones agree reasonably well, and the main discrepancies are discussed. Future studies, would then be targeted at improving the current experimental setup, for detailed measurements of the plug flow region along the radial length, which remains a challenging issue for studies on YSFs and engineering applications such as rock grouting design. / Cementbaserade injekteringsmedels reologiska egenskaper har en stor påverkan på strömning och inträngningslängd i sprickigt berg. Medlens reologi är komplex, inklusive tixotropi, men strömningen beskrivs ändå oftast med den enkla linjära Bingham modellen i injekteringssammanhang. De två parametrarna från denna modell, flytgräns och viskositet, används sedan inom injekteringsdesign, för t.ex. tunnlar och dammar, för att bedöma inträngningen. Eftersom cementbaserade medel är tixoptropa suspensioner försvåras utvärderingen vid mätning med konventionella rotationsviskometrar på grund av glidning vid fasta begränsningsytor, sedimentation/separation av partiklarna och instabila flöden vid låga deformationshastigheter. En systematisk mätprocedur för att studera ovanstående problem med rotationsviskometer och koncentriska cylindrar samt olika vanliga vattencementtal, har utförts inom ramen för detta licentiatarbete. Av särskilt intresse har varit att studera effekten av olika geometrier och tidsintervallet mellan mätningarna, inklusive den instabila delen av flödeskurvan då deformationshastigheten är lägre än ett kritiskt värde. Denna del av kurvan har i litteraturen beskrivits som karakteristisk för tixotropa suspensioner, som t.ex. cementbaserade injekteringsmedel. Praktiskt kan ovanstående kunskap användas för att förbättra mätningen av de reologiska egenskaperna. Existensen av en kritisk deformationshastighet under vilken det inte finns något stabilt flöde, i kombination med glidning vid fasta begränsningsytor, diskuteras särskilt med hänsyn till dess påverkan på faktisk inträngning i släta och råa bergsprickor. Ett annat fokus i licentiatarbetet har varit att studera icke-Newtonska modellvätskors (Carbopol) radiella strömning mellan parallella plattor. Denna typ av strömningsgeometri används ofta som en idealiserad konfiguration för strömning i bergsprickor. I jämförelse med andra enklare geometrier, finns endast en begränsad forskning utförd för denna geometri både då det gäller analytiska och numeriska beräkningar men framförallt då det gäller experiment. Som ett första steg inför en mer systematisk undersökning av icke-Newtonsk radiella strömning presenteras i detta arbete framtagandet av en fysisk laboratoriemodell där hastighetsprofilerna mellan plattorna för första gången visualiserats med hjälp av ultraljud. De utförda mätningarna med tre olika öppningar mellan plattorna sam tre olika värden på det konstanta flödet, visar på en distinkt plugg som är ett resultat av vätskans flytgräns samt glidning i gränsskiktet mellan vätskan och plattornas fasta begränsningsytor. En jämförelse mellan uppmätta hastighetsprofiler och analytiskt beräknade diskuteras där resultaten överensstämmer relativt väl, med beaktande av de långtgående förenklade antaganden som krävs för beräkningarna. Fortsatta studier kommer att fokuseras på att förbättra laboratoriemodellen för en mer detaljerad studie av icke-Newtonska vätskors strömning och hur pluggen utvecklas under den radiella inträngningen, vilket fortsättningsvis är av betydelse för design av injektering i bergsprickor. / <p>QC 20190521</p>

Preplaced aggregate concrete (PAC) is produced by grouting high workability cement based grouts among the voids of compacted coarse aggregate mass. Because of its low shrinkage, PAC has been used for many repair jobs like; tunnel lines, dams and bridge piers. Moreover, it has been used for underwater construction. Grout has a major effect on the properties of produced PAC and well defined grout controls the properties of resulted PAC. The effect of types and amount of powder materials, admixtures, sand and water content on the properties of fresh and hardened grout for the production of PAC have been investigated. Tests on hardened grout and PAC properties have also been carried out to investigate the most important effects. A correlation between hardened properties of grout and PAC has also been analyzed. Grout rheology using four different gradation sands at two different cement-sand and at different w/c ratios ratios has been identified experimentally; no added chemical admixtures or mineral additives had first employed, then superplasticizer (SP) was added at 2% and 1%, and finally a combination of 1% SP and pulverized fuel ash (Pfa) at 20% of the cement weight was employed for all mixes. Grout tests have included two point workability tests by the Viskomat NT, flow time funnel test, Colcrete flow meter test, and water bleeding test. After that, eighteen grout mixes with high workability were produced using three different sands at three w/c ratios and two c/s ratios with 1% SP and Pfa at 20% of the cement weight were designed. Eighteen hardened grout and PAC then produced and their compressive strength and sorptivity were tested. Grout rheology can be defined by the rheology of cement paste employed and the internal distance between sand particles. The effect of sand surface texture on grout rheology is important at very low internal distances. Fresh grout yield stress is the most important property which gives the same degree of sensitivity for all grouts regardless the material type and content used in the mix. There are strong relations between compressive strength of grout and PAC, but less correlation between them in sorptivity test because of the effect high quantity of coarse aggregate of PAC. Sorptivity of PAC is low comparing with different kinds of concrete suggesting its advantage for underwater construction. / Libyan High Education Ministry

Nowadays, construction industry is rapidly moving towards digitalization and automation that should enable increased rates and efficiency of construction processes, as well as higher possibilities for customization and architectural freedom. Among all technologies under development, digital fabrication with concrete by means of layered extrusion appears to be one of the most promising for purposes of fast mass housing construction. It enables formwork-free production of structures via layer-by-layer concrete printing. Freedom from formwork potentially makes the construction process more cost- and time-saving, but poses multiple challenges to mix design and test methods, especially in terms of concrete rheology. A special focus must be put on the structural build-up of concrete at rest, which is related to its buildability, i.e. capacity of the material to retain the shape of the extruded layers under their own weight and the weight of the subsequently placed layers. This research investigates into the structural build-up of cementitious materials, i.e. evolution of their strength and deformation properties over time at rest, and includes development and refinement of methodology to assess the structural build-up, as well as its modelling and prediction. With respect to methodology, major attention was directed to the constant rotational velocity (CRV) test used for evaluation of the static yield stress development, and rationalization of its application under field conditions. Based on a large amount of experiments performed with two rheometers of different design, characteristic curves and points describing patterns in behaviour of cementitious materials during a CRV test were established. The experimental study also dealt with assessing the effects of alterations in main elements of the CRV test protocol, such as test approach (single- versus multi-batch), pre-shear regime, applied CRV, on the test results. Possible errors in CRV tests were addressed and methods to improve the procedures of testing and data evaluation were suggested. In particular, the single-batch approach was enhanced by implementation of the developed breaking criterion, a concept of zero measurement for non-pre-sheared samples was introduced, and a method for simplified evaluation of elasticity by a single-head rheometer was proposed. General methodological recommendations on the design of a CRV test protocol were formulated. The results are applicable for various cementitious materials and not limited to concretes for layered extrusion. Furthermore, test methods for assessing the structural build-up of printable concretes were studied in terms of their applicability under field conditions, potential for automation, descriptiveness of obtained data and efficiency in predicting the buildability of printed concrete structures. The methods under investigation included CRV test, unconfined uniaxial compression test (UUCT), fast penetration test and newly proposed confined uniaxial compression test (CUCT); all tests were performed on extruded samples of eight printable concrete mixtures with various compositions and rheological properties. The corresponding results were juxtaposed in order to establish correlations between the data and compared to the results of buildability tests, in which hollow cylindrical structures were produced using a laboratory-scale 3D printer. The developed methodology was further used to conduct an in-depth investigation into the influence of aggregates on the structural build-up of ordinary concrete. In the experimental program, the binder composition was kept constant while the aggregate was varied in terms of the volume fraction and the surface area (per unit volume of concrete); the main focus was put on compositions with elevated aggregate content (45−55 % by volume). A mechanism lying behind the effects of the aggregate properties on the structural build-up of concrete was discovered by studying the structure of constitutive paste in concrete. Aggregate-induced inhomogeneity of constitutive paste allowed to introduce a three-component model of fresh concrete. Furthermore, to find models capable of predicting the parameters of structural build-up of concrete, i.e. static yield stress and structuration rate, concrete was viewed as a suspension of aggregate particles in suspending medium. Three approaches were employed to define the correspondent components. Suspending medium was represented by plain cement paste, screened cement paste and fine mortar considered as a part of concrete comprising particles below 0.5 mm; a substantiation for such a definition was provided. Applicability and limitations of the models based on all three approaches were compared. The modelling approach was further extended to printable concretes with nearly identical aggregate compositions, but different properties of paste. Opportunities and challenges in modelling the structural build-up of printable concrete, including the problem of material dependency of the models and the relevancy of fitting coefficients, were discussed. A modified Chateau-Ovarlez-Trung model based on the definition of suspending medium as fine mortar was acknowledged as best suited to describe the structural build-up of both ordinary and printable concrete.