In this work the influence of alkaline activator on immobilization of lead and copper in alkali-activated blast furnace slag was investigated. A total of five activators were used; sodium water glass, potassium water glass, sodium hydroxide, potassium hydroxide and sodium carbonate. The leaching test according to ČSN EN 12457-4 was used to evaluate the level of immobilization of heavy metals, the leached solutions were analyzed by ICP-OES. For a better understanding of immobilization, the selected samples were characterized by analytical methods (FTIR, XRD, SEM, XPS). It was found that the degree of immobilization Pb2+ and Cu2+ in AAS was very high, regardless of the type of alkaline activator used.

Air entraining admixtures are surfactants, that are commonly used in Portland cement materials, because they form and stabilize small air bubbles distributed in the binder, thereby changing the pore size distribution. The aim of these additives is to increase the durability of the cured binder, especially in climatic conditions, where it must withstand low temperatures, and simultaneously improving the workability in the plastic state. The effect of air entraining admixtures in alkali-activated slag was studied for certain properties. Air entraining admixtures were able to entrain the air in the alkali-activated matrix, they changed the pore size distribution, which resulted in a reduction in capillary pressure in the porous complex, and there was a reduction of shrinkage under autogenous conditions, respectively. The improvement of workability is certainly also positive, but on the other hand there has been a bad effect on flexural strength and compressive strength. The morphology of the air entrained binder was observed by scanning electron microscopy, and simultaneously the effect of air entrained admixtures on hydration was observed by isothermal calorimetry.

No / The presence of free water in mortars destined for silo or bagged storage can lead to the degradation of the binder phase. Such water may be present as a result of using wet, as-delivered sand or as a consequence of prior processes such as de-activation of Roman cement. Thus, water must be removed from the system prior to storage. Part 1 of this paper describes the control of a technique by which quicklime is added to the wet system which principally dries it by both slaking the quicklime and evaporation as a consequence of the exothermic slaking reaction. Two examples of mortars are presented in which excess water is removed from the system by the inclusion of quicklime. In the first, the water is present in the as-delivered sand and the binder is a combination of the slaked lime and ggbs. In the second, the water remains after pre-hydration of a Roman cement which is a process to retard its rapid setting characteristics. It is shown that optimally dried mortars are not subject to degradation following storage of both mortar types. (C) 2015 Elsevier Ltd. All rights reserved.

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Combination of fine ground granulated slag with proper alkaline activator gives alkali-activated slag – a material with remarkable properties. Theoretical part of the thesis deals with summarizing basic informations about alkali-activated slag, its properties, production and utilization. It also follows research devoted to effects of curing of alkali activated slag and shrinkage-reducing admixtures on its properties. Objective of the experimental part is to determine the influence of curing conditions on the mechanical properties and microstructure of alkali-activated slag. These properties are also monitored in alkali-activated slag with carbon nanotubes and hydroxypropylmethylcellulose as an shrinkage-reducing admixtures.

Le travail décrit dans ce manuscrit s’inscrit dans le cadre de la gestion de déchets nucléaires, de faible activité à vie longue (FA-VL), composés d’alliage de magnésium et de graphite, produits pendant l’exploitation de la première génération de réacteurs nucléaires en France. Il s’agit d’étudier la possibilité de leur immobilisation par cimentation et de comprendre le comportement des colis ainsi fabriqués tout au long de leur vie. Plusieurs mécanismes couplés sont à considérer : l’alliage de magnésium peut se corroder au sein de la matrice d’enrobage, en particulier lors du couplage galvanique avec le graphite. La croissance de produits de corrosion autour du métal et la restriction des déformations propres de la matrice cimentaire engendrent des contraintes à l’intérieur du matériau. La vérification de certaines exigences de sureté (stabilité dimensionnelle du colis et faible production d’hydrogène) nécessite donc le développement d’un outil numérique pouvant prédire le comportement mécanique des colis. En particulier, un mortier de laitier activé à la soude, qui présente un intérêt particulier, est examiné. Ce liant appartient à la famille des matériaux alcali-activés dont la modélisation numérique du comportement est peu abordée dans la littérature. La construction du modèle numérique passe ainsi par une large campagne expérimentale (caractérisation du comportement thermo-chemo-mécanique du mortier de laitier alcali-activé et de la corrosion du magnésium dans les matrices cimentaires) puis par un travail d’homogénéisation par éléments finis pour pouvoir déterminer les propriétés de l’ensemble (mortier + déchets) et mener des simulations à l’échelle du colis. Concernant le premier axe d’étude expérimentale, un faible échauffement accompagne l’avancement des réactions d’hydratation, ce qui est bénéfique vis-à-vis des contraintes internes résultantes de l’auto-restriction des déformations thermiques au sein des structures massives. Néanmoins, les déformations de retrait endogène montrent un développement important à long terme. Ceci peut générer des contraintes internes dans le colis (en présence de restrictions), mais la grande capacité de fluage du matériau empêche la fissuration. Concernant le deuxième axe d’étude expérimentale, le mortier de laitier activé est comparé avec deux autres mortiers à base de CEM I, pour évaluer le comportement à la corrosion de l’alliage de magnésium. Les observations microscopiques montrent que la corrosion galvanique de l’alliage est particulièrement agressive dans les mortiers à base de CEM I (corrosion localisée se manifestant par des creusements et des microstructures en feuillets) contre une corrosion uniforme, mais faible dans le mortier de laitier alcali-activé. La cinétique de corrosion est déterminée en utilisant des techniques gravimétriques et électrochimiques. Les résultats de ces deux types de mesure sont complémentaires et témoignent également d’une faible corrosion dans le mortier de laitier activé. De plus, ils montrent une certaine passivation du métal au-delà de 6 mois d’enrobage. Cette propriété spécifique du mortier de laitier activé peut être expliquée par une grande résistivité électrique par rapport aux mortiers de CEM I déterminée en analysant les données de spectroscopie d’impédence électrochimiques. Ensuite, des premières simulations simplifiées par éléments finis à l’échelle mésoscopique sont effectuées sur Cast3m, pour modéliser l’effet mécanique du développement de la corrosion sur le mortier d’enrobage. Plusieurs paramètres sont intégrés comme la cinétique de corrosion de l’alliage ainsi que la nature des produits formés et leurs propriétés mécaniques, identifiées par des observations MEB/EDS et nano-indentation. Les résultats indiquent que les contraintes générées dans la matrice d’enrobage n’entrainent pas d’endommagement. / The operation phase of the first generation of nuclear reactors in France has generated magnesium and graphite long lived low-level wastes (LLW-LL). Their conditioning in a hydraulic binder matrix is being addressed. In order to study the behavior of these packages, several coupled mechanisms have to be considered: the magnesium alloy can corrode within the encapsulating matrix, especially when galvanic coupling with the graphite occurs. The corrosion of the metal results in the development of corrosion products. The growth of corrosion products around the metal and the restriction of the hydraulic binder’s delayed strains may lead to the generation of internal stresses. The verification of certain safety requirements (dimensional stability of the package and low hydrogen production) is therefore essential. It requires the development of a numerical model able to predict the behavior of these packages.In particular, a sodium hydroxide activated blast furnace slag mortar is being addressed. It belongs to the family of alkali-activated materials for which the modelling of ageing behavior is rarely approached. Hence, the construction of the numerical model involves a large experimental campaign covering the thermo-chemo-mechanical behavior of the alkali-activated mortar and the corrosion of magnesium in hydraulic binders. Meso-scale homogenization calculations are undertaken in order to determine upscaled properties of the mix (matrix + wastes) and carry out simulations on the scale of the packages.Regarding the first experimental study axis, a relatively low hydration heat is measured. This is beneficial with respect to the internal stress generated from the self-restriction of the thermal strains within massive structures.Nevertheless, the materials undergoes a particular autogenous shrinkage strains showing an increase even at long term. However, its basic creep strains are shown to be important which could result in stress relaxation and avoids damage related to shrinkage restriction.Regarding the metal’s corrosion behavior in the alkali-activated mortar, it is compared to the one in two different ordinary Portland cement (OPC) based mortars. Microscopic observations are conducted on samples especially designed to monitor the galvanic corrosion of the alloy. They show the aggressiveness in OPC mortars (localized corrosion manifested by holes and layered microstructure) against limited homogeneous corrosion in alkali-activated mortar. Additionnaly, corrosion kinetics are determined using different experimental methods: mass loss and electrochemical measurements. The complementary results of these two types of measurements also show a low corrosion in the alkali-activated slag mortar with a passive state of the metal achived at 6 months of embedment. This advantage of slag mortar is explained by a high electrical resistivity with respect to OPC mortars, determined by electrochemical impedance spectroscopy.Finite element simulations are performed using Cast3m software on meso-scale in order to evaluate the mechanical effect of the corrosion layer development on the surrounding matrix. The corrosion kinetics of the alloy, the nature of corrosion products and their mechanical properties identified using SEM/EDS and nano-indentation techniques are implemented. The calculations indicate low stress generation in the alkali-activated mortar.

Production of construction materials requires a large amount of energy. That can be decreased by using of waste materials. This thesis deals with the self-sensing properties of composites. It presents electrical properties of building materials and their measurement. In the experimental part, the influence of conductive fillers on the self-sensing properties of aluminosilicate composites was examined. Test cubes were made of alkali-activated slag with a content of graphite powder, carbon black, carbon fibers, steel fibers or carbon nanotubes. The fractional change in resistence during cyclic compressive loading was monitored.