This research targets Metakaolin as main material, with various kinds of combination materials and binder, and uses a mechanism to make colding metakaolin lightweight aggregate and then makes five different proportion of metakaolin lightweight aggregate, with an aim to know the effects of different proportion on aggregate through the destruction of point load , sift analysis , and unit weight. Choosing suitable aggregate based on ACI norm to set three groups of different water-cement ratio A(0.54)¡BB(0.46)¡BC(0.35) to mix into lightweight aggregate concrete, this is to find out the correlation between physical properties and mechanical behavior of metakaolin lightweight aggregate concrete through pressure resistance , splitting off , absorption capacities. The result shows that different proportions of metakaolin lightweight aggregate also take different effects, a suitable formula is selected in accordance with the application. Of all the groups, group D (cement¡Gslaked lime¡Gmetakaolin¡Gfly ash¡Gsand =12.5%¡G12.5%¡G28.125%¡G 9.375%¡G37.5%) has the best mechanical and physical performance. The mechanical properties such as pressure resistance and splitting strength of aggregate made from metakaolin lightweight aggregate concrete can meet up with CNS and ASTM norms, and it is superior to fly ash lightweight aggregate concrete.

Partial replacement of cement by metakaolin is known to improve concrete durability, by refining the pore structure to improve fluid transport properties and by reducing the alkalinity of the pore solution to make ASR less problematic. A gap exists in the literature as to the salt scaling performance and magnesium sulphate performance of metakaolin concrete. 10 concrete mixes were cast at w/cm ratios of 0.4 and 0.5. In addition to metakaolin, grade 80 slag was used as well as CSA GU cement. All replacement levels were tested for setting properties, compressive strength, drying shrinkage, sulphate resistance, salt scaling, ASR mitigation and chloride diffusion characteristics according to the appropriate CSA and ASTM standards. It was found that metakaolin showed better performance in magnesium sulphate solutions than slag and that metakaolin concretes attained strength and other durability properties much faster than mixes without it. Keywords: metakaolin, ASR, sulphate, magnesium, scaling, setting, diffusion

Partial replacement of cement by metakaolin is known to improve concrete durability, by refining the pore structure to improve fluid transport properties and by reducing the alkalinity of the pore solution to make ASR less problematic. A gap exists in the literature as to the salt scaling performance and magnesium sulphate performance of metakaolin concrete. 10 concrete mixes were cast at w/cm ratios of 0.4 and 0.5. In addition to metakaolin, grade 80 slag was used as well as CSA GU cement. All replacement levels were tested for setting properties, compressive strength, drying shrinkage, sulphate resistance, salt scaling, ASR mitigation and chloride diffusion characteristics according to the appropriate CSA and ASTM standards. It was found that metakaolin showed better performance in magnesium sulphate solutions than slag and that metakaolin concretes attained strength and other durability properties much faster than mixes without it. Keywords: metakaolin, ASR, sulphate, magnesium, scaling, setting, diffusion

Efflorescence is the presence of insoluble salts upon the surface of concrete or masonry products. The aims of this project were to understand efflorescence and to evaluate metakaolin as an additive for efflorescence prevention. Computer modelling was used in order to simulate the effect of alkali upon relevant phases. Alkali was shown to depress the solubility of calcium hydroxide via the common ion effect, increase, in general, the solubility of calcium carbonate via the foreign ion effect and dramatically increase the solubility and rate of uptake of carbon dioxide into solution. The raindrop model is an attempt to simulate the processes leading to efflorescence. A raindrop falling onto a roof tile is assumed firstly to leach ions from the tile, secondly, to absorb atmospheric carbon dioxide and thirdly to precipitate calcium carbonate. The raindrop model calculates that the formation of efflorescence is primarily dependant upon leaching rather than drying effects. Sensitivity studies show that even when significant sulphate is leached, calcium carbonate remains the prevalent efflorescent phase. Metakaolin, a type of burnt clay pozzolan, had previously been cited as preventing efflorescence. However, this study showed that the performance of metakaolin is affected by the presence of micaceous and other impurity phases which are activated upon heating to metakaolinization temperatures, and readily release alkalis. This study found that the main products of metakaolin hydration in alkaline solutions are gehlenite hydrate and amorphous C-A-S-H gels. The latter was shown to absorb alkalis, particularly potassium, from solution. Results are presented of wet-dry and renewal of leachant leaching tests on two metakaolin blends and a neat OPC paste control. Wet-dry leaching, judged to be the most realistic leach test, produces leaching trends not noted in other leaching tests.

L'utilisation du kaolin calciné, sous forme de métakaolin, comme matériau pouzzolanique pour le mortier et le béton a suscité une attention considérable ces dernières années. Le travail actuel décrit les résultats d'un projet de recherche lancé pour étudier la calcination d'un kaolin local sous diverses températures (650-950°C) et durées (2, 3 et 4 heures) qui ont produit le métakaolin avec une activité pouzzolanique élevée. L'activité pouzzolanique a été évaluée par des méthodes de la chaleur d'hydratation et la résistance à la compression à 28 jours. L'activité maximale a été obtenue à une température de 850°C pendant 3 heures. Les résultats observés établissent qu'une augmentation de la chaleur d'hydratation et de la résistance à la compression a été obtenue lorsque le ciment Portland Ordinaire a été remplacé par 10% de métakaolin. L'utilisation du ciment ternaire améliore la résistance au jeune âge et à long terme. La durabilité a été également améliorée où une meilleure résistance des mortiers à l'attaque des acides a été observée. / The utilisation of calcined clay, in the form of metakaolin as a pozzolanic material for mortar and concrete has received considerable attention in recent years. The present work describes the results of a research project initiated to study the calcination of a local kaolin at various temperatures (650-950°C) and durations (2, 3 and 4 hours) to produced a metakaolin with a high pozzolanic activity. The pozzolanic activity was assessed by 28-days compressive strength and hydration heat methods. The maximum identified activity was obtained at 850°C for 3 hours duration. The observed results establish that an increase of both hydration heat and compressive strength was obtained when ordinary Portland cement was replaced by 10% metakaolin. The use of ternary blended cement improves the early age and the long-term compressive strength. The durability was also enhanced as better acidic resistance was observed.

Calcined clay and fly ash supplementary cementitious materials (SCMs) used in cement based materials were examined for their chemical and mechanical performance, as well as their pollutant interaction. This dissertation addresses three primary research questions, namely: (i) can zincite additions facilitate the use of calcined clay as SCMs by compensating for reductions in early-age mechanical performance or by compensating for their reduced pozzolanic reactivity, (ii) can cement renders, containing metakaolin calcined clays, be engineered for passive carbon dioxide and ozone removal, and (iii) how do the specific activity and emanation fractions of concrete constituents, including fly ash and metakaolin, as well as assembled concretes impact concrete radon emanation and indoor radon concentrations? The first question relates directly to the development of new, sustainable material options, which can replace a portion of cement in a concrete mixture. Results from the experiments with zincite showed that the treatment method removed the dilution effect that occurs when using less reactive materials to substitute a portion of portland cement, but did not considerably influence mechanical properties. Therefore, zincite additions are not a good means of enhancing the utilization of non-kaolinite clays in concrete. As an integrated system, the latter two questions of this dissertation investigate the interaction between airborne pollutants and the cement based materials containing SCMs. The use of SCMs in render and concrete systems resulted in different pollutant uptake and exhalation behavior, relative to non-SCM control systems. For pollutant uptake, render systems containing metakaolin increased the carbon dioxide ingress while decreasing the ozone uptake. For radon exhalation rates, modeling results demonstrated that concretes without fly ash have a higher probability of containing less total radium and lower radon exhalation rates, when compared to samples with fly ash, assuming an emanation fraction of 5%, as suggested in the literature. Experimental results demonstrated that metakaolin, fly ash and control concretes had emanation fractions of 7%, 9% and 13%, respectively, confirming that (i) an assumed fraction of 5% would underpredict indoor radon concentrations and potential health consequences, and (ii) SCMs can reduce the total concrete emanation fraction. This dissertation demonstrates how the use of sustainable material selections, such as calcined clays and fly ashes, not only influences the microstructure and mechanical performance of the cement based materials, but also alters the interaction of the material with its surrounding environment. / text

<p>Predmet ovog istraživanja je razvoj nove generacije<br />mineralnih dodataka, dobijenih termičkom i<br />mehanohemijskom aktivacijom kaolinske gline i ispitivanje<br />svojstava kompozita, u kojima je deo portland cementa<br />zamenjen dobijenim pucolanskim materijalima,<br />metakaolinom i amorfnim kaolinom, za različite režime<br />nege. Rezultati su pokazali da su termička i mehanohemijska<br />aktivacija kaolinske gline jednako pogodne metode za<br />dobijanje pucolanskih materijala. Pozitivni efekti na<br />čvrstoće pri pritisku postižu se primenom do 30 %<br />metakaolina u kompozitima pri normalnom režimu nege, a uz<br />dodatno mlevenje, sadržaj metakaolina se može povećati do<br />40 %, uz dodatak CH. Amorfni kaolin se može primeniti u<br />kompozitima, sa stepenom zamene portland cementa do 10 %,<br />pri normalnom i autoklaviranom režimu nege.</p> / <p>The subject of this research is development of a new generation<br />of mineral admixtures, obtained by thermal and<br />mechanochemical activation of kaolin clay, and testing of the<br />properties of the cement based composites, where a part of the<br />portland cement is replaced by pozzolanic materials, metakaolin<br />and amorphous kaolin, for different curing conditions. The<br />results showed that thermal and mechanochemical activation of<br />kaolin clay were equally suitable for obtaining pozzolanic<br />materials. Positive effects on the compressive strength could be<br />achieved by using up to 30 % of MK, and with additional grinding<br />after thermal activation, content of MK could be increased up to<br />40 %, with the addition of CH, under the normal curing<br />conditions. Amorphous kaolin could be used in composites with<br />a cement replacement level of 10 %, under the normal and<br />autoclave curing conditions.</p>

La nécessité de construire de manière durable, rationnelle et écologique incite à l’innovation et la recherche d’alternatives, telles que la géopolymérisation et l’activation alcaline, qui suscitent un intérêt croissant. Dans ce sens, ces technologies permettent de valorise rdes matières premières à plus faible impact environnemental pour le développement d’une nouvelle famille de matériaux. Cependant, ces mécanismes réactionnels sont complexes et il est encore nécessaire de lever plusieurs verrous avant leur implémentation : la confusion entre les deux processus, l’absence d’approches de formulation rationnelles, la méconnaissance de certaines vulnérabilités, etc. La thèse s’intègre dans cette dynamique et a pour objectif une meilleure connaissance des géopolymères et des matériaux alcali-activés. Le cadre de travail est le développement de coulis d’injection. Un programme expérimental basé sur une sélection de compositions est établi afin de caractériser leurs principales propriétés. Les différences entre les deux processus de structuration sont relevées à travers une étude physico-chimique (DRX, RMN) et liées aux évolutions macroscopiques au jeune âge. Un travail d’optimisation de formulation est mené afin de répondre à des critères d’application et définir les paramètres influençant le comportement rhéologique et mécanique des coulis. Une méthodologie basée sur l’analyse micromécanique et l’homogénéisation multi-échelles a permis d’évaluer le module élastique des matériaux et peut servir de plateforme pour une analyse globale du comportement mécanique. Enfin, une étude de la durabilité est entamée en évaluant la sensibilité au séchage et à la lixiviation en milieu acide. / The need for more durable, rational and ecological constructions encourages innovation and the search for alternatives, such as geopolymerization and alkali-activation, with a growing interest. These technologies allow the use of resources with a lower environmental impact in developing a new class of materials. However, both reaction mechanisms are complex and some issues need further investigation before a proper implementation: the confusion between these processes, the absence of a rational design approach, the lack of knowledge concerning some mechanisms of degradation, etc. The present thesis joins this dynamic and aims at a better understanding of geopolymers and alkali activated materials to design soil injection grouts. An experimental program has been established based on selected mix designs to study their main properties. The differences between both structuration processes were determined through a physicochemical study (XRD, NMR). They were correlated to the macroscopic phenomena observed at early age. An optimization of the mixtures was carried to satisfy the application criteria and define the parameters controlling the rheological and mechanical behavior of the grouts. Using a micromechanical characterization and multiscale homogenization, a methodology has been designed to determine the elastic modulus of the materials.This can be used as a first tool to analyze the global mechanical behavior. Finally, the sensitivity to drying and exposure to acid environments was assessed.

Actualmente los materiales cementicios suplementarios como el metacaolín, son comúnmente empleados en la industria cementera y de la construcción, debido a factores ambientales, económicos y técnicos. La mayoría de estudios que evalúan la influencia del metacaolín en sistemas cementicios, se enfocan en aspectos de desempeño y de resistencia mecánica, en edades avanzadas. Existen pocos estudios que evalúan la etapa inicial de hidratación. Por tanto, este trabajo tiene como propósito entender mejor la influencia que tiene la sustitución parcial de metacaolín en pastas de cemento Portland, durante las primeras 72 horas de hidratación. Normalmente para evaluar la cinética de hidratación se analiza el calor liberado, usando un calorímetro de conducción isotérmico. Sin embargo, otra técnica relativamente nueva usada en este estudio, es medir la retracción química en forma continua; en Brasil son raros los estudios que usen retracción química para obtener la cinética de hidratación. Para tal fin se elaboraron pastas utilizando reemplazos de metacaolín de 5, 10 y 20% en masa, además de una pasta de referencia, usando una relación constante agua/sólido de 0.5. La retracción química fue medida en forma continua automatizando el método de la dilatometría, también se evaluó la cinética de hidratación usando un calorímetro isotérmico. Adicionalmente, el desarrollo de los productos hidratados fue estudiado por análisis termogravimétrico y difracción de rayos X. Los resultados obtenidos muestran que existe una excelente relación entre la retracción química y la calorimetría y que la adición de metacaolín produce cambios en la cinética de hidratación, que también afectan a la retracción química. / Currently the supplementary cementitious materials such as metakaolin are commonly used in the cement and construction industry, due to environmental, economic and technical factors. Most studies evaluating the influence of metakaolin in cementitious systems focus on aspects of performance and mechanical strength at older ages. There are few studies evaluating the initial stage of hydration. Therefore, this paper aims to better understand the influence of the partial replacement of metakaolin in Portland cement pastes during the first 72 hours of hydration. Normally to evaluate the kinetics of hydration heat released is analyzed using an isothermal calorimeter. Nevertheless, another relatively new technique used in this study is to measure the chemical shrinkage continuously; in Brazil are rare studies using chemical shrinkage to obtain hydration kinetics. This study shows the influence of partial replacement of Portland cement by metakaolin in the hydration reactions and chemical shrinkage of cementitious pastes. For this, pastes were prepared using metakaolin replacements of 5, 10 and 20% by mass, and a reference paste, using a constant water/solid ratio of 0.5. Chemical shrinkage was measured continuously automating the method of dilatometry, hydration kinetics was evaluated using an isothermal conduction calorimetry. Additionally, the development of hydrated products was studied by thermogravimetric analysis and X-ray diffraction. The results show that there is an excellent relationship between chemical shrinkage and calorimetry and the addition of metakaolin leads to changes of the hydration kinetics, which also affect the chemical shrinkage.

Geopolímero é um material que possui boas propriedades físicas e químicas como resistência mecânica, resistência a ataque químico, material inerte depois de pronto, é de fácil obtenção, pois a sua base é uma argila, material abundante e de baixo custo. Muitos trabalhos são desenvolvidos com o geopolímero, como aplicações para pisos, cimentos, refratários, adesivos e isolamento acústico e térmico. O desenvolvimento do geopolímero é simples, são necessário um percussor que pode ser metacaulim ou argilas com quantidades aceitáveis de SiO2 e Al2O3, um ativador alcalino como NaOH, KOH ou silicato de sódio e aditivos se necessário para contribuir com algumas relações molares que devem ser atendidas para a formação do geoplímero. A formação do geopolímero ocorre através de reações de policondensação originando uma estrutura amorfa e até cristalina dependendo do processo. O uso de aditivos e agregados conferem características desejadas como melhor resistência mecânica, melhor capacidade de isolamento térmico ou acústico, melhor resistência química entre outros fatores. A execução foi a partir do metacaulim com o uso de NaOH e aditivos, a serragem e fibras de sisal ( algave sisalana ) para conferir maiores porosidades no geopolímero desenvolvido. O geopolímero desenvolvido gerou valores de resistência mecânica na ordem de 20 MPa em um tempo de cura de 11 dias, sua densidade variou de 1,0 a 2,5 g/ml, a porosidade volumétrica ficou na faixa de 25,0% a 47,0%, as concentrações utilizadas de NaOH foram entre 0,0 e 15,0 mol/Litro. Todos os dados foram compatíveis com dados verificados em literatura. / Geopolymer is a material that has good physical and chemical properties such as mechanical resistance, chemical etch resistance, inert material after ready, it is easy to obtain because its base is a clay, abundant material and low cost. Many jobs are developed with the geopolymer, such as floor applications, cements, refractories, adhesives and acoustic and thermal insulation. The development of the geopolymer is simple, a percussor is required which may be metakaolin or clays with acceptable amounts of SiO2 and Al2O3, an alkaline activator such as NaOH, KOH or sodium silicate and additives if necessary to contribute some molar ratios that must be met for the formation of the geoplímero. The formation of the geopolymer occurs through polycondensation reactions leading to an amorphous and even crystalline structure depending on the process. The use of additives and aggregates impart desired characteristics such as better mechanical strength, better thermal or acoustic insulation capacity, better chemical resistance among other factors. The execution was from metacaulim with the use of NaOH and additives, sawdust and sisal fibers (algae sisalana) to impart larger porosities in the developed geopolymer. The developed geopolymer generated values of mechanical strength in the order of 20 MPa in a cure time of 11 days, its density ranged from 1.0 to 2.5 gmL-1, the volumetric porosity was in the range of 25.0% to 47,0%, the concentrations of NaOH used were between 0.0 and 15.0 mol / Liter. All data were compatible with data verified in the literature.