Submitted by Luciana Ferreira (lucgeral@gmail.com) on 2015-04-27T15:25:17Z No. of bitstreams: 3 Dissertação - Sandra Kurotusch de Melo - 2010 - (1).pdf: 4813708 bytes, checksum: 1d9f47d43918bba38729e74a5014833d (MD5) Dissertação - Sandra Kurotusch de Melo - 2010 - (2).pdf: 12360828 bytes, checksum: 0c969028600897645eaa255c2ea06346 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) / Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2015-04-27T15:28:35Z (GMT) No. of bitstreams: 3 Dissertação - Sandra Kurotusch de Melo - 2010 - (1).pdf: 4813708 bytes, checksum: 1d9f47d43918bba38729e74a5014833d (MD5) Dissertação - Sandra Kurotusch de Melo - 2010 - (2).pdf: 12360828 bytes, checksum: 0c969028600897645eaa255c2ea06346 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) / Made available in DSpace on 2015-04-27T15:28:35Z (GMT). No. of bitstreams: 3 Dissertação - Sandra Kurotusch de Melo - 2010 - (1).pdf: 4813708 bytes, checksum: 1d9f47d43918bba38729e74a5014833d (MD5) Dissertação - Sandra Kurotusch de Melo - 2010 - (2).pdf: 12360828 bytes, checksum: 0c969028600897645eaa255c2ea06346 (MD5) license_rdf: 23148 bytes, checksum: 9da0b6dfac957114c6a7714714b86306 (MD5) Previous issue date: 2010-07-05 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / Delayed ettringite formation (DEF) is a special type of an internal sulfate attack with SO42- ions from cement. This process is distinguished by neoformation of ettringite in concrete thermally cured at high temperature levels and exposed to high moisture in service life. This phenomenon can promote expansion and cracking, leading to rupture and spalling, achieving severe deterioration. This research had an experimental approach with the purpose to investigate DEF in concretes with pozzolanic Portland cement containing fly ash. These concretes were undergone to temperature rise by heat of hydration. It was produced two types of pumped concrete with cement content of 350 kg/m3 and 450 kg/m3 containing basaltic aggregate. Two big specimens were cast containing 200 liters of concrete and were immediately submitted to adiabatic temperature rise tests. After that, several specimens were drilled from them in order to evaluate compressive strength and elasticity modulus, as well as microstructural investigations by scanning electron microscopy (SEM) and X Ray diffraction (XRD) along 270 days. In addition, it was cast several cylindrical and prismatic samples with concrete containing 350 kg/m3of cement. Some of them were stored at the same condition of those during the thermal cure and others were conditioned in a moist room as reference, for properties and microstructural investigation. Prismatic ones were submitted to mass variation study, ultrasonic wave tests and also expansion tests. In order to complement this experimental program, a specific study on cement pastes was performed. This involved casting three series of cylindrical samples submitted to different cure cycles followed by evaluation of mass variation, ultrasonic velocity and also microstructure investigation by SEM and XRD. Main results proved that rising internal temperature of concrete by hydration heat above 60ºC promote delayed ettringite formation by microstructural analyses, although this formation had not caused negative consequences on mechanic properties of concretes up to age of 270 days evaluated. The study on the cement pastes confirmed that high temperatures affects the microstructure of cement matrix and also the formed products, collaborating to the formation of hydrated alumina phases besides ettringite. The presence of suggestive thaumasite at advanced ages seems to indicate that this calcium silicate sulfo-carbonate hydrate can accompany DEF process. / A formação da etringita tardia - Delayed Ettringite Formation (DEF) é um tipo especial de ataque por sulfato interno, em que os íons SO42- são provenientes do cimento. O processo se distingue pela neoformação da etringita em concretos curados termicamente às elevadas temperaturas e expostos às altas umidades na etapa de serviço. Tal fenômeno pode promover expansão e consequente fissuração, culminando na ruptura e lascamento do material, levando-o à severa deterioração. Este trabalho, de caráter experimental, objetivou investigar a formação da etringita tardia em concretos de cimento Porltand pozolânico, contendo cinza volante, submetido à elevação da temperatura devido ao calor de hidratação do cimento. Para isso, foram produzidos dois concretos bombeados, contendo agregados basálticos, e com consumos de cimento de 350 kg/m3 e 450 kg/m3, com os quais foram moldados dois corpos-de-prova (CPs) de 200 litros, que foram, separadamente, submetidos aos ensaios de elevação adiabática de temperatura. Após o ciclo de cura térmica nestes ensaios, deles foram extraídos corpos-de-prova para a avaliação da resistência à compressão e módulo de elasticidade, além de investigações microestruturais por microscopia eletrônica de varredura (MEV) e difração de Raios X (DRX) durante 270 dias. Adicionalmente, foram moldadas duas séries de corpos-de-prova cilíndricos e prismáticos com o primeiro concreto, sendo que uma foi armazenada na câmara adiabática juntamente com o CP de 200 L e a outra curada continuamente em câmara úmida, servindo de referência para as análises do comportamento mecânico e investigações microestruturais dos CPs cilíndricos. Os CPs prismáticos foram utilizados para a avaliação da variação de massa, velocidade ultrassônica e expansão. Para complementar a pesquisa, realizou-se, também, um estudo específico em pastas de cimento, sendo moldadas três séries de CPs cilíndricos, que foram submetidas a três diferentes ciclos de cura seguidas por uma avaliação da variação de massa e velocidade ultrassônica, além de investigações microestruturais por MEV e DRX. Os principais resultados mostraram que o aumento da temperatura interna do concreto, acima de 60ºC, por calor de hidratação do cimento, propiciou a formação da etringita tardia, constatada pela presença de etringita neoformada durante as análises microestruturais, porém sem efeito negativo sobre as propriedades mecânicas avaliadas até a idade investigada de 270 dias. O estudo de pasta comprovou que as altas temperaturas influem na porosidade da microestrutura da matriz cimentícia e sobre o tipo de produto formado, favorecendo a formação de aluminatos hidratados ao final do ciclo térmico e da etringita durante a estocagem sob alta umidade. A sugestiva presença da taumasita, em idades mais avançadas, parece indicar que este sulfocarbonato de cálcio e sílica hidratado pode acompanhar o processo de DEF.

Fosfogesso é um resíduo sólido da produção de ácido fosfórico pelas indústrias de fertilizantes. A produção anual deste material no mundo é de cerca de 180 milhões de toneladas, e isto causa problemas com a sua armazenagem. O fosfogesso tem sido estudado para uso como material de construção de bases e sub-bases de pavimentos. O fosfogesso tem pouca durabilidade frente à ação da água quando sujeito somente à estabilização mecânica. O cimento Portland é então adicionado ao fosfogesso, resultando em misturas mais estáveis. A reação do aluminato tricálcico contido no cimento e dos sulfatos presentes no fosfogesso poderia conduzir à formação de cristais de etringita e à expansão subseqüente. O objetivo desta pesquisa é avaliar a influência do tipo de cimento na expansibilidade das misturas de fosfogesso e cimento para uso na construção de pavimentos. Analisou-se o comportamento expansivo de corpos de prova compactados com diferentes proporções de fosfogesso e cimento, variando-se o tipo de cimento, energia de compactação e período de cura. Para todos os cimentos usados nesta pesquisa, considerando-se o período de 84 dias de cura, a maior parte da expansão ocorreu nos primeiros 28 dias. A influência do tipo de cimento na expansão das misturas de fosfogesso e cimento é significante, mas o teor de aluminato tricálcico não é a única explicação para o comportamento de expansão observado neste estudo, visto que os resultados experimentais indicam que quantidades crescentes de aluminato tricálcico conduzem a menores expansões, fato que contraria a expectativa inicial desta pesquisa. / Phosphogypsum is a solid by-product resulting from the phosphoric acid process for manufacturing fertilizers. The annual worldwide production of this material is about 180 million de tons and it causes problems with its disposal. The phosphogypsum has been studied for use in pavement base and sub-base materials. Phosphogypsum has poor durability when subjected to mechanical stabilization only in wet conditions. The addition of stabilizing materials, such as Portland cement, is one method of overcoming this deficiency. The chemical reaction between tricalcium aluminate present in Portland cement and sulfate ions supplied by phosphogypsum could lead to the formation of ettringite and subsequent expansion. The objective of this research is to evaluate the influence of Portland cement type on the expansion of cement-stabilized phosphogypsum mixtures for use as pavement construction. The expansion behavior was analyzed through compacted specimens composed by different phosphogypsum and cement proportions, varying the cement type, compaction energy and curing period. For all cements used in this research, most of expansion occurred within the first 28 days in relation to the 84 days of curing. There is a significant influence of cement type on the expansion of the cement-stabilized phosphogypsum mixtures, but the aluminate tricalcium content is not the only explanation for the expansion behavior observed in this study. The experimental results show that an increasing amount of tricalcium aluminate yields lower expansion, fact that thwarts the initial expectation of this research.

Up to present, ettrigite has been prepared by two means in the Institute of Technology of Building Materials and Components of the BUT Faculty of Civil Engineering: originally by the hydration of the yeelimite clinker; recently by the direct synthesis of ettringite from calcium hydroxide and aluminum sulfate, the latter being considered more suitable in qualitative and quantitative terms. This diploma thesis focuses on the comparison of both means, using ettringite produced by the latter as control sample. This endeavor focuses on monitoring the stability of ettringite and its possible conversion to other minerals using X-ray diffraction analysis, thermal analysis and scanning electron microscopy (SEM).

The diploma thesis deals with development and properties of historic mortars, evolves and optimizes recipe of historicizing universal mortar with mixture binder, which have been evolves in previous phase. Binder system is based on lime hydrate and metakaolin and is modified with fast-pacing gypsum. Thesis follow up technological properties of mixtures of historicizing mortars and modifies them for current construction industry. It also follows effect of modification to phase composition of binder system and eventually rise of AFt phases.

This diploma thesis is focused on long term monitoring of thermodynamic stability of ettringite under selected conditions and its possible destabilization or transformation into another AFt phase, especially thaumasite. Ettringite samples were made in two ways, by hydrating the yeelimite in the system with the alite and by addition of aluminium sulphate and calcium hydroxide.

The thesis is oriented on monitoring of hydration process of portland cement based on fluidized bed ash, firstly on investigation of AFt phases, mainly ettringite and thaumasite. Specific aim of the task is to prepare the scheme of these minerals synthetic preparation and to verify their laboratory preparation by different ways, using methods of RTG-diffraction analysis and scanning electron microscopy.

The thesis deals with the development of self-leveling cement screed with compensated shrinkage. It is a ternary binder system with the majority of portland cement, that in the beginning of setting and hardening form an expandable folder ettringite. At first there was a background research of volume changes of hydrating cement composites and methods for measuring these changes. Various sort of expansion additives were also introduced, the main emphasis was on concepts of calculated formation of ettringite, which are typical for self-leveling underlayment. Background research included the issues of formation of ettringite, influences on it’s nucleation and it’s stability. The practical development of the screed began by measuring volume changes of different pastes on a ternary composition. Selected formulations suitable for use are verified together with additives to semi-application tests. After the final configuration of the screed mixture, there was a test in real application of an representative area. Individual formulations were tested in terms of long-term stability of ettringite in dry and moist environments.

Masters`s thesis deals with study of binder concept based on purposeful creation of ettringite, assessment of physic-mechanical properties and durability. The teoretical part is the mention of ettringite and his function in building materials, are described binder concepts based on purposeful creation of ettringite and self-levelling screed for which the controlled formation ettringite typical. In the practical part are did analysis of raw materials and the composition of the mixture, including types corrosive environment for the assessment of durability. In addition are checked properties of the proposed mixture and evaluated the appropriateness of use of each type of waste materials with regard to the resulting properties.

En France, les chaudières à lit fluidisé circulant (LFC) ont une vingtaine d'années d'existence. Malgré leur âge, l'intérêt de leur système de désulfuration des fumées est amoindri du fait de la difficulté à valoriser les cendres qu'elles produisent. A l'heure actuelle, les voies de valorisation envisageables pour ces co-produits sont faiblement consommatrices de cendre et la filière du génie civil, c'est-à-dire la confection de ciment et de béton, leur reste inaccessible. Ces travaux de thèse visent à démontrer que sous réserves de plusieurs précautions, il est possible et même intéressant de confectionner un ciment contenant la cendre volante LFC. Du point de vue minéralogique, les cendres volantes LFC se différencient clairement des cendres volantes silico-alumineuses issues des chaudières à charbon pulvérisé (CP) normalisées par la présence de minéraux argileux, proches de ceux contenus dans les combustibles. A l'aide de la diffraction des rayons X et d'un logiciel de traitement de données par méthode de Rietveld, plusieurs couples de combustible et de cendre ont été caractérisés afin d'étudier leur filiation minéralogique. Du point de vue chimique, le système de désulfuration des chaudières LFC conduit à une grande diversité de composition chimique, de par l'ajout en quantité variable d'une fraction sulfo-calcique aux résidus silico-alumineux de la combustion des charbons. Cette fraction, constituée d'anhydrite et de chaux vive, est le principal frein à la valorisation de la cendre dans la filière du génie civil. Que la cendre soit hydratée seule ou en mélange avec du ciment, son anhydrite conduit à la formation d'ettringite, hydrate responsable de désordres dans la pâte de ciment. Les travaux de thèse eurent comme objectif d'étudier ce phénomène, en tâchant de le relier aux variations dimensionnelles de mortier et de béton. Au final, nos résultats dressent une liste de spécifications, suffisantes pour rendre réalisable la confection d'un ciment composé destiné à une utilisation industrielle. De plus, des essais mécaniques montrent que la nature physique, chimique et minéralogique de la cendre constitue un avantage en terme de résistance mécanique pour confectionner des ciments composés. En détaillant les principaux facteurs qui influencent le gonflement ettringitique et en apportant un nouvel éclairage sur la nature minéralogique de la cendre, cette étude pourrait aider, à terme, à la prise en compte de cette addition minérale dans les normes relatives à la confection de ciment et de béton.

Os investimentos iniciais em moldes na indústria de pré-moldados de concreto de cimento Portland, em geral, são altos, havendo a necessidade de utilizá-los o mais intensivamente possível entre uma e outra moldagem. A conseqüência é que a desforma pode ocorrer em instantes inadequados, comprometendo a durabilidade do produto. Isto contraria o conceito fundamental da pré-moldagem que está relacionado ao rigoroso controle de qualidade do produto. A cura térmica é uma alternativa, pois é utilizada para acelerar a resistência mecânica inicial do concreto. Esse beneficio imediato é acompanhado por uma redução na resistência final comparativamente à cura normal em câmara úmida. Esta redução é atribuída ao desenvolvimento de uma microestrutura modificada. Para investigar esse fenômeno, com base nos conhecimentos em ciência e engenharia dos materiais, desenvolve-se um estudo experimental, aplicado a pré-moldados com pequena espessura. O objetivo principal é analisar tais modificações e os compostos hidratados, formados ao longo do tempo após a cura térmica, considerando os materiais empregados e estabelecendo relações com a perda de resistência final. Leva-se em conta a influência das adições e da duração dos ciclos térmicos. A análise da microestrutura está baseada nos seguintes ensaios: porosimetria por intrusão de mercúrio, microscopia eletrônica de varredura, termogravimetria e difração de raio-X. Confirma-se com base nos resultados que a cura térmica favorece a maior formação de portlandita e também acelera a reação pozolânica. Para a composição entre cimento Portland, a escória de alto forno (30%) e a sílica ativa (10%), submetidas a ciclos térmicos longos (12 horas Tmax=61°C), observa-se a maior perda na resistência mecânica a longo prazo. Neste caso, há fortes indícios de que há formação de fases com menor desempenho mecânico. Através de micrografias, para essa amostra, sugere-se a formação da etringita secundária com maior prejuízo na interface pasta-agregado. As conclusões sugerem que para minimizar as interferências no processo de cura e garantir resistências mínimas nas desmoldagens rápidas, com poucas perdas a longo prazo, é interessante associar ciclos térmicos curtos, cimento de alta resistência inicial, sílica ativa e superplastificante. / The initial investments of molds in the industry which makes pre-cast of Portland cement concrete is usually very high, thus creating a necessity to maximize the utilization of each moldings. The consequence is that the forms can be removed at inadequate time, which compromise the durability of the product. This contradicts the fundamental concepts of the pre-castings, which is related to a severe quality control. Steam curing is an alternative treatment and is used to accelerate the initial mechanical resistance of the concrete. This immediate benefit is accompanied by the decrease on final resistance compared to normal curing in humid chamber. This reduction is attributed to the development of a modified microstructure. To investigate this phenomenon, based on knowleledge of materials science and engineering, an experimental study is developed which is applied in pre-cast wich small thichness. The main objective of this work is to analyze the microstructure modifications and the hydrated compounds formed, after a period of steam curing, taking in account the used materiaIs, also to establish a relations with the loss of final strength. The influence of additions and duration of steam cycles are considered. The analyses of microstructures are based on the following tests: mercury intrusion porosimetry, scanning electron microscope, thermogravimetry and X-ray diffraction. Based on the results it can be confirmed that steam curing favors a large formation of ponlandite and also accelerates pozzolanic reaction. For the composition of Portland cement, slag fumace blast (30%) and active silica (10%), submitted for long period of thermal cycles (12 hours, Tmax=61°C), a great loss strength was observed. In this case it is possible the formation of phases with poor mechanical performance. Through micrographs, for this sample, it is observed the formation of secondary ettringite with a large damage in the interface aggregate-paste. The conclusions suggest that to minimize the interference in the process of curing and to guarantee a minimum strength during the rapid separation of the concrete from the molds, with a minor loss in a long term, it is interesting to associate short steam cycles, high initial resistance cement, adive silica and superplasticizer.