Orientadores: Antonio Ludovico Beraldo, Holmer Savastano Júnior / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Agrícola / Made available in DSpace on 2018-08-21T10:15:51Z (GMT). No. of bitstreams: 1 Rodrigues_MichelleSantos_D.pdf: 5803870 bytes, checksum: c6cbc3e5bb60178760286846f51dffb6 (MD5) Previous issue date: 2012 / Resumo: Neste trabalho produziram-se cinzas de palha de cana-de-açúcar por queima controlada para avaliar a sua aplicação como adição mineral em matrizes cimentícias. As palhas foram submetidas a quatro diferentes temperaturas de queimas: 600 °C, 700 °C, 800 °C e 900 °C, e as cinzas foram denominadas CPCA600, CPCA700, CPCA800 e CPCA900, respectivamente. Após a queima cada cinza passou por um processo de moagem e foi submetida a análises de fluorescência de raios X, difração de raios X, microscopia eletrônica de varredura, granulometria a laser, massa específica real por picnometria a gás e superfície específica por B.E.T (Brunauer-Emmett-Teller). A reatividade das cinzas foi avaliada por meio de medições de condutividade elétrica em soluções insaturadas de Ca(OH)2/cinzas. Foram analisadas pastas com cimento Portland ou hidróxido de cálcio em função da idade de cura úmida (7, 28, 63 e 91 dias) por meio das técnicas de termogravimetria, compressão simples, compressão diametral, absorção de água, porosidade aparente, massa específica aparente, porosimetria por intrusão de mercúrio, microscopia eletrônica de varredura, calorimetria e difração de raios X de alta resolução, realizada no Laboratório Nacional de Luz Síncrotron. As cinzas CPCA600 e CPCA700 foram consideradas mais reativas e foram aplicadas em compósitos de fibrocimento. As caracterizações das cinzas mostraram que a CPCA600 e a CPCA700 contêm composição química de material pozolânico, partículas com elevada nano e microporosidade e elevadas áreas de superfície específica, assim como foi observado um halo de amorficidade nos difratogramas de ambas as cinzas. O ensaio de condutividade elétrica no sistema hidróxido de cálcio/cinzas mostrou elevada reatividade dessas cinzas. Na avaliação das pastas, as cinzas CPCA600 e CPCA700 apresentaram maior consumo de hidróxido de cálcio, maior resistência à compressão simples e menor volume de poros. As caracterizações físicas (absorção de água, porosidade aparente e massa específica aparente) e mecânicas (módulo de ruptura, energia específica, módulo de elasticidade e limite de proporcionalidade) dos compósitos mostrou que aqueles produzidos com a CPCA700 apresentaram características físicas e mecânicas similares àquelas do controle, o que viabiliza a substituição parcial do cimento Portland pela mesma / Abstract: This research work produced sugarcane straw ashes by controlled burning and evaluates its application as mineral admixture in cementitious matrices. Straws were subjected to four different burning temperatures. Straws were dried and burned at 600 °C, 700 °C, 800 °C and 900 °C that were named SCSA600, SCSA700, SCSA800 and SCSA900, respectively. After firing the material passed through a milling process and it was subjected to analysis of X ray fluorescence, X ray diffraction, scanning electron microscopy (SEM), particle size laser, real density and specific surface area by B.E.T (Brunauer-Emmett-Teller). The reactivity evaluation of the ashes was performed by measuring the electrical conductivity of insaturated solutions of Ca(OH)2/ash. Pastes with Portland cement or calcium hydroxide were evaluated according to the curing hydration age (7, 28, 63 and 91 days) by means of thermogravimetry, compressive strength, splitting test, water absorption, apparent porosity and bulk density, mercury intrusion porosimetry, scanning electron microscopy, calorimetry and high-resolution X-ray diffraction, at the National Laboratory of Synchrotron Light. The ashes SCSA600 and SCSA700 were considered more reactive and have been applied in cement composite. The characterizations show that SCSA600 and SCSA700 ashes contain chemical composition of pozzolanic material, and nano particles with high microporosity, and consequently, with high specific surface areas, as has been observed halo amorphicity in both diffractograms ashes. Electrical conductivity obtained at the system calcium hydroxide/ashes showed high reactivity for these ashes. In the pastes evaluation, the ashes SCSA600 and SCSA700 showed higher consumption of calcium hydroxide, higher compressive strength and reduced volume of pores. The physical characterizations (water absorption, apparent porosity and bulk density) and mechanical (modulus of rupture, specific energy, elastic modulus and proportionality limit) of the composites showed that those produced with the ash SCSA700 were similar to the control ones, which enables the partial replacement of Portland cement by this kind of ash / Doutorado / Construções Rurais / Doutora em Engenharia Agrícola

Neste trabalho, por meio de uma metodologia experimental foram analisados vários aspectos de tijolos modulares compostos por misturas binárias e ternárias de solo-cimento e solo cimento-sílica produzidos em prensa manual modelo SAHARA, com a finalidade de se obter parâmetros e diretrizes que visam um melhor desempenho do material. Realizaram-se ensaios em corpos-de-prova cilíndricos de maneira acessória no decorrer do trabalho, o que resultou no suporte para fundamentação de diversas avaliações sobre as composições de traços utilizados na fabricação dos tijolos. Foram executados painéis de parede com o objetivo de verificar o comportamento da alvenaria em relação à resistência à compressão e à deformabilidade das paredes, possibilitando correlações com os resultados dos ensaios de prismas, tijolos e argamassa de assentamento. As contribuições da pesquisa permitem relacionar a tecnologia da fabricação de tijolos de solo-cimento com o contexto de construção sustentável e o aproveitamento de resíduos industriais, além de sistematizar informações para a elaboração de um projeto tecnológico com os tijolos modulares / In this work, several aspects of modular bricks composed by binary and ternary mixtures of soil-cement and soil-cement-silica, produced by manual press model SAHARA, were analyzed by means of an experimental methodology, with the purpose of obtaining parameters and guidelines to aim a better performance of the material. During the work, tests in cylindrical samples were executed in an accessory way, what resulted in the support for theoretical basement of several evaluations about the compositions of proportions used in brick's production. Wall panels were constructed with the objective of verifying the masonry’s behavior in relation to the compressive strength and wall’s strain, promoting correlation with the test’s results in prisms, bricks and mortar. The research’s contributions allow to relate the technology of the production of soil-cement bricks with the context of sustainable construction and the use of industrial residues in the production of construction materials, besides systematizing information for the elaboration of a technological project with the modular bricks

Orientador: Darcy Flavio Nouer, Simonides Consani / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Odontologia de Piracicaba / Made available in DSpace on 2018-08-02T02:37:45Z (GMT). No. of bitstreams: 1 Valdrighi_HeloisaCristina_D.pdf: 2776014 bytes, checksum: e51a23872c56c05e6ae98411da802807 (MD5) Previous issue date: 2002 / Resumo: O objetivo desta pesquisa foi avaliar a resistência ao cisalhamento da resina composta e do cimento de ionômero de vidro na fixação de diferentes tipos - de bráquetes metálicos (Morelli, Abzil-Lancer, Dentaurum e GAC). Foram utilizados 120 pré-molares humanos. As faces vestibulares de 80 prémolares receberam condicionamento ácido e os bráquetes foram fixados utilizando Concise Ortodôntico e Transbond XT, enquanto em outros 40 prémolares, os bráquetes foram fixados com Fuji Ortho LC. As amostras foram armazenadas em solução de soro fisiológico a 0,9% a 37°C por 24 horas. Em seguida, foram submetidas ao teste de resistência ao cisalhamento em uma máquina Instron, com velocidade de 0,5mm/min. Os resultados foram submetidos à análise de variância e ao teste de Tukey (p<0,05). Associando sistemas adesivos aos respectivos bráquetes, os resultados mostraram que: a) com o Concise ortodôntico, a resistência (kgf/mm 'POT. 2¿)do bráquete GAC (1,698) foi significantemente maior que os bráquetes Abzil-Lancer (1,353), Dentaurum (1,293) e Morelli (0,828), que apresentou a menor média; b) com o Transbond XT, observou-se que os bráquetes Dentaurum (1,082) e GAC (1,225) apresentaram médias significantemente maiores do que os bráquetes Morelli (0,583) e Abzil-Lancer (0,621); e, c) com o Fuji Ortho LC, não foram observadas diferenças entre as médias dos diferentes bráquetes testados (Morelli=0,301, Abzil-Lancer=0,309, Dentaurum 0,230 e GAC=0,338). Os autores concluíram que o Concise Ortodôntico apresentou maiores valores de resistência ao cisalhamento, seguidos do Transbond XT e Fuji Ortho LC. O bráquete GAC apresentou maior resistência em todos os materiais e o bráquete Morelli a menor resistência / Abstract: The aim of this study was to evaluate the shear bond strength of composites and glass ionomer cement of different metallic brackets bonding (Morelli, Abzil-Lancer, Dentaurum e GAC). One hundred and twenty human premolars were used. For eighty premolars, the vestibular faces were etched and were bonded to enamel surface using Concise Ortho and Transbond XT, whereas in others forty premolars the brackets were bonded with Fuji Ortho LC in the vestibular faces without acid etching. All samples were stored in fisiologic solution 0,9% at 37°C for 24 hours. Afier the sample were submitted to shear bond strength in an Instron at a crosshead speed of 0.5 mm/min. The results were submitted to ANOVA and Tukey's test (p<0.05). Associating adhesives systems to respective brackets, the data indicated that: a) with Concise Ortho, the strengths (kgt/mm¿POT. 2¿) of GAC bracket (1.698) was significant1y higher than Abzil-Lancer (1.353), Dentaurum (1.293) and Morelli (0.828) brackets; b) with Transbond XT, Dentaurum (1.082) and GAC (1.225) brackets showed average higher than Morelli (0.583) and Abzil-Lancer (0.621); and, c) with Fuji Ortho LC, it wasn't showed difference between the average of different brackets tested (Morelli=0.301, Abzil-Lancer=0.309, Dentaurum 0.230 and GAC=0.338). The authors concluded that the Concise Ortho showed highest shear bond strength values followed by Transbond XT and Fuji Ortho LC. The GAC bracket showed higher strength in alI adhesives systems and the Morelli bracket the lowest strength / Doutorado / Doutor em Ortodontia

Low level nuclear waste arising from UK nuclear sites, research establishments, hospitals and industry is currently disposed of at the Drigg Disposal Facility in Cumbria. Waste is packed into steel canisters before being compacted and grouted into larger steel storage containers. The aqueous chemistry of wastes, especially radionuclides, in the presence of grout material is of major interest. The gout used at the Drigg site is a mixture of Ordinary Portland Cement and Pulverised Fly Ash additive, from which ingressing water will leach high levels of calcium, sodium and potassium and produce waters of a high pH. Aerobic environments are expected to dominate over the early period of the vault life, after which the combined effect of canister corrosion and microbial activity will lead to anaerobic conditions. After a much longer period (100,000 years) anaerobic conditions may cease and yield once again an aerobic environment where migration of radionuclides may be sorption-controlled rather than on hydroxide precipitation at high pH. Work has been performed under both aerobic and anaerobic conditions to study uranium solubility in the presence of complexing ligands that may be present in the waters of the nearfield of a low-level waste disposal vault. Eleven ligands have been investigated: carbonate, phosphate, chloride, sulphate, acetate, citrate, EDTA, NTA and organic matter- humic acid, fulvic acid and iso-sacchannic acid. Anaerobic conditions were achieved by two different procedures; the first used ferrous ions in hydroxide solution and the second used dithionite in hydroxide solution. Both methods produce reducing electrode potentials and high pH. Computer software has been used to model experimental results, thereby predicting uranium solubilities and speciation, and to propose new formation constants to fit the experimental results more closely. Studies have also been perforined to measure uranium sorption by grout material at high pH in the presence of the above ligands. This work makes a significant contribution to the understanding of uranium solubility and speciation in waters. at high pH and under conditions relevant to low level nuclear waste disposal.

Heat of hydration is a property of Portland cement and a direct result of the chemical reaction between cement and water. The amount of heat released is dependent upon the cement mineralogical composition, curing temperature, water to cement ratio, and cement fineness. High temperature resulting from heat of hydration (thereon referred to as HOH) of cement can affect the hydration process, and consequently the kinetics of development of the mechanical properties of concrete. One of the main reasons triggering the interest in HOH of cement is its implication in thermal cracking of concrete. The high temperature gradient between the inner core and the outer surface of a concrete element is known to result in large tensile stresses that may exceed tensile strength, thus leading to early–age thermal cracking in mass concrete. This dissertation initially addresses accurately predicting the heat of HOH of Portland cement at seven days based on the heat flow data collected from isothermal calorimetry for a time interval of 0-84 h. This approach drastically reduces the time required to identify the seven day HOH of Portland cement. The second part of this study focuses on cement fineness and its critical role on the heat generated by Portland cement during hydration. Using a matrix of four commercially available Portland cements, representing a wide range of mineralogical composition, and subjecting each of the as-received cements to several grinding increments, a linear relationship was established between cement fineness and heat of hydration. The effect of cement fineness and mineralogical composition on HOH of Portland cement was then related through a mathematical expression to predict the HOH of Portland cement based on its mineralogical composition and fineness. Three expressions were proposed for the 1, 3 and 7 day HOH. The findings indicate that the equations developed, based on cement main phase composition and fineness, can be used to identify cements with high heat of HOH that may cause thermal cracking in mass concrete elements. Also, the equations can be used to correlate the HOH with the other properties of Portland cement for quality control and prediction of chemical and physical properties of manufactured Portland cement and concrete. Restrained shrinkage experiments results on mortar specimens prepared with cements of variable phase composition and fineness indicate that interaction of C3A and sulfate source is the prime phenomenon followed by cement fineness as the second main factor influencing concrete cracking. In order to minimize this effect, the third part of this study focused on studying alternatives that can lower the heat generated by concrete on hydration through the incorporation of nanomaterials; namely, graphene nanoparticles. The results indicate that incorporation of graphene a as replacement for Portland cement improves thermal diffusivity and electrical conductivity of the cement paste. Consequently, the use of graphene can trigger improvement of the thermal conductivity of concrete elements thus reducing the cracking potential of concrete. Measurements of HOH of graphene-cement paste, at w/c=0.5, using isothermal conduction calorimetry, indicate that incorporation of graphene up to 10% increases the length of the induction period while reduces the magnitude of the alite main hydration peak due to the filler effect. Furthermore, increasing the w/c ratio from 0.5 to 0.6 and graphene content from 1 % to 10% (as a partial replacement of cement) increases the 7 day HOH of Portland cement by 50 J/g. Isothermal conduction calorimetry heat flow curves show that incorporation of graphene particles up to 10% does not have significant effect on interaction of aluminates and sulfates sources since the time of occurrence of the C3A sulfate depletion peak is not affected by graphene substitution up to 10%. Full factorial statistical design and analysis conducted on compressive strength data of mortar specimens prepared at two w/c ratios, using cements of different finenesses and graphene content indicates that the quantity of graphene and the physical interaction due to variable w/c, graphene and cement fineness, have the smallest P-value among all the samples, representing the most significant impact on compressive strength of mortar samples. It appears that in graphene cement paste composites, addition of 1% graphene results in 21% reduction of Young’s modulus. Increasing the graphene content from 1% to 5% and/or 10% does not show significant effect on Young’s modulus. Similar trends can be observed in the hardness of graphene cement paste samples. In conclusion, partial replacement of Portland cement with graphene nanoparticles in concrete mixtures is a good alternative to lower the cracking potential in mass concrete elements.

Two different research projects were investigated for this thesis, which has consequently been presented in two parts. PART 1 An attempt has been made to improve the high temperature performance of phenol-formaldehyde thermosets by modification of their structure with inorganic phosphate groups. Transesterification of tri-phenyl phosphate with resorcinol has given a resorcinol phosphate resin, which cured with hexamethylenetetramine. A pilot scale batch of this resin has been made and used in high temperature stability studies. Post-cured resorcinol phosphate resin-chrysotile asbestos (30: 70) moulded bars retained 59.5% of their flexural strength after ageing at 523K for 1000 hr in air. Similar phenol-formaldehyde composite bars aged under identical conditions retained only 5.3% of their initial flexural strength. The utility of the resorcinol phosphate resin composite as a commercial product is limited, since the bars had a much lower initial flexural strength (30.85 MNm-2) than the phenol-formaldehyde resin composite bars (108.5 MNm-2). Thermogravimetry and isothermal heating studies have indicated that the degradation of resorcinol phosphate resin was greatly accelerated by chrysotile asbestos, which may catalyse a bond re-organisation process that has been tentatively proposed as a mechanism for the fragmentation of the resin. PART 2 Recently an ionomer dental cement (ASPA), prepared from aqueous poly(acrylic acid) and an ion-leachable aluminosilicate glass, has been developed. The system has been extended by studying other aqueous polymers. The factors influencing the gelation and the properties of the set cements have been examined. Poly(carboxylic acids) with hydrophobic, or no pendant substituents were found to be the most satisfactory polymers for preparing water stable cements. To study the influence of the nature of the cation and polymer structure on the gelation and water stability of ionomer cements, a wide range of metal oxide-polyacid products have been studied. The formation of water stable cements depended markedly on the type of oxide and polyacid employed and appeared to involve factors such as the co-ordination geometry and radius of the cation and the nature of the cation-polyanion bonding in the matrix. A comparison between the water stabilities of ASPA cement and poly(acrylic acid)-CaO, Al2O3, or Al(OH)3 cements has shown that the chemistry of ASPA cement is more complex than has been hitherto reported. Stability constants have been determined for Ca 2+ and Cd 2+ with poly(acrylic acid) and ethyl ethylene-maleic acid copolymer by a potentiometric titration method developed by Gregor and modified by Mandel and Leyte. The stability constants obtained in 1.0M NaNO3 at 298.2 ± 0.2K were: for poly(acrylic acid), with Cat2+, log b1 Ca2+ PAA ~ -3.35 with Cd2+, log Bav Cd2+ PAA = -2.30 for ethylene-maleic acid copolymer, with Cat2+, log b1 CA2+ EMA ~ -4.05 with Cd2+, log Bav Cd2+ EMA = -1.95 The log b1 values probably had little precise meaning, although to a first approximation, log b1 Ca2+ PAA > log b1 Ca2+ EMA The determined stability constants have been used with limited success in predicting the water stabilities of the corresponding metal oxide-polyacid cements.

Depuis la fin du 20ème siècle, notre société a pris conscience que la protection de l’environnement et le développement durable sont nécessaires à notre épanouissement futur. Des directives ont contraint les pouvoirs publics, les collectivités, ainsi que les industriels à réagir notamment en s’impliquant dans la recherche. Les cimentiers sont aussi concernés. La fabrication du ciment nécessite énormément de matières premières.L’objectif principal de cette thèse est donc de valoriser les sous-produits industriels en matériaux cimentaires. Le contexte et la problématique des déchets sont abordés, ainsi que la possibilité de valorisation par les ciments. La méthodologie mise en place et son originalité sont expliqués. Dans un premier temps, le protocole de caractérisation des déchets minéraux a été développé et les résultats en laboratoire sont prometteurs pour le remplacement du calcaire et de l’argile dans le cru d’un ciment. Les cuissons en laboratoire ont permis d’obtenir un ciment comportant les 4 phases d’un Portland. La synthèse en plus grande quantité d’une formulation en laboratoire a mis en évidence de bonnes performances mécaniques sur mortiers au jeune âge. Dans un deuxième temps, les meilleures formulations ont été testées à l’échelle industrielle, dans le four de ARF. Le cru, malaxé par trémies agitatrices, a été une réussite. Enfin, l’immobilisation des polluants dans une matrice cimentaire des résidus de combustion, provenant des combustibles secondaires de ARF a permis de déclasser le déchet stabilisé/solidifié par réduction granulométrique du matériau avant tabilisation/solidification. / Since 20th century’s end, our society started to take conscience of environmental protection and sustainable development are required to our future blooming. Directives have obliged public authorities, communities, such as industry to be reacted particularly while being implied in research. The cement-manufacturers are also concerned. The process cement-manufacturer requires large quantities of raw materials. The main objective of the thesis is to value industrial by-products by cementitious materials. Context and problem of wastes were discussed, as well as the possibility of valorization such as the cements. The methodology set up for the thesis and its originality are explained. First, the protocol of characterization of mineral wastes was developed. The results in laboratory are promising for the replacement of limestone and clay in the cement’s raw meal and different formulations. The cookings in laboratory allowed obtaining a cement containing 4 phases of Portland. The synthesis in bigger quantity of a formulation in laboratory highlighted good mechanical performances on mortars at the young age. In a second stage, the best formulations were tested on an industrial scale in the ARF’s kiln. The raw meal, mixed by hoppers agitators, was a success. Finally, immobilization of pollutants in a cement matrix of the residues after combustion, resulting from secondary fuels of ARF, was studied to be able to downgrade the waste stabilized/solidified by grading reduction of the material before stabilization/solidification.

La cimentation est une étape cruciale de la construction d'un puits de pétrole, qui vise à garantir l'isolation des différentes zones du puits. La couche protectrice de ciment s'hydrate dans des conditions extérieures de température et de pression qui peuvent varier largement selon les cas, et une mauvaise maîtrise de cette hydratation peut provoquer des déformations internes qui compromettent l'efficacité de la cimentation. On s'intéresse ici à un modèle industriel prédictif de l'évolution d'un annulaire de ciment, qui combine un système d'équations retranscrivant l'hydratation du matériau d'un point de vue thermochimique et un algorithme de calcul viscoélastique vieillissant faisant appel à la poromécanique pour décrire les contraintes et les déformations internes selon un mécanisme de pression capillaire. Ce modèle fait un certain nombre d'hypothèses simplificatrices, nécessaires au vu de la myriade de paramètres importants dans la modélisation du retrait d'hydratation. On s'interroge ici quant aux domaines de validité de ces hypothèses ainsi qu'à la pertinence des jeux de paramètres choisis. Pour ce faire, il a été décidé de comparer des résultats de simulation obtenus avec notre algorithme dérivé du modèle initial et des résultats expérimentaux de mesures d'hydratation et de déformations avec et sans contraintes extérieures. La réaction d'hydratation a été étudiée par des mesures standard comme la calorimétrie ainsi que par résonnance magnétique nucléaire. Cette méthode est relativement récente dans le domaine des matériaux cimentaires en comparaison des autres et possède des avantages pour les suivis d'hydratation à long terme ainsi que pour une détection précise de la prise du matériau sans recours à une sonde mécanique. Les mesures mécaniques ont permis d'étudier le matériau à plusieurs âges et avec plusieurs températures de cure afin de mesurer les courbes d'évolution des modules mécaniques avec le degré d'hydratation. Ces essais regroupent des tests statiques utilisant une presse, permettant de mesurer les propriétés élastiques, ainsi que des essais de fluage et des mesures par un analyseur visco-dynamique afin de mesurer le comportement viscoélastique. Enfin, une analyse critique de certains des choix faits dans le travail de modélisation a été proposée avec des pistes pour améliorer la précision des résultats au jeune âge, à la fois en termes de degré d'hydratation comme de fluage à court terme / Cementing is a crucial step of the construction phase of an oil well, which aims at ensuring zonal isolation between the different parts of the well and the environment. The protective cement annulus hydrates in external conditions of temperature and pressure that can vary widely from one job to another, and poor control of the hydration phase can lead to autogenous shrinkage that reduces the effectiveness of the cementing. In this work, we investigate an industrial predictive model for the evolution of a cement annulus, which combines a thermochemical system describing the cement hydration at the macroscopic scale and an aging viscoelastic system including poromechanics to describe the stress and strain resulting of a capillary pressure mechanism. This model makes a number of simplifying hypotheses that are necessary considering the large amount of important parameters used in the modeling of hydration shrinkage. The range of validity of these assumptions has been investigated, as well as the relevance of the selected parameters used in the model. In this scope, it has been decided to compare simulation results obtained with our algorithm derived from the original model with experimental results of hydration and of deformations obtained with external loading or caused by internal stresses. The hydration reaction was studied by standard calorimetric measurements as well as by nuclear magnetic resonance. This method is relatively new in the field of cementitious materials in comparison with other methods and offers several benefits for following long-term hydration as well as for accurate detection of the setting time of the material without requiring mechanical probing. The mechanical measurements were used to examine the material at various ages and with various curing temperatures to measure the evolution curves of mechanical modules with degree of hydration. These tests include tests using a static press, to measure the elastic properties and creep tests as well as dynamic mechanical analyzer tests to measure viscoelastic behavior. Finally, a critical analysis of some of the choices made in the modeling work has been proposed with suggestions to improve the accuracy of simulations at early age, both in terms of degree of hydration as of short-term creep strains

Cette thèse a pour objet la mesure de déformations sans contact lors d'un essai de traction à l'aide de la méthode de corrélation d'images numériques DIC (Digital Image Correlation). Cette technologie utilise le repérage d'un motif aléatoire de tachetures pour mesurer avec précision les déplacements sur une surface donnée d'un objet subissant une déformation. Plus précisément, un algorithme DIC plus efficace a été formulé, appliqué et validé. La présente thèse comporte cinq parties consacrées au développement et à la validation du nouvel algorithme DIC: (a) la formulation mathématique et la programmation, (b) la vérification numérique, (c) la validation expérimentale, par essai de traction, en comparant les mesures DIC à celles obtenues par des jauges de déformation, (d) l'étude d'un procédé d'atomisation novateur pour générer de façon reproductible le motif de tachetures pour un repérage plus exact, et (e) l'analyse des sources d'erreur dans les mesures DIC. Plus précisément, l'algorithme DIC a servi à analyser, à titre d'exemple d'application, les propriétés mécaniques du polyméthyl métacrylate utilisé pour la reconstruction du squelette. Avec l'algorithme DIC, les images d'un objet sont acquises pendant la déformation de celui-ci. On applique ensuite des techniques d'optimisation non linéaire pour suivre le motif de tachetures à la surface des objets subissant une déformation en traction avant et après le déplacement. Ce procédé d'optimisation demande un choix de valeurs de déplacement initiales. Plus l'estimation de ces valeurs de déplacement initiales est juste, plus il y a de chances que la convergence du processus d'optimisation soit efficace. Ainsi, cette thèse présente une technique de traitement novatrice reposant sur une logique floue incluant aussi l'approximation des valeurs initiales du déplacement pour démarrer un processus itératif d'optimisation, ayant pour résultat une reproduction plus exacte et efficace des déplacements et des déformations. La formulation mathématique du nouvel algorithme a été développée et ensuite mise en œuvre avec succès dans le langage de programmation MATLAB. La vérification de l'algorithme a été faite à l'aide d'images de synthèse simu­lant des déplacements de corps rigides et des déformations de traction uniformes. Plus particulièrement, les images de déplacement simulaient (1) des déplacements de 0, 1 - 1 pixel en translation, (2) des angles de rotation de 0, 5 - 5°, et (3) de grandes déformations en traction de l'ordre de 5000 à 300000µE déformation, respectivement. Les processus de vérification ont démontré que le taux d'exactitude du nouvel algorithme DIC est supérieur à 99% en ce qui concerne les mesures des différents types et niveaux de déplacements simulés. Une validation expérimentale a été menée afin d'examiner l'efficacité de la nouvelle tech­nique dans des conditions réalistes. Des échantillons de PMMA normalisés, respectant la norme ASTM F3087, ont été produits, inspectés et soumis à une charge de traction jus­qu'à la rupture. La déformation de la surface des échantillons a été mesurée au moyen (a) du nouvel algorithme DIC, et (b) des techniques utilisant des jauges de déformation de type rosette. La force maximale moyenne et la limite de résistance mécanique des quatre échantillons étaient de 880 ± 110 N et 49 ± 7 MPa, respectivement. La limite moyenne de déformation mesurée par la jauge de déformation et provenant de l'algorithme DIC étaient de 15750±2570 et 19890±3790 µs déformation, respectivement. Des déformations d'un tel ordre sont courantes pour les matériaux polymériques, et jusqu'à maintenant, la technique DIC n'n’était pas développée pour faire des mesures de déformations aussi importantes. On a constaté que l'erreur relative de la mesure DIC, par rapport à la technique de la jauge de déformation, s'élevait à 26 ± 8%. Par ailleurs, le module de Young moyen et le coefficient de Poisson moyen mesurés en utilisant des jauges de déformations étaient de 3, 78 ± 0, 07 G Pa et 0, 37 ± 0, 02, alors qu'ils étaient de 3, 16 ± 0, 61 GPa et 0, 37 ± 0, 08, respectivement lorsque mesurés avec l'algorithme DIC. L'écart croissant entre les mesures de déformation DIC et celles obtenues au moyen de jauges de déformation est probablement lié à la dis­torsion graduelle du motif de tachetures à la surface des échantillons de traction. Par la suite, on a introduit un facteur de correction de 1, 27 afin de corriger l'erreur systématique dans les mesures de déformation provenant de l'algorithme DIC. La limite de déformation des mesures DIC a été rajustée à 15712±357 µs déformation avec un taux d'erreur moyen relatif de -0, 5 ± 7, 1 %, comparé aux déformations mesurées par la jauge de déformation. Le module de Young moyen et le coefficient moyen de Poisson de l'algorithme DIC et des mesures obtenues par la jauge de déformation ont par ailleurs été rajustés à 3, 8 ± 0, 4 GPa et 0, 368 ± 0, 025, respectivement. Au moyen d'un procédé d'atomisation, des taches de peinture ont été générées de façon reproductible sur la surface d'un objet. Une approche expérimentale de planification facto­rielle a été utilisée pour étudier le motif de tachetures (répartition et gradient de l'échelle des tons de gris) pour mesurer l'exactitude de l'algorithme DIC. Plus particulièrement, neuf motifs de tachetures différents ont été générés au moyen du procédé d'atomisation et testés pour la translation et la rotation de corps rigides. Les résultats ont révélé que l'erreur moyenne relative parmi les neuf motifs de tachetures variait de 1, 1 ± 0, 3% à -6, 5 ± 3, 6%. Le motif de tachetures préféré, lequel se démarquait par une large gamme de taches claires et de valeurs de tons de gris, a produit une erreur relative de 1, 1 ± 0, 3%. Une analyse des erreurs et des sources d'erreurs relatives de la mesure de l'algorithme DIC a été menée. Ti-ois catégories de sources d'erreurs, incluant l'algorithme lui-même, les paramètres du processus (taille des sous-ensembles, nombre de pixels calculés) et l'en­vironnement physique (uniformité des échantillons, motifs de tachetures, effet thermique de la caméra CCD et distorsion de la lentille, erreur de non-linéarité dans le circuit de la jauge de déformation) ont fait l'objet d'une étude et de discussions. Enfin, des solutions ont été amenées afin d'aider à réduire les erreurs systématiques et aléatoires en lien avec les trois catégories de sources d'erreurs susmentionnées. Pour terminer, un nouvel algorithme DIC permettant une approximation plus juste de l'estimation initiale, entraînant par conséquent une convergence efficace et précise de l'op­timisation a été développé, programmé, mis en oeuvre et vérifié avec succès pour ce qui est des déformations importantes. La validation expérimentale a fait ressortir une erreur systé­matique inattendue des mesures DIC lorsque comparées aux mesures obtenues au moyen de la technique des jauges de déformation. Plus l'échantillon se déformait, plus l'erreur augmentait proportionnellement. Par conséquent, la distorsion graduelle des tachetures sur la surface de l'objet était probablement la cause de l'erreur. L'erreur étant systéma­tique, elle a été corrigée. Le procédé d'atomisation a permis de générer des tachetures de façon reproductible sur la surface d'un objet. Grâce aux mesures DIC, le comportement mécanique des polymères soumis à des déformations importantes, comme le polyméthyl métacrylate servant à la reconstruction du squelette, peut être étudié et une fois maîtrisé, servir à l'élaboration de matériaux plus efficaces. / Abstract : The present thesis is focused on the non-contact and efficient strain measurement using the Digital Image Correlation (DIC) method, which employs the tracking of random speckle pattern for accurate measurement of displacements on a surface of an object undergoing deformation. Specifically, a more efficient DIC algorithm was successfully developed, implemented, and validated. This thesis consists of five parts related to the novel DIC algorithm: (a) the development and implementation, (b) the numerical verification, (c) the experimental validation, for tensile loading, by comparing to the deformation measurements using the strain gauge technique, (d) the investigation of a novel atomization process to reproducibly generate the speckle pattern for accurate tracking, and (e) the analysis of the error sources in the DIC measurements. Specifically, the DIC algorithm was used to exemplarily examine the mechanical properties of polymethyl methacrylate (PMMA) used in skeletal reconstruction. In the DIC algorithm, images of an object are captured as it deforms. Nonlinear optimization techniques are then used to correlate the speckle on the surface of the objects before and after the displacement. This optimization process includes a choice of suitable initial displacement values. The more accurate the estimation of these initial displacement values are, the more likely and the more efficient the convergence of the optimization process is. The thesis introduced a novel, fuzzy logics based processing technique, approximation of the initial values of the displacement for initializing iterative optimization, which more accurately and efficiently renders the displacements and deformations as results. The mathematical formulation of the novel algorithm was developed and then successfully implemented into MATLAB programming language. The algorithmic verification was performed using computer-generated images simulating rigid body displacements and uniform tensile deformations. Specifically, the rigid motion images simulated (1) displacements of 0.1-1 pixel for the rigid body translation, (2) rotation angles of 0.5-5 ̊ for rigid body rotation and (3) large tensile deformations of 5000-300000µɛ, respectively. The verification processes showed that the accuracy of the novel DIC algorithm, for the simulated displacement types and levels above 99%. The experimental validation was conducted to examine the effectiveness of the novel technique under realistic testing conditions. Normalized PMMA specimens, in accordance to ASTM F3087, were produced, inspected and subjected to tensile loading until failure. The deformation of the specimen surface was measured using (a) the novel DIC, and (b) strain gauge rosette techniques. The mean maximum force and ultimate strength of four specimens were 882.2±108.3 N and 49.3±6.2 MPa, respectively. The mean ultimate deformation from the gauge and DIC groups were 15746±2567µɛ and 19887±3790µɛ, respectively. These large deformations are common in polymeric materials, and the DIC technique has thus far not been investigated for large deformation. The relative mean error of the DIC measurement, in reference to those of the strain gauge technique, was found to be up to 26.0±7.1%. Accordingly, the mean Young's modulus and Poisson's ratio of strain gauge measurement were 3.78±0.07 GPa and 0.374±0.02, and of the DIC measurements were 3.16±0.61 GPa and 0.373±0.08, respectively. The increasing difference of the DIC strain measurements relative to those of the strain gauge technique is likely related to the gradual distortion of the speckle pattern on the surface of the tensile specimen. Subsequently, a Correction Factor (CF) of 1.27 was introduced to correct for the systematic error in the deformation measurements of the DIC group. The corrected ultimate deformation of the DIC measurements became 15712±357µɛ with the relative mean error of -0.5±7.1%, if compared to those measurements of the strain gauge techniques. Correspondingly, the mean Young's Modulus and Poisson's ratio of the DIC and of the strain gauge measurements became 3.8±0.4 GPa and 0.368±0.025, respectively. Using an atomization process, paint speckles were reproducibly generated on the surface of an object. A factorial design of experiments was used to investigate the speckle pattern (grey value distribution and gradient) for the DIC measurement accuracy. Specifically, nine different speckle patterns were generated using the atomization process and tested for rigid body translation and rotation. The results showed the relative mean errors among the nine speckle patterns varied from 1.1±0.3% to -6.5±3.6%. The preferred speckle pattern, which was characterized by a wide range of sharp speckle and of grey values, produced a mean error of 1.1±0.3%. The analysis of errors and relating sources in the DIC measurement was conducted. Three categories of sources including algorithmic sources, processing parameters sources (subset size, number of pixels computed) and physical environment sources (specimen uniformity, speckle pattern, self-heating effect of the CCD camera and lens distortion of the camera, non-linearity error in strain gauge circuit) were investigated and discussed. Finally, the solutions were provided in order to help reduce the systematic and random errors relating to the aforementioned three categories of sources for errors. In conclusion, a novel DIC algorithm for a more accurate approximation of the initial guess and accordingly for an efficient and accurate convergence of the optimization was successfully formulated, developed, implemented and verified for relatively large deformations. The experimental validation surprisingly showed a systematic error of the DIC measurements, if compared to the measurements of the strain gauge technique. The larger the deformation applied to the specimen, the larger the error gradually became. Therefore, the gradual distortion of the speckles on the surface of the object was likely the underlying cause of the error. The error was systematic and therefore corrected. The atomization process allowed generating reproducible speckles on the surface of an object. Using the DIC measurements, the mechanical behavior of polymers, undergoing large deformations, such as polymethyl methacrylate used in skeletal reconstruction can be investigated and, once understood, the knowledge gained can help develop more effective materials.

Le travail présenté porte sur l’étude de la réactivité des scories de la métallurgie du cuivre et leur utilisation comme additions minérales actives en remplacement partiel au ciment. <p>Les scories étudiées appartiennent soit au système CaO-MgO-Al2O3-SiO2 (Scorie A épuisée en métaux « lourds »), soit au système CaO-FeO-SiO2 (Scories B, C, D et E) avec des teneurs en MgO, Al2O3 et ZnO appréciables ainsi que des proportions en métaux « lourds », autres que le Zn, non négligeables (Cu, Co et Pb). A l’exception de la scorie A, toutes les scories étudiées peuvent être classées comme « déchets dangereux » pour l’homme et pour l’environnement, car elles sont riches en métaux « lourds ». <p>La R.D.Congo regorge des quantités énormes de ces scories qui occupent des grands espaces avec tous les risques de pollution qu’elles présentent. En général, pour gérer ces types des matériaux, plusieurs techniques peuvent être utilisées. Dans ce travail, nous nous sommes proposés d’utiliser ces scories comme additions minérales actives au ciment afin de stabiliser leurs métaux « lourds », de les éliminer de la nature et de leur donner une valeur économique. Une telle étude n’a jamais été réalisée en R.D. Congo. De ce fait, trois axes d’études expérimentales ont été mis en œuvre :<p><p>- une étude théorique de la réactivité des scories fondée sur leurs caractéristiques chimiques et structurales.<p><p>- une étude de la réactivité intrinsèque des scories réalisée dans différents systèmes (NaOH, Ca(OH)2 et ciment), à partir de leurs verres. La méthode qui a été utilisée consiste à suivre la disparition des exothermes de cristallisation des verres de scories, lors de l’hydratation, par analyse thermique différentielle (ATD). A l’issu de cette étude, nous avons trouvé que toutes les scories ont un potentiel hydraulique qui dépend de la nature et de la proportion en verres qui les composent ainsi que des types d’activateurs utilisés. Les verres les plus réactifs sont ceux qui contiennent une grande quantité en éléments structuraux basiques (Si2O76-, Si2O88-, etc.) et en cations modificateurs de réseaux (Ca2+, Mg2+, Al3+ et Zn2+). <p>Le ciment, utilisé comme activateur, constitue un des meilleurs composés qui permet une hydratation facile et rapide des différents types de verres à 25°C. Lors de cette hydratation, il s’établit des interactions entre les verres des scories et les phases anhydres et/ou hydratées du ciment qui affectent directement l’évolution de l’hydratation des phases du clinker ainsi que les propriétés mécaniques des pâtes durcies des mélanges « scories-ciments ». <p>Les produits issus de l’hydratation des scories et/ou du ciment (C-S-H) sont les phases qui permettent de « stabiliser» les métaux « lourds » par insertion dans leur structure. <p>Toutes les scories étudiées peuvent être valorisées comme ajouts au ciment. Cependant, cette valorisation sera plus rentable si la scorie est épuisée en éléments recherchés en métallurgie tels que le Cu, le Co, le Ge et le Zn, comme c’est le cas des scories A et E. <p> <p>- une étude des ciments à base des scories A et E a porté sur leur cinétique d’hydratation afin de corréler leurs processus d’hydratation à l’évolution de la microstructure et des propriétés mécaniques de leurs pâtes durcies. Les temps de prise de ces ciments ont aussi été déterminés. <p> / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished