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Made available in DSpace on 2016-12-08T17:19:24Z (GMT). No. of bitstreams: 1 Elder Gregol dos Santos.pdf: 4072797 bytes, checksum: c4f0d20ac13dce8a35fd04f90bc3545d (MD5) Previous issue date: 2014-11-07 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / The carburiser materials have been widely used in the foundry industry, motivated by increasing use of scrap steel and consequent reduction in the use of pig iron. Several factors, besides of recovery of carbon in the metal bath, can be associated with the use of carburisers, including the effect on the levels of silicon, sulfur, nitrogen and degree of nucleation of metal. This paper evaluates the effects of the use of carburisers materials, of the types natural graphite, synthetic graphite, graphite permanent mold residue (used in molds of continuous casting) and synthetic graphite with low sulphur amount. The method of addition was chosen on the surface of the liquid bath, at a medium frequency induction furnace, 2500 kg capacity, tests at three different temperatures. Was observed that there was no incorporation of nitrogen of carburisers to liquid metal, and the sulfur content was altered only when used synthetic carburiser. The increase in temperature caused an increase in the value of carburation efficiency, regardless of the type of carburisers. In general, it was observed an increase 21-32% when the temperature is changed from 1480 to 1545 ° C. Only the special synthetic carburisers showed lower sensitivity to temperature increase, showing an increase of only 5% efficiency. It was found that the ash content of the carburiser is a variable that affects significantly the dissolution process of the carburiser. The results showed that the carburisers with lower ash content, have higher carburation efficiency. This paper proposed the concept of rate of gain of associated carbon, which was effective for predicting the behavior of % C of liquid metal after the addition of the carburiser. It was found that the rate of gain associated initial carbon is favored with increasing temperature and the sulfur content of liquid metal, and impaired with an increase in the percentage of ash in carburiser. As for the value of the combined rate of dissolution, this showed an increase when the temperature of addition is growing. It was noted that the value of maximum rate of efficiency has relation with the value of the combined rate of dissolution, allowing to conclude that the higher the value of the combined dissolution rate, the faster the process reaches its maximum efficiency. The results observed for the residue of graphite mold, in the carburation efficiency, efficiency rate and combined rate of dissolution, showed that this material has the potential to be used as carburante in foudry. Comparing the initial and final conditions of the experiments, it was found that bath treated with synthetic carburiser with low% S, showed a reduction in the degree eutetic supercooling at temperatures of 1485 and 1545 ° C and the chill residue contributed to the reduction of degree eutetic supercooling at temperatures of 1485, 1515 and 1545 ° C. When analyzing the behavior of the degree eutetic supercooling with time after the addition of carburiser, was possible to identify three different behaviors. / Os materiais carburantes têm sido amplamente utilizados na indústria de fundição, em função da crescente utilização de sucata de aço e a consequente redução do uso de ferro gusa. Vários fatores, além da recuperação de carbono no banho metálico, podem ser associados ao uso dos carburantes, entre eles o efeito nos teores de sílicio, enxofre, nitrogênio e no grau de nucleação do metal. Este trabalho apresenta a avaliação dos efeitos do uso de materiais carburantes, dos tipos grafite natural, grafite sintético, resíduo de coquilha de grafite (utilizado em matrizes de fundição contínua) e grafite sintético com baixo teor de enxofre. O método de adição escolhido foi sobre a superfície do banho líquido, em um forno à indução de média frequência, de 2500 Kg de capacidade, realizando testes em três temperaturas distintas. Observou-se que não houve incorporação de nitrogênio do carburante pelo metal líquido, e o teor de enxofre sofreu alteração somente quando usado o carburante sintético. O aumento da temperatura provocou um aumento no valor da eficiência de carburação, independente do tipo de carburante. De maneira geral, observou-se um aumento de 21 32% na eficiência, quando a temperatura é alterada de 1480 a 1545°C. Apenas o carburante sintético especial apresentou menor sensibilidade ao aumento da temperatura, mostrando um aumento de apenas 5% de eficiência. Verificou-se que o teor de cinzas do carburante é uma variável que afeta significativamente o processo de dissolução do carburante. Os resultados evidenciaram que os carburantes com menor teor de cinzas, apresentam maiores valores de eficiência de carburação. Este trabalho propôs o conceito da taxa de ganho de carbono associada, a qual se mostrou efetiva para a previsão do comportamento do % C do banho, após a adição do carburante. Verificou-se que a taxa de ganho de carbono associada inicial, é favorecida com o aumento da temperatura e do teor de enxofre do metal, sendo prejudicada com aumento do percentual de cinzas do carburante. Quanto ao valor da taxa de dissolução combinada, esta mostrou um aumento quando a temperatura de adição é crescente. Notou-se que o valor da taxa de eficiência máxima possui relação com o valor da taxa de dissolução combinada, permitindo concluir que quanto maior o valor da taxa de dissolução combinada, mais rapidamente o processo atinge a sua eficiência máxima. Os resultados observados para o resíduo de coquilha de grafite, na eficiência de carburação, taxa de eficiência e na taxa de dissolução combinada, evidenciaram que este material tem potencial para ser utilizado como carburante. Comparando as condições iniciais e finais dos experimentos, verificou-se que banhos tratados com carburante sintético com baixo %S, apresentaram uma redução no super-resfriamento do eutético, nas temperaturas de 1485 e 1545°C, e o resíduo de coquilha contribuiu para a redução do super-resfriamento do eutético nas temperaturas de 1485, 1515 e 1545°C. Quando analisado o comportamento do grau de super-resfriamento com o tempo, após a adição dos carburantes, foi possível identificar três comportamentos distintos.

Due to recent legislation aimed at reducing carbon emissions into the environment through weight reduction, the automotive and aerospace industries are using light alloys such as aluminium silicon (Al–Si) and aluminium zirconium (Al–Zr) instead of steel due to their excellent mechanical properties and low weight to strength ratio. In order to further improve mechanical and metallurgical properties in these alloys, grain refinement is usually used in industry. However, the current and most widely used grain refiner Al–5Ti–B is unable to refine Al–Si alloys with silicon content greater than 3 wt.%., and Al–Zr alloys due to poisoning of the refiner by silicon and zirconium. The Al–5Ti–B refiner also contains larger Al3Ti particles and agglomerates of TiB2 which affect its efficiency and suitability in industrial applications where thin sheets are required. In this study, a new technique which improves the microstructure and efficiency of the Al–5Ti–B refiner has been developed. This involves the reaction of potassium tetrafluoroborate (KBF4) and potassium hexafluorotitanate (K2TiF6) salts at shorter reaction time before ultrasonic processing during solidification. This leads to the formation of a new Al3Ti morphology and de-agglomeration of TiB2 particles which enhances its grain refinement efficiency by 20%. Secondly, through phase diagram analysis of Al grain refining systems and crystallography studies, it was observed that Al3Ti and Al3Nb display similar lattice parameters with atomic misfit of 4.2% and would undergo a peritectic reaction with α-Al at low contact angles. Based on this, and using the duplex nucleation theory and poisoning by Si and Zr, a new quaternary grain refiner containing aluminium, titanium, niobium and boron (Al–4Ti–Nb–B) has been developed. This novel grain refiner has been found to be efficient in Al–Si alloys and Al–Zr, both at laboratory and industrial scales, and to improve the mechanical properties of the alloys despite the presence of Ti in the alloy. It was observed that the addition of Nb to an Al–Ti–B system leads to the formation of solid solution phases of Al3Ti1-xNbx, Al3Nb1-xTx, and (Ti1-xNbx)B2 which prevents poisoning by Si and Zr. Experimental simulations showed that Al3Nb1-xSix rather than Ti(Al1-xSix)3 are formed in Al–Si alloys, and Al3(Ti1-xNbx) and (Al3Ti1-xNbx)B2 phases are formed in Al–Zr alloys rather than Al3(Zrx,Ti1-x), B2(Zrx,Ti1-x) or ZrB2 phases. A new grain refining mechanism, ‘The Quad Nucleation Theory’ based on four nucleation events in Al–4Ti–Nb–B has been proposed. Other newly developed quaternary and ternary novel grain refiners capable of refining aluminium silicon alloys are also presented in this thesis. This includes a novel method of refining Al–Si alloys using phosphorus and niobium.

abstract: Zinc oxide (ZnO) has attracted much interest during last decades as a functional material. Furthermore, ZnO is a potential material for transparent conducting oxide material competing with indium tin oxide (ITO), graphene, and carbon nanotube film. It has been known as a conductive material when doped with elements such as indium, gallium and aluminum. The solubility of those dopant elements in ZnO is still debatable; but, it is necessary to find alternative conducting materials when their form is film or nanostructure for display devices. This is a consequence of the ever increasing price of indium. In addition, a new generation solar cell (nanostructured or hybrid photovoltaics) requires compatible materials which are capable of free standing on substrates without seed or buffer layers and have the ability introduce electrons or holes pathway without blocking towards electrodes. The nanostructures for solar cells using inorganic materials such as silicon (Si), titanium oxide (TiO2), and ZnO have been an interesting topic for research in solar cell community in order to overcome the limitation of efficiency for organic solar cells. This dissertation is a study of the rational solution-based synthesis of 1-dimentional ZnO nanomaterial and its solar cell applications. These results have implications in cost effective and uniform nanomanufacturing for the next generation solar cells application by controlling growth condition and by doping transition metal element in solution. / Dissertation/Thesis / Ph.D. Materials Science and Engineering 2012

Submitted by MARCIA ROVADOSCHI (marciar@unifra.br) on 2018-08-20T12:45:35Z No. of bitstreams: 2 Tese_MarceloAdrianoDuart.pdf: 8331452 bytes, checksum: d69e28005ad96f39781d95f4cfc7f7fb (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) / Made available in DSpace on 2018-08-20T12:45:35Z (GMT). No. of bitstreams: 2 Tese_MarceloAdrianoDuart.pdf: 8331452 bytes, checksum: d69e28005ad96f39781d95f4cfc7f7fb (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Previous issue date: 2017-07-31 / Civil construction industry has been developing technologically with the growth in the number of works in various sectors such as housing, transport, industry and infrastructure. This study is intended to contribute to the development of scientific cementitious materials by studying the use of carbon nanomaterials as carbon nanotubes (CNT) and nanoparticles of Hydrated Calcium Silicate (C-S-H) incorporated into the matrix of these materials, which can be categorized as composite, in this case nanocomposites. Materials performance is usually related to the existence of considerable flaws or deficiencies in some properties or characteristics. The incorporation of nanomaterials is a possibility for the amelioration or even create some characteristic and materials property. The use of CNT has already been investigated and the results have shown that though with increase of costs produced materials have positive characteristics such compression and tensile resistance increase and still elasticity modulus increase. Currently steel is used but the fibers and filler materials such as CNT may be an alternative because they can have tensile strength up to 100 times higher than steel, as recent research has shown. The main assumption is that nanoparticles such as C-S-H and oxidized multi walled carbon nanotubes (MWCNT-OX) favor the kinetics of cement hydration and contribute to the nucleation and crystal growth enhancing material characteristics produced as concrete and mortar, for example. In general, it was verified that the combined additions of C-S-H with Ca / Si = 0.8 ratio with nanotubes brought positive results of nanocomposite nanostructure improvements, verified by porosity, permeability analysis and qualitative analysis of electron microscopy images. An increase in the value of the mechanical properties analyzed was shown as a 33% increase in compressive strength, 38% increase in modulus of elasticity and 30% in tensile strength. It is also concluded that using the C-S-H addition with Ca/Si ratio = 0.8 in isolation is a viable alternative to produce relevant results with a lower cost than to opt for mixed additions, since CNT are still materials with high cost and more complex production than C-S-H. / A construção civil vem se desenvolvendo tecnologicamente acompanhando o crescimento do número de obras em vários setores como habitacional, transportes, industrial e infraestrutura. Este projeto pretende contribuir cientificamente para o desenvolvimento de materiais cimentícios através do estudo da utilização de nanomateriais de carbono como nanotubos de carbono (NTC) e também nanopartículas de Silicato de Cálcio Hidratado (C-S-H) incorporadas à matriz destes materiais, que podem ser classificados como compósitos, neste caso nanocompósitos. O desempenho dos materias normalmente está relacionado a existência de falhas ou deficiências consideráveis em algumas propriedades e caracteristicas. A incorporação de nanomateriais é uma possibilidade para o melhoramento ou até mesmo a criação de alguma característica ou propriedade em determinados materiais. A utilização de NTC já vem sendo pesquisada e os resultados têm demonstrado que, embora com elevação dos custos, os materiais produzidos apresentam características positivas como: aumento da resistência à compressão e flexão e também do módulo de elasticidade. Atualmente usa-se o aço e fibras mas a adição de materiais como NTC pode ser uma alternativa, pois estes podem apresentar resistência à tração até 100 vezes maior que o aço, conforme pesquisas recentes já demonstram. A hipótese principal é que nanopartículas de C-S-H e também NTC favorecem a cinética de hidratação de cimentos e contribuem para a nucleação e crescimentos de cristais de produtos hidratados melhorando características dos materiais produzidos como por exemplo: concretos e argamassas. De forma geral, verificou-se que as adições combinadas de C-S-H com relação Ca/Si=0,8 com nanotubos de carbono paredes múltiplas oxidados (NTCPM-OX) trouxeram resultados positivos de melhoria na nanoestrutura dos nanocompósitos produzidos, verificados pela análise da porosidade, permeabilidade e também pela análise qualitativa de imagens de microscopia eletrônica. Veficou-se aumento do valor das propriedades mecânicas analisadas como 33% de aumento da resistência à compressão, 38% de aumento do módulo de elasticidade dinâmico e 30% da resistência à tração. Conclui-se ainda que usar a adição de C-S-H com relação Ca/Si=0,8 de forma isolada é uma alternativa viável produzindo resultados relevantes com um custo mais baixo que optar por adições mistas, visto que ainda os NTC são materiais com custo elevado e produção mais complexa do que o C-S-H.

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Pseudomonas syringae produz núcleos de gelo biológicos de grande eficiência. Bioaerossóis destas células tem potencial de participar na glaciação de nuvens, podendo influenciar a precipitação. Foram estudadas como as condições as quais P. syringae está sujeita em suspensão na atmosfera afetam sua sobrevivência e sua atividade de nucleação de gelo. Duas cepas foram testadas, e ambas apresentaram baixa tolerância ao UV-C e ao UV-B, mas exibiram uma maior resistência quando expostas a um espectro semelhante ao encontrado no ambiente. A atividade de congelamento de uma das cepas (pv. syringae) não foi afetada pelo UV, enquanto que para a outra (pv. garcae) houve uma redução moderada. Em resposta à dessecação, pv. garcae foi substancialmente mais resistente que pv. syringae. Isto também afetou a nucleação de gelo das cepas. Em ensaios adicionais, estas bactérias foram expostas em um voo de balão estratosférico, e a uma simulação em laboratório das condições no topo da troposfera. Nestes dois experimentos, sobreviventes protegidos do UV foram recuperados. / Pseudomonas syringae produces biological ice nuclei of great efficiency. Bioaerosols of these cells have the potential to take part in cloud glaciation, possibly influencing the precipitation. It was studied how the conditions to which P. syringae is subjected while in suspension in the atmosphere affect its survival and its ice nucleation activity. Two strains were tested, and both showed a low tolerance to UV-C and UV-B, but exhibited a higher resistance when exposed to a spectrum similar to the one found in the environment. The freezing activity of one of the strains (pv. syringae) was not affected by the UV, while that for the other (pv. garcae) there was a moderate reduction. In response to desiccation, pv. garcae was substantially more resistant than pv. syringae. This also affected the ice nucleation by the strains. In additional assays, these bacteria were exposed in a stratospheric balloon flight, and to a laboratory simulation of the conditions at the top of the troposphere. After these two experiments, survivors protected from the UV were recovered.

Este projeto faz parte de uma Rede Interdisciplinar de Pesquisa em Superligas no Brasil (Projeto Pró-Engenharias - CAPES), que tem como objetivo o desenvolvimento técnico e científico do Brasil nesta classe de materiais. A rede é composta por especialistas de estabelecida competência em assuntos fundamentais para o desenvolvimento de materiais estruturais, tais como: fusão em vácuo, solidificação direcional, relações orientação-propriedade, tratamentos térmicos, fluência, fadiga em alta temperatura, oxidação e corrosão a quente. Assim, na parte que compete a este pesquisador, foram estudadas as propriedades de fadiga em altas temperaturas da liga MAR-M247 e de uma nova liga, a liga MAR-M247 modificada pela substituição do Ta pelo Nb, e sendo doravante denominada MAR-M247(Nb). Foram desenvolvidos estudos correlacionando parâmetros intrínsecos do material, como composição química e microestrutura adicionalmente a parâmetros extrínsecos, tais como: temperatura, estudo de oxidação, propriedades de fadiga, ensaios de tração em temperatura ambiente, 250, 500, 700, 800, 900 e 1000ºC, conforme as normas AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) E 8M-00 e ASTM E 21-00. Em relação aos ensaios de fadiga foram realizados ensaios de nucleação de trincas , conforme a norma ASTM E466-07 e os resultados foram apresentados na forma de curvas S-N e analisados estatisticamente segunda a norma ASTM E739-10. Para auxiliar na definição dos micromecanismos de fadiga, as superfícies de fratura foram analisadas utilizando o microscópio eletrônico de varredura (MEV) e microscópio ótico estereoscópico (MO). Foi realizado ensaio de oxidação para verificar a susceptibilidade a oxidação das ligas, sendo este um dos fatores que afetam a vida em fadiga em alta temperatura. / This project is part of an interdisciplinary network of Research in Super League in Brazil (Project Pro-Engineering - CAPES), which aims to technical and scientific development of Brazil in this class of materials. The network is composed of experts of established competence in matters fundamental to the development of structural materials, such as: vacuum melting, directional solidification, relationships property-oriented, heat treatment, creep, fatigue in high temperature oxidation and hot corrosion. Thus, at the racing this researcher, were studied the fatigue properties at high temperatures MAR-M247 alloy and a new league, which in reality is the MAR-M247 alloy modified by replacing the Ta by Nb, and being hereinafter referred to as MAR-M247 (Nb). Were designed studies correlating parameters intrinsic material, such as chemical composition and microstructure, with extrinsic parameters such as: temperature and type of loading, with the properties fatigue. Thus, tensile tests at room temperature environment, 250, 500, 700 and 900ºC, and tests for compression at temperatures of 700 and 900ºC were performed to determine the elastic behavior and elastoplastic material, according to the ASTM E-8M 00, ASTM E 21-00 and ASTM E209-00. Were also conducted testing of fatigue crack nucleation, as ASTM E466-07. The results were presented at form of SN curves and statistically analyzed the second ASTM E739-10. To assist in the definition of micromechanics of fatigue, the fracture surfaces were examined in a scanning electron microscope (SEM) and stereoscopic optical microscope (OM). Was oxidation test performed to check susceptibility to oxidation of the alloy, which is the factor affecting the fatigue life.

La cristallisation est influencée par plusieurs paramètres tels que la sursaturation, la température, le milieu et l’hydrodynamique. Pour cela le criblage rapide des conditions de cristallisation est souvent exigé lors de l’étude de la cristallisation d’une molécule. Cependant lorsqu’une faible quantité de matière est disponible, un outil expérimental adapté est indispensable.Dans notre cas, le système microfluidique dédié à la cristallisation est basé sur la génération des gouttes de volume nanométrique dans lesquels la cristallisation peut avoir lieu de façon indépendante. Des gouttes monodispersées en taille et en conditions expérimentales nous permettent de réaliser des études statistiques pour répondre à la stochasticité du phénomène de nucléation, ceci tout en consommant peu de matière.Le but de cette thèse est de créer un montage microfluidique universel, qui soit compatible à tout solvant et toute molécule. Pour cela, nous utilisons des jonctions et des capillaires microfluidiques simples résistants à de nombreux solvants. Nous cherchons d'abord à contrôler les écoulements microfluidiques et à réduire les volumes mis en jeu. Nous avons étudié les régimes de génération des gouttes et la loi d'échelle de la taille des gouttes. Dans le cadre de l’étude de la cristallisation, nous montrons la faisabilité de notre dispositif pour l’étude de la cristallisation en variant la viscosité avec l’exemple de l’urate oxydase recombinante ou rasburicase que nous avons cristallisée dans une solution aqueuse de PEG. Pour finir, nous avons intégré un module de caractérisation en ligne dans notre système microfluidique afin d'analyser la composition chimique de chaque goutte. / Crystallization is influenced by several parameters such as supersaturation, temperature, environment, and hydrodynamics. Thus, a rapid screening of crystallization conditions is often required during the study of the crystallization of a molecule. But when a small amount of material is available, a suitable experimental tool is essential. In our case, the microfluidic system dedicated to crystallization is based on the generation of nanoliter droplets in which crystallization can occur independently. Forming hundreds of droplets with monodisperse sizes and experimental conditions, we can make a large number of experiments per condition for statistical studies to meet the stochasticity of the phenomenon of nucleation while consuming little material. Our goal is to create a universal microfluidic assembly which is compatible with all solvents and molecules. Thus, we are interested in simple microfluidic junctions and tubings which is resistant to many solvents. From such systems, we have first characterized the hydrodynamic properties of the set-up: we sought to control microfluidic flow and reduce the volumes put-in. We studied the droplet generation regimes and the scaling law of drop size and frequency. For crystallization study of biomolecule, we have validated our microfluidic set-up for crystallization studies in a viscous media, on the recombinant urate oxidase or the rasburicase in an aqueous solution of PEG. Finally, we integrated a module for on-line characterization of each droplet’s chemical composition.

Ce travail examine des nanofils III-V synthétisés en mode vapeur-liquide-solide, une goutte liquide catalysant la croissance unidimensionnelle. En conjuguant expériences d’épitaxie par jets moléculaires, caractérisations structurales et analyses théoriques, j'étudie et clarifie plusieurs questions cruciales. L’une d'elles est le contrôle de la phase cristalline, qui s’avère souvent un mélange de segments cubiques et hexagonaux. Au moyen d’une analyse probabiliste de la séquence d'empilement de nanofils d’InP, je montre que la sélection de phase est déterminée non seulement par les conditions de croissance mais aussi par des interactions entre monocouches. Je souligne et discute le rôle de l'énergie de bord du germe qui médie la formation de chaque monocouche. On sait par ailleurs que le caractère abrupt des interfaces dans les hétérostructures axiales est limité par l’accumulation de matière dans la goutte (effet réservoir). J'étudie la formation de telles hétérostructures dans des nanofils de GaAs auto-catalysés en utilisant un second élément des groupes V (P) ou III (Al). Les profils compositionnels des insertions ternaires sont analysés à la résolution atomique. Les interfaces se révèlent soit plus larges (GaAsP) soit plus étroites (AlGaAs) qu’attendu et la morphologie du front de croissance dépend de la supersaturation. Je montre que, dans les deux cas, la largeur d’interface peut être réduite à quelques monocouches et je suggère d’autres améliorations. Enfin, je présente mes tentatives pour réaliser des nanofils ultraminces de GaAs et GaP et je discute du contrôle de la croissance à l’échelle d’une monocouche par réduction du caractère stochastique de la nucléation. / This work investigates III-V nanowires synthesized via the vapor-liquid-solid method, whereby a catalyst droplet promotes one-dimensional growth. By combining molecular beam epitaxy experiments, structural characterization and theoretical analyses, I study and clarify several critical issues. One of them is the control of the crystal phase, which is frequently found to be a mix of cubic and hexagonal segments. By performing a probabilistic analysis of the stacking sequence of InP nanowires, I show that phase selection is determined not only by growth conditions but also by interactions between layers. I highlight and discuss the role of the edge energy of the nucleus that mediates the formation of each monolayer. Another important problem is the formation of axial heterostructures, which interface sharpness is severely limited by material accumulation in the droplet (‘reservoir effect’). To this end, I study the formation of such heterostructures in Ga-catalyzed GaAs nanowires using either a second group V element (P) or a second group III element (Al). The composition profiles of the ternary insertions are analyzed with monolayer resolution. The interface widths are found to be larger (GaAsP) or narrower (AlGaAs) than expected, and the morphology of the growth front depends on supersaturation. In both cases, I demonstrate that the interface width can be reduced to a few monolayers and suggest further improvements. Attempts to achieve ultrathin GaAs and GaP nanowires that would permit lateral quantum confinement are presented. Finally, I consider the possibility of minimizing the stochastic character of nucleation ultimately to control the growth of single monolayers.