Rozprawy doktorskie na temat „FERROUS MATERIAL”

Slag is a vital part of metal production since it removes impurities from the metal. As slag is continuously produced, the options are either to dispose slag in landfill or acknowledge slag as a product. Slag can be used in many different applications, ranging from fertilizer to construction material; in some cases, the properties of slag make it a superior alternative to virgin stone materials. The properties and thereby the field of application is determined by the mineralogical composition of the slag. Slag is considered an environmentally friendly material as long as the leaching of certain elements stay below specified thresholds, for leaching of chromium the limit is at 0.5 mg/kg for slag to be considered inert material. The most common leaching approach is to compare leaching analyses from slag samples to deduce which elements and/or phases contribute or prevent leaching of specific elements. With this method each slag need to be investigated separately and the result may only apply for that specific slag type. In this thesis the approach is different: individual minerals are synthesized and dissolved separately at various pH to accurately assess their dissolution capabilities. By studying the dissolution of individual minerals the leaching of any type of slag with known mineralogical composition can be anticipated. Slag leaching can then be tailored, for example, chromium leaching can be eliminated if all chromium containing phases are removed or not capable of dissolving. In this thesis the dissolution of akermanite, β- and γ-dicalciumsilicate, merwinte, monticellite, pseudowollastonite and magnesiowüstite with varying FeO/MgO ratios are studied. Leaching tests of magnesiowüstite with 4 wt% Cr2O3 were also included. The dissolution of each mineral is calculated by the acid addition required to maintain a constant pH with 50 mg of mineral in 100 ml water. As expected, the dissolution decreases as pH increases, with exception of the dicalcium silicates which dissolved completely at pH 4 to 10. The dissolution of the minerals is largely connected to the elemental composition. In the silica based minerals a high Ca ratio promotes dissolution while a high Si ratio impedes the dissolution rate. Both dissolution and chromium leaching of magnesiowüstite depends on the FeO content, with increasing FeO content the dissolution and leaching decreases, magnesiowüstite with at least 60 wt% FeO does not dissolve at pH 10. None of the magnesiowüstite compositions were close to the chromium leaching limit of inert material, 0.5 mg/kg, as the highest leaching sample, with 52 wt% FeO, leached 0.069 mg/kg.

Properties of cast aluminum components can be improved by strategically placing ferrous inserts to locally improve properties such as wear resistance and stiffness. A cost-effective production method is to cast-in the insert using the solidification of the molten aluminum as a joining method. Metallurgically bonding between the metals could potentially improve both load and heat transfer across the interface. The metallurgical bond between the steel and the aluminum has to be strong enough to withstand stresses related to solidification, residual stresses, thermal expansion stresses, and all other stresses coupled with the use of the component. Formation of a continuous defect free bond is inhibited by the wetting behavior of aluminum and is governed by a diffusion process which requires both energy and time. Due to the diffusional nature of the bond growth in combination with post manufacturing heat treatments defects such as Kirkendall voids can form. The effect of aluminum alloying elements during liquid-solid bond formation in regards to microstructural changes and growth kinetics has been described. A timeframe for defect formation during heat treatments as well as microstructural changes has been established. The effect of low melting point coatings (zinc and tin) on the nucleation of the metallurgical bond has been studied as well the use of a titanium coating for microstructural modification. A set of guidelines for successful metallurgical bonding during multi- material metal casting has also been constructed.

Detection of stress concentration zones using stand-off magnetometry based on the magnetomechanical effect has recently been applied to pipeline inspection. This study addresses the lack of scientific evidence encountered in the development of the technology by using a combination of laboratory experiments, field observations, and computer simulations to study the magnetic indication of local stress concentrations in the bulk material. It then offers new techniques to determine features of underground pipelines, and evaluates their performance using field survey data and standard inspection reports. The models proposed in this study are capable of simulating the effects of stress cycles on magnetisation of steel bars and pipes placed in the earth's magnetic field. The experimental and simulation results have shown that the magnetic indication of a local stress concentration zone (SCZ) is due to the distribution of magnetisation between the local SCZ and the surrounding area or the bulk material, which has explained the reverse in the polarity of the magnetic indication when varying the applied stress. It also implies the possibility to monitor stress conditions in ferrous material. It is proposed that the gradient magnetic field should be used in order to extract the magnetic indication from the measured magnetic field, together with a parameter K as the criteria for detection and characterisation of local SCZ using the remote magnetic field. It has found that K is linear with the initial magnetic condition induced in low field at a given stress. Inversely, at a given initial condition, variation of K with stress follows the stress-magnetisation relationship of the material. K is more sensitive with stress at stronger initial conditions. The study has also established the quantitative exponential relationship between K and the measurement distance, which implies a technique to solve for stress condition from the remote magnetic field. A study on circumferential welded joints of pipelines has found magnetic features of the welds, which implies the possibility to locate them using above-ground surveys. A technique is proposed and is capable of locating 70% of the actual welds with an offset of 3 meters and the probability of false call of 20% for the pipelines of 17 meters constructed length buried with more than 2 meters depth of cover. A new practical technique to estimate the depth of cover of underground pipelines from the remote passive magnetic field, which has the tolerance of 8% of the measurement depth, is also proposed. Importantly, this study proposes a preliminary technique to detect SCZs in underground pipelines using the remote magnetic field, which can detect side bends and sag bends, and shows promises for detection of SCZs caused by mechanical defects. The development of these techniques are important milestones in non-invasive remote pipeline condition monitoring.

This study focused on molten salt purification processes to effectively reduce or eliminate the corrosive contaminants without altering the salt's chemistry and properties. The impurity-driven corrosion behavior of HAYNES® 230® alloy in the molten KCl-MgCl2-NaCl salt was studied at 800 ºC for 100 hours with different salt purity conditions. The H230 alloy exhibited better corrosion resistance in the salt with lower concentration of impurities. Furthermore, it was also found that the contaminants along with salt's own vaporization at high temperatures severely corroded even the non-wetted surface of the alloy. The presence of Mg in its metal form in the salt resulted in an even higher mass-loss possibly due to Mg-Ni interaction. The study also investigated the corrosion characteristics of several nickel and ferrous-based alloys in the molten KCl-MgCl2-NaCl salt. The average mass-loss was in the increasing order of C276 < SS316L < 709-RBB* < IN718 < H230 < 709-RBB < 709-4B2. The corrosion process was driven by the outward diffusion of chromium. However, other factors such as the microstructure of the alloy i.e. its manufacturing, refining, and heat-treatment processes have also shown to influence the corrosion process. Lowering the Cr content and introducing W and Mo in the alloy increased its resistance to corrosion but their non-uniform distribution in the alloy restricted its usefulness. To slow-down the corrosion process, and enhance the material properties, selected alloys were boronized and tested for their compatibility in the molten KCl-MgCl2-NaCl salt. The borided alloys exhibited better resistance to molten salt attack, where the boride layer in the exposed alloy was still intact, non-porous, and strongly adhered to the substrate. The alloys also did not show any compensation in their properties (hardness). It was also found that the boride layer always composed of an outermost silicide composite layer, which is also the weakest and undesired layer as it easily cracks, breaks, or depletes under mechanical and thermal stresses. Various different grades of "virgin" nuclear graphites were also tested in the molten KF-UF4-NaF salt to assist in the selection of tolerable or impermeable graphites for the MSR operational purposes. It was found that molten salt wettability with graphite was poor but it still infiltrated at higher pressure. Additionally, the infiltration also depended on the pore-size and porosity of the graphite. The graphite also showed severe degradation or disintegration of its structure because of induced stresses.
Doctor of Philosophy
Molten salts are considered as potential fuel and coolant candidates in MSRs because of their desirable thermophysical properties and heat-transfer capabilities. However, they pose grave challenges in material selection due to their corrosive nature, which is attributed to the impurities and their concentration (mostly moisture and oxygen-based) in the salt. This study focused on purifying the salt to reduce these contaminants without compromising its composition and properties. The influence of purification processes on the corrosion behavior of HAYNES® 230® alloy was studied in the molten chloride salt with different purity conditions. Various nickel and ferrous-based alloys were also studied for their compatibility in the molten chloride salt. This will assist in expediting the material selection process for various molten salt applications. It was observed that several factors such as alloy composition, its microstructure, impurities in the salt attribute to molten salt corrosion. It was also quite evident that corrosion in molten salts is inevitable and hence, the focus was shifted on slowing down this process by providing protective barriers in the form of coatings (i.e. boronization). The borided (coated) alloys not only improved the corrosion resistance but also enhanced and retained their properties like hardness after exposure to molten salts. Since these studies were conducted under static conditions, a more detailed investigation is needed for the selected alloys by subjecting them to extreme flow-conditions and for longer a duration of time. To achieve this objective, a forced circulation molten salt loop was designed and fabricated to conduct flow corrosion studies for alloys in molten chloride salt. Graphite is another critical component of the MSR where it is used as a moderator or reflector. Generally, molten salts exhibit poor wettability with graphite, but they can still infiltrate (graphites) at higher applied pressures, and result in the degradation or disintegration of graphite's structure, and eventually its failure in the reactor. This study provides infiltration data, and understanding of the degradation of various 'virgin' nuclear graphite grades by the molten fluoride salt. This should assist in the selection of tolerable or impermeable graphite grades for MSR operational purposes.

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This thesis was motivated by the study of voids and non-metallic inclusions influence on the high cycle fatigue of ferrous materials like steel, powder metal and gray cast iron. A second objective was to obtain simpler parameters, like the ones measured in hardness, static bending or axial tests, to evaluate materials in early phases of projects, in a way to avoid long fatigue tests. Initially the average fatigue strength was obtained for a high carbon steel. The effect of a silicon oxide inclusion near the surface on the performance of heavy-duty Cr-Si spring wire was also analyzed. The evaluation was done in terms of stress concentrating on the inclusion contours, due to the shot peening application on the surface and normal fluctuating loads. Mechanical properties of powder metal and cast iron were revised. Static tests without and with the presence of notches were performed, with the objective of obtaining a static notch sensitivity factor, to correlate with torsion fatigue results. The relation between hardness and torsion fatigue strength was evaluated for the cast iron, and simulations using linear elastic and nonlinear materials were performed to obtain geometric stress concentrating factors. A mesoscale simulation was done in plane stress, making it possible to evaluate local stress concentration in the cast iron matrix.
Esta tese foi motivada pelo estudo da influência de vazios e inclusões não metálicas na fadiga de alto ciclo de materiais ferrosos como aços, materiais obtidos por metalurgia do pó e ferros fundidos cinzentos. Foi objetivo também, avaliar parâmetros de medição mais simples, como os obtidos de ensaios de dureza e de flexão ou tração estáticos, como forma de avaliar materiais em fases iniciais de projeto, evitando-se longos ensaios de fadiga. Inicialmente obteve-se a resistência à fadiga de alto ciclo de um aço de alto teor de carbono. Analisou-se também o efeito da presença de uma inclusão de óxido de silício próximo à superfície de um arame de aço Cr-Si utilizado em molas submetidas a cargas reversas. A análise foi feita em termos de concentração de tensão nos contornos da inclusão, devido à aplicação de shot peening na superfície e também devido às cargas de operação. Uma revisão de propriedades mecânicas de aços obtidos por metalurgia do pó e do ferro fundido foi realizada, assim como ensaios estáticos sem e com entalhe, no intuito de obter um fator de sensibilidade ao entalhe estático, como forma de correlacionar com a sensibilidade ao entalhe na fadiga em torção. Foi avaliada a relação entre a dureza do ferro fundido e a sua resistência à fadiga na torção e realizadas simulações com material linear elástico e não linear para obter um fator de concentração de tensão geométrico. Uma simulação em mesoescala em estado plano de tensão foi realizada, podendo-se determinar a concentração de tensões locais na matriz do ferro fundido.

This work deals with the damage due to the simultaneous presence of hydrogen in atomic form and stress – straining.

The aim of this work is twofold: to better understand the hydrogen embrittlement mechanisms and to translate the acquired knowledge into a more appropriate qualification test.

The phenomena of hydrogen entry and transport inside the metals, together with the different types of damages due to the presence of hydrogen, are presented.

The analysis of the most important models proposed up to now for hydrogen embrittlement (HE) indicated that the slow dynamic plastic straining is a key factor for the embritteling process. There is a synergistic effect of hydrogen – dislocations interactions: on one hand hydrogen facilitates the dislocations movement (according to the HELP mechanism) and on the other hand dislocations transport hydrogen during their movement when their velocity is lower than a critical value.

This work is focused on supermartensitic stainless steels, base and welded materials. The interest on these materials is due to their broad use in offshore oil production.

First, the material’s characterisation with regards to hydrogen content and localisation was performed. This was conducted in charging conditions that are representative of industrial applications.

Because of previous industrial experience it was necessary to find a more appropriate qualification test method to asses the risk of HE.

In this work we proposed the stepwise repeated slow strain rate test (SW R – SSRT) as a qualification test method for supermartensitic stainless steels.

This test method combines hydrogen charging, test duration, plastic, dynamic and slow strains. Thus, this test method is coherent with both the model HELP proposed for hydrogen embrittlement and the observations of industrial failures.

The stepwise repeated slow strain rate test (SW RSSRT) is interesting not only as a qualification test of martensitic stainless steels, but also as a qualification test of conditions for using these materials (type of straining, range of strain and stress, strain rate, hydrogen charging conditions, etc.).

Ce travail se rapporte à l’endommagement provoqué par la présence simultanée de l’hydrogène sous forme atomique et une contrainte (appliquée où résiduelle).

Ce travail a comme but une meilleure compréhension du mécanisme de la fragilisation par l’hydrogène (FPH) et la recherche d’un essai de qualification qui soit cohérent avec ce mécanisme.

Les phénomènes liés à l’entrée et au transport de l’hydrogène au sein des métaux, ensemble avec les différents types d’endommagements dus à la présence de l’hydrogène, sont présentés.

L’analyse des modèles proposés jusqu’au présent pour la fragilisation par l’hydrogène (FPH) suggère que la déformation lente plastique dynamique est le facteur clé pour le processus de la fragilisation. Il y a un effet synergétique des interactions entre l’hydrogène et les dislocations: d’un coté l’hydrogène facilite le mouvement des dislocations (d’après le modèle HELP) et d’un autre coté les dislocations transportent l’hydrogène pendant leur mouvement, pourvu que leur vitesse soit en dessous d’une valeur critique.

Le travail a été conduit sur des aciers supermartensitiques, matériau de base et soudé. L’intérêt pour ces matériaux réside de leur large utilisation dans la production du pétrole en offshore.

D’abord, le matériau a été caractérisé du point de vu de la teneur et de la localisation de l’hydrogène. Les essais ont été conduits dans des conditions représentatives pour les cas industriels.

L’expérience industrielle d’auparavant indique qu’il est nécessaire de trouver un test de qualification plus approprié pour estimer la susceptibilité à la fragilisation par l’hydrogène.

Dans ce travail on propose un essai de traction lente incrémentée (SW R – SSRT) comme méthode de qualification pour les aciers supermartensitiques.

L’essai combine le chargement en hydrogène, la durée d’essai, la déformation lente, plastique et dynamique. Donc, cette méthode d’essai est cohérente avec le modèle HELP proposé pour FPH et les observations des accidents industriels.

Cet essai est intéressant pas seulement comme essai de qualification pour les aciers supermartensitiques, mais aussi comme essai de qualification pour les conditions d’utilisation des ces matériaux (type de déformation, niveau de déformation et contrainte, vitesse de déformation, conditions de chargement en hydrogène, etc.).

Doctorat en sciences appliquées
info:eu-repo/semantics/nonPublished

The current state of degradation of most archaeological collections has compromised the research and protection of this heritage. To respond to these problems, some initiatives that seek to modify the current practices of preservation of archaeological collections are emerging, as the fieldwork in the Charqueada Santa Barbara archaeological site ( Pelotas, RS, Brazil ), linked to the research project Pampa Negro: Arqueologia da Escravidão na Região Sul do Rio Grande do Sul (1780-1888), which has brought together a multidisciplinary team to talk about the praxis of each area and to think of appropriate solutions for the better management and protection of archaeological collections. In the context of the conservation, protocols for preventive and curative intervention of different types of materials were developed and tested in field and laboratory. Among the types of material recovered in the excavation, metal objects, especially iron, are those most susceptible to deterioration due to the process of recovery and to the speed at which the corrosive processes occur as well as the complexity of the products resulting from these. In this context, the aim of this study was to analyze, from a study of the interface between conservation and archeology, how the conservation procedures performed in the field and laboratory in the ferrous artifacts contributed to the preservation of archaeological collections. It was expected to verify which interventions enable a better conservation of archaeological origin and of the associated information material culture, and disseminate the need for greater integration between the experts related to the safeguard of the archaeological heritage areas. It was concluded that conservation practices directly assist in the preservation of archaeological collections in its material, documentary and symbolic aspects. Therefore, the conservator has become more of a manager of these collections, in a performance that, increasingly, is turning into an agent crucial to the management of the archaeological heritage.
O estado atual de degradação de grande parte dos acervos arqueológicos tem comprometido as pesquisas e a salvaguarda destes bens. Destas problemáticas vêm surgindo iniciativas que buscam a modificação das práticas atuais de preservação dos acervos arqueológicos, como o trabalho de campo do sítio Charqueada Santa Bárbara (Pelotas, RS, Brasil), vinculado ao projeto O Pampa Negro: Arqueologia da Escravidão na Região Meridional do Rio Grande do Sul (1780-1888), que reuniu uma equipe multidisciplinar a fim de dialogar a respeito da práxis de cada área e pensar de forma conjunta soluções adequadas para um melhor gerenciamento e salvaguarda dos acervos arqueológicos. No âmbito da conservação, foram elaborados e testados em campo e em laboratório protocolos de intervenção preventiva e curativa para distintos materiais. Dentre os materiais recuperados na escavação, os objetos metálicos, em especial os de ferro, estão entre aqueles mais suscetíveis à deterioração decorrente deste processo, em função da velocidade em que ocorrem os processos corrosivos e da complexidade destes. Neste contexto, o objetivo da presente pesquisa foi analisar, a partir de um estudo da interface entre Conservação e Arqueologia, de que forma os procedimentos de conservação realizados em campo e em laboratório nos artefatos em ferro contribuíram para a preservação dos acervos arqueológicos. Almejou-se verificar as intervenções que possibilitam a melhor conservação da cultura material de origem arqueológica e da informação associada, e difundir a necessidade de uma maior integração entre os especialistas das áreas relacionadas à salvaguarda do patrimônio arqueológico. Concluiu-se que as práticas de conservação auxiliam diretamente na preservação dos acervos arqueológicos, em suas instâncias material, documental e simbólica. O conservador vem se configurando, portanto, como mais um gestor destes bens, em uma atuação que, cada vez mais, se torna indispensável ao gerenciamento do patrimônio arqueológico.

A liga de alumínio designada AA4006 é muito utilizada na indústria. É uma liga do sistema Al-Fe-Si, com teores (% em massa) de Si na faixa de 0,8 a 1,2% e Fe entre 0,5 e 0,8%. Apesar de ser bastante utilizada, ela foi pouco estudada. Neste trabalho foi realizado um estudo comparativo da microestrutura e da textura cristalográfica entre chapas da liga AA4006 produzidas por dois processos industriais de lingotamento: contínuo (Twin roll caster TRC) e semicontínuo (Direct chill DC). Para a caracterização microestrutural, foram utilizadas as técnicas de microscopia óptica com luz polarizada, microscopia eletrônica de varredura com microanálise química, medidas de condutividade elétrica e ensaios de dureza Brinell. A textura cristalográfica foi determinada por difração de raios X. Foram detectadas e discutidas diferenças significativas nas morfologias e distribuições de grãos e de partículas de fases intermetálicas. O estudo da textura cristalográfica foi realizado ao longo da espessura das tiras e os resultados mostraram variações significativas da textura entre as chapas ao longo da espessura. A chapa produzida por lingotamento contínuo apresentou uma típica textura de cisalhamento nas proximidades de sua superfície, enquanto nas regiões mais internas a fibra foi observada. O estudo da recristalização de chapas metálicas laminadas a frio é muito útil para a obtenção da temperatura de amolecimento do material submetido a um tratamento térmico. Tratamentos térmicos isócronos no intervalo de uma hora foram feitos em amostras das duas chapas e a chapa produzida pelo processo TRC apresentou a temperatura para 50% de recristalização em torno de 290 ºC e a amostra da chapa produzida pelo processo DC em torno de 270 ºC. A textura cristalográfica pode mudar com a recristalização e com a laminação do metal. Utilizando estas etapas de processamento do material, a orientação dos grãos de uma tira metálica pode ser otimizada, a fim de, por exemplo, melhorar a estampabilidade de chapas na obtenção de um dado produto com valor agregado. Neste trabalho as curvas de amolecimento para duas chapas produzidas por lingotamento contínuo e lingotamento semicontínuo da liga de alumínio AA4006 também foram determinadas e comparadas. Embora as diferenças detectadas entre as curvas de amolecimento tenham sido pequenas, foi possível verificar que a recristalização da chapa produzida por twin roll caster TRC ocorre em temperaturas mais elevadas do que na chapa produzida pelo processo direct chill DC. Resultados da textura cristalográfica em amostras destas chapas (laminadas e recozidas) foram obtidos utilizando difração de raios X e difração de elétrons retroespalhados EBSD. Estes resultados indicaram a presença da textura de cisalhamento na superfície e a fibra no centro da amostra laminada a frio (70% de redução) da chapa obtida por lingotamento contínuo. Na amostra da chapa obtida por lingotamento semicontínuo, a componente cubo e a fibra foram vistas na superfície e no centro. Uma textura fraca com grãos orientados ao acaso foi vista nas duas amostras (TRC e DC) recristalizadas das duas chapas, possivelmente, devido à nucleação estimulada por partículas. A fibra desapareceu nas amostras (TRC e DC) recristalizadas.
AA4006 Aluminum alloy is extensively used in industry. It belongs to the Al-Fe-Si system, with Si between 0,8 and 1,2 % mass, and Fe between 0,5 and 0,8 % mass. This alloy is less studied despite its extensive use. A comparative microstructural study has been performed in as-received AA4006 alloy strip produced by two industrial casting processes: twin roll caster (TRC) and direct chill (DC). Polarized optical microscopy, scanning electron microscopy with microanalysis, electrical conductivity measurements and Brinnel hardness tests have been used for microstructural characterization. Significant differences in the grain and intermetallic particle sizes, morphologies and distributions were detected and are discussed. Thermal treatments effects on the silicon content in solid solution were also studied. Crystallographic textures have been also determined. Textures across thickness of both sheets have been analyzed and compared. Results showed significant texture changes across thickness of the specimens. Texture analysis was carried out using X-ray diffraction technique. Twin roll caster (TRC) sheet presented the typical shear texture near the surface, while, in internal regions, the -fibre was observed. A recrystallization study of cold rolled metallic sheets is very important to obtain softening temperature for the material during annealing. After cold rolling with 70% of reduction in thickness, followed by isochronous heat treatments, the samples of the two sheets produced by TRC and DC presented a 50% recrystallization temperature around 290 ºC and 270 ºC, respectively. Crystallographic texture can change during the metal rolling and recrystallization. These processing steps can optimize the grain orientation distribution in a metal strip to improve, for instance, the stamping process, in order to obtain an aggregated value product. Softening curves were also compared and determined for the two sheets (rolled and annealed) of the AA4006 aluminum alloy produced by twin roll caster TRC and direct chill DC processes. It was detected that the recrystallization of the strip produced by TRC process occurs at a higher temperature than that for the DC process, despite the little differences in their softening curves. Crystallographic texture results, for the sheet samples, were obtained by using X-ray diffraction and electron back scatter diffraction EBSD techniques. These results indicated the shear texture presence on the surface and fiber at the center of the cold rolled (70% area reduction) sample for the sheet produced by TRC process. In the sheet sample produced by the DC process, under the same conditions, the cube component and fiber texture (at the surface and at the center) were observed. A texture with random oriented grains was detected in two deformed and recrystallized samples of the two sheets (TRC and DC). It is suggested that this texture occurs due to the particle stimulated nucleation. There was fiber absence in the recrystallized samples (TRC and DC).

Thesis (Sc.D.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 1985.
MICROFICHE COPY AVAILABLE IN ARCHIVES AND SCIENCE.
Vita.
Includes bibliographical references.
by Keith Allen Taylor.
Sc.D.

Tese (doutorado) - Universidade Federal de Santa Catarina, Centro Tecnológico. Programa de Pós-Graduação em Engenharia Elétrica.
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In one of the facilities at the Stena Recycling plant in Halmstad, Sweden, about 300 tonnes of metallic waste is processed each day with the aim of sorting out all non-ferrous material. At the end of this process, non-ferrous materials are manually sorted out from the ferrous materials. This thesis investigates a computer vision based approach to identify and localize the non-ferrous materials and eventually automate the sorting.Images were captured of ferrous and non-ferrous materials. The images areprocessed and segmented to be used as annotation data for a deep convolutionalneural segmentation network. Network models have been trained on different kinds and amounts of data. The resulting models are evaluated and tested in ac-cordance with different evaluation metrics. Methods of creating advanced train-ing data by merging imaging information were tested. Experiments with using classifier prediction confidence to identify objects of unknown classes were per-formed. This thesis shows that it is possible to discern ferrous from non-ferrous mate-rial with a purely vision based system. The thesis also shows that it is possible to automatically create annotated training data. It becomes evident that it is possi-ble to create better training data, tailored for the task at hand, by merging image data. A segmentation network trained on more than two classes yields lowerprediction confidence for objects unknown to the classifier.Substituting manual sorting with a purely vision based system seems like aviable approach. Before a substitution is considered, the automatic system needsto be evaluated in comparison to the manual sorting.

Heusler based functional or smart materials are a deep well of solutions to future energy, heat transport and mechanization problems. The half-metallic ferromagnetic nature of these crystalline intermetallic compounds is the source of their extraordinary properties. The loss of this magnetic ordering places limits on the range of application temperatures making knowledge of the Curie point of these novel materials essential for understanding of their limitations. High throughput continuous wavelet transform spectrum analysis of magnetic balance data generated on a custom modified Setaram Setsys Evolution 16/18 Differential Scanning Calorimeter-Differential Thermal Analyzer with simultaneous Thermogravimetric Analyzer was performed on select Fe, Co and Mn based Heusler compounds. The phase stability of Co-Fe-Si compounds is explored in relation to the high-Curie Temperature Co2FeSi and Fe2CoSi compounds via generation of equilibrium ternary isothermal phase diagrams at 1160 °C and 800 °C to enable greater control of the microstructure for future thermomechanically processed bulk smart device fabrication.

Les matériaux caloriques à l'état solide, qui subissent un changement de température adiabatique ou un changement d'entropie isothermal lorsque certains stimuli externes (champ électrique, champ magnétique, contrainte ou pression mécanique) est appliquée ou retirée, sont prometteurs pour la réfrigération à l'état solide, comme alternative aux dispositifs de refroidissement conventionnels inventé il y a cent ans qui utilisent des gaz dangereux. Compte tenu des améliorations des systèmes de réfrigération à compression de vapeur approchant très vite de leur limite d'efficacité théorique, en plus des préoccupations environnementales accrues, il y a eu récemment une recrudescence de la recherche mondiale pour de nouvelles solutions de réfrigération plus économiques et respectueuses de l'environnement. Les caloriques les plus importants sont les matériaux "ferroiquement" ordonnés (ferroélectriques, ferroélastiques et ferromagnétique / antiferromagnétique) qui présentent souvent des effets caloriques géants près de leurs transitions ferroïques. Dans cette thèse, nous présentons nos résultats théoriques et expérimentaux sur l'effet électrocalorique, élastocalorique, barocalorique et magnétocalorique dans différents matériaux ferroïques. Nos résultats montrent que tous ces effets caloriques peuvent donner des solutions de réfrigération prometteuses avec un faible impact environnemental. Nous abordons les ferroélectriques qui apparaissent comme matériaux idéaux permettant à la fois des réponses électrocaloriques, élastocaloriques et barocaloriques géantes près de la température ambiante. Pour la première fois, nous mettons en évidence un effet électrocalorique négatif dans des films minces antiferroélectriques et nous proposons un nouveau mécanisme pour comprendre la réponse calorique dans antiferroiques en général incluant antiferroélectrique et antiferromagentique. Par ailleurs, pour la première fois en utilisant une caméra infra-rouge, nous effectuons la mesure résolue spatialement sur l'effet électrocalorique dans des condensateurs multicouches, l'un des systèmes les plus étudiés considérés comme le prototype électrocalorique le plus prometteur. Nos résultats fournissent la première preuve expérimentale directe sur le flux de chaleur électrocalorique à la fois temporellement et spatialement dans un dispositif électrocalorique spécifique. En outre, pour la première fois, nous concevons un cycle de réfrigération multicalorique combinant effet électrocalorique avec des effets élastocaloriques / magnétocaloriques via des matériaux ferroélectriques. Nous avons réalisé ce cycle mutlicalorique pour résoudre un problème réel et de longue date, à savoir une grande hystérésis magnétique qui a empêché l'utilisation pourtant prometteuse de FeRh découvert il y a près de 26 ans en tant que matériau magnétocalorique. Nous espérons que cette thèse fournira non seulement des connaissances utiles pour comprendre fondamentalement l'effet calorique à l'état solide dans les matériaux ferroïques et ce qui est véritablement mesuré, mais pourra aussi servir de guide pratique pour exploiter et développer les ferrocalorics vers la conception de dispositifs appropriés
Solid-state caloric materials, which undergo an adiabatic temperature change or isothermal entropy change when some external stimulus (electric field, magnetic field, stress and pressure) is applied or withdrawn, are promising for solid-state refrigeration, as an alternative to hazardous gases used in conventional cooling devices invented a hundred years ago. Given that the highly refined vapor-compression refrigeration systems asymptotically approach their theoretical efficiency limit in addition to the concern on environment, there has been a recent upsurge in worldwide search for new refrigeration solution which is economical and environmentally friendly. The most prominent calorics are ferroically ordered materials (ferroelectric, ferroelastic and ferromagnetic/antiferromagentic) that often exhibit giant caloric effects near their ferroic transitions. In this thesis, we present our theoretical and experimental results on electrocaloric effect, elastocaloric effect, barocaloric effect and magnetocaloric effect in different ferroic materials. Our findings show that all these caloric effects may appear promising with low environmental impact. We address ferroelectrics emerging as ideal materials which permit both giant elastocaloric, electrocaloric and barocaloric responses near room temperature. For the first time, we find a large negative electrocaloric effect in antiferroelectric thin films and we propose a new mechanism to understand the caloric response in antiferroics including antiferroelectric and antiferromagentic. In addition, for the first time using Infra-red camera we carry out spatially-resolved measurement on electrocaloric effect in multilayer capacitors, one of the most studied systems which are regarded as the most promising electrocaloric prototype. Our findings provide the first direct experimental evidence on the electrocaloric heat flux both temporally and spatially in a specific electrocaloric device. Moreover, for the first time, we design a multicaloric refrigeration cycle combining electrocaloric effect with elastocaloric/magentocaloric effects bridged by ferroelectric materials. We realized such mutlicaloric cycle to solve a real and longstanding problem, i.e., a large hysteresis that impeded reversibility in an otherwise promising magnetocaloric material FeRh discovered almost 26 years ago. We hope that this thesis will not only provide a useful background to fundamentally understand the solid-state caloric effect in ferroics and what we are really measuring, but also may act as a practical guide to exploit and develop ferrocalorics towards design of suitable devices

This thesis investigates the possibility of utilizing data from multiple modalities to enable an automated recycling system to separate ferrous from non-ferrous debris. The two methods sensor fusion and hallucinogenic sensor fusion were implemented in a four-step approach of deep CNNs. Sensor fusion implies that multiple modalities are run simultaneously during the operation of the system.The individual outputs are further fused, and the joint performance expects to be superior to having only one of the sensors. In hallucinogenic sensor fusion, the goal is to achieve the benefits of sensor fusion in respect to cost and complexity even when one of the modalities is reduced from the system. This is achieved by leveraging data from a more complex modality onto a simpler one in a student/teacher approach. As a result, the teacher modality will train the student sensor to hallucinate features beyond its visual spectra. Based on the results of a performed prestudy involving multiple types of modalities, a hyperspectral sensor was deployed as the teacher to complement a simple RGB camera. Three studies involving differently composed datasets were further conducted to evaluate the effectiveness of the methods. The results show that the joint performance of a hyperspectral sensor and an RGB camera is superior to both individual dispatches. It can also be concluded that training a network with hyperspectral images can improve the classification accuracy when operating with only RGB data. However, the addition of a hyperspectral sensor might be considered as superfluous as this report shows that the standardized shapes of industrial debris enable a single RGB to achieve an accuracy above 90%. The material used in this thesis can also be concluded to be suboptimal for hyperspectral analysis. Compared to the vegetation scenes, only a limited amount of additional data could be obtained by including wavelengths besides the ones representing red, green and blue.

O aço especial UNS S31254 (aço 254), um aço inoxidável austenítico contendo 20,1% de cromo, 18,4% de níquel e 6,42% de molibdênio foi estudado com o objetivo de ser aplicado em técnicas eletroanalíticas, tais como a potenciometria, a condutimetria e como eletrodo indicador em medidas de pH. Os estudos eletroanalíticos foram precedidos de curvas de polarização potenciostáticas e potenciodinâmicas e de ensaios não eletroquímicos (FTICR, MEV e XPS), em que se caracterizou a presença do filme passivante. Grande parte dos estudos incluíram, para efeito de comparação, os aços UNS S 31603 (aço 316 L) e UNS S31678 (aço F 138), o primeiro de largo emprego comercial e o último, aplicável em implantes ortopédicos. Os estudos, realizados a 25° C, se iniciaram com a caracterização eletroquímica dos referidos materiais imersos em meios aquosos de ácidos clorídrico, acético, nítrico, sulfúrico e galacturônico, e dos sais cloreto de sódio, sulfato de sódio e nitrato de sódio, variando-se a concentração do eletrólito. O aço 254 se mostrou passivado, na grande maioria dos meios estudados, em toda a faixa de potenciais que se estende do potencial de corrosão (Ecorr, potencial de circuito aberto estacionário) até o potencial de transpassivação (onde ocorre o rompimento do filme e, na maioria dos meios, a oxidação generalizada da superfície e a reação H2O/O2). Em meio de ácido acético a faixa de potencial em que o referido aço se mantém passivado é a mais ampla, indicando que o rompimento do filme passivo exige maior energia, em virtude do maior teor de molibdênio superficial detectado por MEV. A corrosão por pite foi observada em meios de HCI e de NaCI a potenciais mais positivos do que o de transpassivação. A caracterização da superfície por MEV mostrou que as inclusões presentes no aço são constituídas basicamente de óxidos de alumínio e de cálcio. A análise por XPS da superfície do aço 254 apenas polido e exposto ao ar revelou a presença de Mo (VI) na superfície; em meio de NaCI 0,15 mol L-1 há o enriquecimento gradual de Mo (VI) quando se varia o potencial desde o Ecorr, passando por um potencial passivo e se estendendo a um potencial 50 mV acima do potencial de transpassivação. O aço 254 pode ser empregado em substituição à platina em todas as determinações eletroanalíticas realizadas neste trabalho, envolvendo titulações potenciométricas, medidas condutimétricas e determinação de pH. Em medidas de pH em sistemas com força iônica mais baixa, entretanto, é necessário um controle mais adequado do tratamento superficial, além dos realizados neste trabalho, para que a resposta do petencial seja mais rápida. Estes estudos podem contribuir para baixar o custo de análises industriais e de experimentos que venham a ser realizados em laboratórios diáticos.
Special UNS S31254 stainless steel (254 SS), an austenitic stainless steel with 20.1% Cr, 18.4% Ni and 6.42% Mo has been studied in order to be applied in electroanalytical techniques as potentiometry, conductimetry and as a sensor in pH measurements. The electroanalytical studies were preceded of potentiostatic and potentiodynamic polarization curves. The surface characterization was made using FTCIR, SEM and XPS as techniques. The studies have included, for comparison, UNS S 31603 (316 L SS) and UNS S31678 (F 138 SS); the former is commercially employed in a large extension and the latter is applicable in orthopedic implants. The experiments were made at 25° C, beginning with the electrochemical characterization of the ferrous materiais in different aqueous media: chloridric, acetic, sulfuric, nitric and D-galacturonic acids and saline solutions of sodium chloride, sodium sulfate and sodium nitrate, changing the electrolyte concentration. SS 254 is passivated in most of the studied media, on the entire potential range analyzed (from corrosion potential to transpassivation potential). In acetic media it was observed the largest potential range where 254 SS is passivated, indicating that a higher energy is necessary to disrupt the passivant film, due to a higher Mo concentration at the surface, detected using SEM. Pitting corrosion was observed in HCl and NaCl media at potential more positive than Etr. SEM surface characterizations have shown aluminium oxide and calcium oxide inclusions. XPS analyses have indicated the presence of Mo (VI) on the polished surface and that there is a gradual Mo (VI) increasing, in solution, when the potential changes from Ecorr to E > Etr. 254 SS can be used in potentiometric and conductimetric titrations and as a sensor electrode for pH measurements. However, in biological applications a more adequate surface treatment is needed in order to obtain rapid responses. Overall the results suggest that 254 can be used as substitute of platinum in different electroanalytical techniques. This finding contributes to lower the cost of experiments to be performed in didactic laboratories and/or industrial analyses.

As análises de tensões não-lineares por elementos finitos situadas no regime plástico do material demandam maior tempo de processamento computacional quando comparadas às análises lineares situadas no regime elástico. Os valores de tensões não-lineares podem ser obtidos por meio de metodologias analíticas de previsão de tensão aplicadas a componentes entalhados. Entre os métodos de obtenção de tensão em entalhes, destaca-se o método de Neuber. O presente trabalho visa avaliar a aplicação deste método aliado à análise de elementos finitos para a obtenção de tensões não-lineares em componentes automotivos fabricados em ferro fundido nodular contendo descontinuidades geométricas na superfície. Como referência foram utilizados valores de tensões obtidos através da técnica de extensometria, aplicados em dois diferentes modelos de alavancas contidas em transmissões de ônibus e caminhões. Todos os dados de entrada para os cálculos de elementos finitos foram obtidos através da caracterização do material por meio da realização de ensaios de dureza, tração e metalografia. A fim de verificar possíveis trincas ocasionadas pelos carregamentos aplicados, os componentes testados foram submetidos a ensaios de partículas magnéticas. Busca-se, assim, uma contribuição para a redução do tempo de desenvolvimento de novos produtos fabricados em componentes de ferro fundido nodular.
The analyzes of nonlinear stresses by finite elements located in the plastic regime of the material demand a longer time of computational processing when compared to the linear analyzes located in the elastic regime. The values of nonlinear stresses can be obtained by analytical methodologies of stress prediction applied to notched components. Among the methods of obtaining stresses in notches, the Neuber method is outstanding. The present work aims to evaluate the application of this method, combined with the finite element analysis to obtain nonlinear stresses in automotive components made of nodular cast iron containing geometric surface discontinuities. As reference, stress values obtained through the strain gauge technique were used, applied in two different shift levers contained in bus and truck transmissions. All input data for the finite element calculations were obtained through the characterization of the material by means of hardness, tensile and metallography tests. In order to verify possible cracks caused by the applied loads, the tested components were subjected to magnetic particle tests. Thus, a contribution is made to reduce the development time of new products manufactured in nodular cast iron components.

Esta tese apresenta o estudo sobre microconformação, no caso microextrusão de quatro materiais diferentes, um aço SAE 1020, um aço inoxidável AISI 304, um alumínio AA6531 e um latão ASTM C34000. Para avaliar o efeito do tamanho da peça sobre o processo de microextrusão, dois tamanhos de corpos de prova foram utilizados, um com ∅ 4 mm e outro com ∅ 1 mm. Para cada tamanho de corpo de prova, três ângulos de extrusão foram utilizados, 30°, 45° e 60°. A primeira parte do trabalho se resume a caracterização dos materiais, com analise química e metalográfica. Após a caracterização dos materiais, as curvas de escoamento através do ensaio de compressão utilizando dois tamanhos de corpos de prova foram feitos em todos os materiais. O atrito foi determinado utilizando o ensaio de anel de atrito com três tamanhos diferentes de corpos de prova. As curvas de calibração foram feitas utilizando o software SIMUFACT. Os ensaios de extrusão foram feitos em uma máquina de ensaio universal com capacidade de captura de dados como força e deslocamento. Um modelo matemático foi utilizado para comparar a força de extrusão calculada com o medido no processo. Os resultados indicam que as curvas de escoamento de tamanho macro podem ser aplicadas a peças de tamanho meso. O atrito medido pelo ensaio de anel de atrito mostrou que os valores de atrito de tamanho micro tem um pequeno valor maior que para tamanho macro. Os valores de força de extrusão calculada e medido no ensaio para peças de tamanho meso tem boa aproximação com diferença de 3,2% para o aço inoxidável. Para peça de tamanho micro, a diferença entre o valor medido e o calculado aumenta chegando a diferença de 995% para o corpos de prova de aço comum.
This thesis presents the study about microforming, in this case microextrusion of the four different materials, an SAE 1020 steel, an AISI 304 stainless steel, an AA6531 aluminum and a C34000 brass. To evaluate the size effect about microextrusion process, two sizes of specimens were used, with a ∅ 4 mm and another with ∅ 1 mm. For each size of specimen, three extrusion angles were used, 30 °, 45 ° and 60 °. The first part of the work was to materials characterizations with chemical and metallographic analysis. Following the materials characterization, the flow stress curves was made using the compression test with two sizes of specimens. The friction was determined using the friction ring test with the three different size. Calibration curves were performed using the software SIMUFACT . The extrusion tests were performed in a universal testing machine capable of capturing such as force and displacement data. A mathematical model was used to compare the extrusion force it was calculated and the force measured in microextrusion. The results indicate that the flow stress curves of macro size can be applied to meso sizes. The ring friction test indicate that the friction values of the micro size has a small value greater than macro size. The extrusion force calculated and measured in the test to meso size has good approximation with a difference of 3.2% in the stainless steel. To pieces of the micro size, the difference between the measured and calculated force increases 995% for the samples of SAE 1020 steel.

The effect of the thermal properties of alumina and CBN abrasives on workpiece temperatures in grinding was investigated. A review of the literature revealed a lack of knowledge of the thermal properties of CBN limiting the accuracy of theoretical predictions of the heat conduction in CBN grinding. A grain contact analysis was developed to predict the energy partitioning between the workpiece and wheel. The analysis takes into account two dimensional transient heat transfer in the grain and maintains temperature compatibility at the grain wear flatworkpiece interface. The proportion of the total grinding energy entering the workpiece, termed the partition ratio, was estimated by correlating measured temperature distributions with theoretical distributions. The partition ratios when grinding with CBN were substantially lower than grinding with alumina wheels for a range of ferrous materials. The lower partition ratios with CBN grinding were attributed to the higher thermal conductivity of the CBN abrasive. The effective thermal conductivity of alumina and CBN grains were quantified by correlating the theoretical partitioning model with the measured results. The effective thermal conductivity of CBN was found to be considerably lower than the reported theoretical value albeit much higher than the effective thermal conductivity of alumina. A model to predict the background temperature in grinding was proposed based on the experimental findings. The thermal model takes into account a triangular heat flux distribution in the grinding zone, the real length of contact and experimentally validated grain thermal properties. The input parameters to the thermal model were specified. To avoid temper colours on the workpiece surface the maximum background temperature must not exceed 450 to 500deg. C. for commonly used ferrous materials.

O aço carbono vem sendo largamente utilizado na indústria de construção em geral, devido a sua resistência mecânica e baixo custo. Entretanto, devido a sua fraca resistência à corrosão são necessários estudos de diferentes métodos de proteção contra a corrosão. Sendo assim, no presente trabalho, o método de proteção contra a corrosão abordado foi o de aplicação de filmes poliméricos condutores mediante a utilização de pré-tratamentos de conversão com ácido fítico (HP), banho de sal de cério/peróxido de hidrogênio (Ce) e a combinação HP-Ce, para aumentar a resistência à corrosão e a aderência de filmes poliméricos. Essa aderência devido à importância frente os processos de corrosão foi quantificada com técnicas específicas de estudo de corrosão, nomeadamente, potencial de circuito aberto (PCA) e polarização potenciodinâmica (PP) em meio NaCl 0,6 mol/L aerado. Os revestimentos poliméricos usados foram a polianilina (PAni), poli-o-metoxianilina (POMA) e blenda de PAni-POMA sintetizados em meio de HP e de H2SO4. A caracterização feita por UV-Vis e FTIR mostrou que foi possível sintetizar os referidos polímeros, e SEM revelou morfologia compacta e granular. O comportamento eletroquímico das amostras foi investigado por OCP e PP em NaCl 0,6 mol/L antes e após 2 h de exposição no ambiente salino. Quando os revestimentos foram aplicados em substratos de aço carbono AISI 1020 sem pré-tratamentos, antes de exposição em solução salina, os resultados mostraram boa resistência e eficiência na proteção à corrosão devido a menor perda de adesão e maior efeito barreira. Após 2 h de exposição em solução salina, os resultados mostraram que a resistência e a eficiência na proteção à corrosão diminuiu de uma forma mais acentuada para PAni, POMA e menos para blenda de PAni-POMA sintetizados em meio de HP e de H2SO4, devido à perda de aderência provocada pela infiltração do eletrólito corrosivo através de poros dos filmes poliméricos. Com o intuito de aumentar a aderência dos revestimentos, pré-tratamentos do aço carbono AISI 1020 foram feitos com HP, Ce e HP-Ce e, constatou-se que a perda de aderência dos revestimentos de PAni, POMA e blenda de PAni-POMA aplicados sobre as amostras pré-tratadas com Ce e HP-Ce foi menor, e com HP foi maior comparada com a amostra sem pré-tratamento. Além disso, os revestimentos de blenda de PAni-POMA, apresentaram em todas amostras sem e com pré-tratamentos melhor desempenho em relação a PAni e POMA.
Carbon steel has been widely used in the construction industry in general, due to its mechanical and low cost resistance. However, due to their low corrosion resistance are required studies of different methods of protection against corrosion. Therefore, in this study, the method of carbon steel AISI 1020 protection against corrosion was dealt with the application of polymeric film conductors using pre-treatments conversion with phytic acid (HP), cerium salt/hydrogen peroxide (Ce) bath and a combined HP-Ce, to increase the corrosion resistance and the adhesion of polymeric films. This adhesion is due to the importance forward corrosion processes, was quantified with specific corrosion study techniques in particular, open circuit potential (OCP) and potentiodynamic polarization (PP) in medium NaCl 0.6 mol/L aerated. Polymeric coatings used were the polyaniline (PAni), poly-o-anisidine (POMA), and blends of polyaniline-poly-o-anisidine (Pani-POMA) synthesized in phytic (HP) and sulfuric (H2SO4) acid means. The characterizations made by UV-Vis and FTIR showed that it was possible to synthesize said polymers, and SEM revealed compact and granular morphology. The electrochemical behaviors of the samples were investigated using OCP and PP in 0.6 mol/L NaCl solutions, before and after 2 h of exposure in saline environment. When polymers coatings were applied to carbon steel AISI 1020 without pretreatments, before of exposure in saline environment, results showed good resistance and high efficient corrosion protection due to less loss of adhesion coatings consequently, high barrier effect. After 2 hours of exposure in saline environment, the results showed that the resistance and efficient corrosion protection decreased largely for PAni, POMA and less for blends of PAni-POMA, due to loss of adhesion caused by the infiltration of corrosive electrolyte pores through the polymer matrix. In order to increase the adhesion of Pani, POMA and blends of Pani-POMA coatings, carbon steel pretreatments were made with HP, Ce and a combined HP-Ce, and found that the loss of adhesion of coatings applied to the pretreated samples with Ce and HP-Ce was lower, and with HP was higher compared to the sample without pretreatment. Moreover, blend of Pani-POMA coating showed in all samples, treated and untreated better performance than PAni and POMA.

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The amorphizable ferrous alloys and/or nanocrystalline ones have high hardness properties and wear resistance which are important technologically. Rapid solidification process with cooling rate between 102 - 106 K/s leads to high hardness properties and wear resistance. The objective of this work is the study and the characterization of microstructure and hardness of white cast iron and nodular gray by rapid solidification, exploring techniques that impose different cooling rates, with different additions of Boron and addition or not of Niobium. The alloys were processed by Discovery® Plasma and melt-spinning, namely: (Fe65Cr17Mo2C14Si2)100-xBx (Fe65Cr17Mo2C14Si2)88B8Nb4 and (Fe75Nb6C10Si4)100-xBx (at%). The characterization was made by X-ray diffraction (XRD), differential scanning calorimetry (DSC), optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Vickers microhardness (HV). The (Fe65Cr17Mo2C14Si2)88B8Nb4 (at%) alloy was selected to spray forming and laser cladding processes obtaining deposit and overspray powders into different particle size from 20 μm and more than 180 μm. The alloys were copper mold cast resulting in plate samples with thickness of 1.0 and 2.0 mm. The cast iron plate microhardness, without Boron and Niobium, showed around 650 HV and about 1400 HV after the addition of 12 at% of Boron. The (Fe65Cr17Mo2C14Si2)88B8Nb4 (at%) alloy has nanocrystalline microstructure after spray forming in the deposit and overspray powders and Vickers microhardness value of about 1040 HV in the deposit. For these alloys it was required high cooling rates of about 106 K/s to obtain amorphous phase by melt-spinning process. The laser cladding process used overspray powders to produce coatings with microhardness up to around 1300 HV. It was possible using power 200 W, in slower scanning travel speeds (6.7 or 10.0 mm/s). The laser cladding process presented good perspectives of application in order to produce wear abrasion and corrosion resistant coatings.
Ligas ferrosas amorfizáveis e/ou nanocristalinas apresentam propriedades como alta dureza e resistência ao desgaste, o que as torna interessantes tecnologicamente, A via de processamento por solidificação rápida, com taxas de resfriamento entre 102 – 106 K/s garante esta alta dureza e resistência ao desgaste. O objetivo do presente trabalho é o estudo e caracterização da microestrutura e microdureza do ferro fundido branco e cinzento nodular através da solidificação rápida, explorando técnicas de solidificação rápida sob diferentes taxas de resfriamento, diferentes teores de boro e adição ou não de nióbio. As ligas foram processadas via Discovery® Plasma e melt-spinning, sendo elas: (Fe65Cr17Mo2C14Si2)100-xBx, (Fe65Cr17Mo2C14Si2)88B8Nb4 e (Fe75Nb6C10Si4)100-xBx. A caracterização foi feita por difração de raios-X, calorimetria diferencial de varredura, microscopia ótica, microscopia eletrônica de varredura e de transmissão, além de microdureza Vickers. Selecionou-se para a conformação por spray e Laser Cladding a liga (Fe65Cr17Mo2C14Si2)88B8Nb4, obtendo depósito e pós overspray em diferentes granulometria, a partir de 20 μm e superior a 180 μm. A fundição em coquilha de cobre na forma de chapas com espessuras de 1,0 e 2,0 mm apresentaram aumento na microdureza de aproximadamente 650 HV, sem Boro, para aproximadamente 1400 HV, com adição de 12%at. boro. A conformação por spray da liga (Fe65Cr17Mo2C14Si2)88B8Nb4 (%at.) apresentou microestrutura nanocristalina no depósito e no pó overspray e valor de microdureza Vickers de aproximadamente 1040 HV no depósito por spray. Para as ligas estudadas foram necessárias altas taxas de resfriamento, impostas por melt-spinning, aproximadamente 106 K/s, para obtenção de fase amorfa. O processamento através de laser cladding a partir do pó overspray levou à microdureza Vickers de 1300 HV, aproximadamente, com potência Laser de 200 W utilizando menores velocidades de varredura, notadamente 6,7 ou 10,0 mm/s, mostrando boas perspectivas de aplicações como recobrimentos resistentes ao desgaste e corrosão através laser cladding.

Inspection of non-ferrous cast material is routinely carried out looking for casting defects inherent for the manufacturing process. The NDT methods employed are Radiography and Ultrasonics, primarily for sub-surface or internal defects and Penetrants fo r surface breaking defects. Electromagnetic techniques have not been used on cast material except maybe for conductivity determination. This limitation resulting fi7om the surface roughness normally associated with cast surfaces and the fact the other techniques mention above have been very successful in finding and evaluating the discontinuities sought. The possible application of Electromagnetic techniques on surfaces in the as-cast condition of non-ferromagnetic material came about because of specific problems experienced by industry. Two major investigations were offered namely; 1) Investigation of CNC material - CuNiCr [1.6%Cr] castings exhibiting oxide entrapment in the form of networks. 2) Investigation of NAB - Nickel Aluminium Bronze exhibiting selective phase corrosion on immersion in seawater. The detection and measurement of both oxide entrapment and phase selective corrosion was difficult and in cases impossible with conventional NDT methods employed for quality control of these material/component types. Time of Flight DiMaction Ultrasonics did give some 50% detectability of phase selective corrosion, but the method was found to be expensive and very time consuming. The metallurgical properties of the material and morphology of the defects have been studied for both Cupro Nickel Chromium and Nickel Aluminium Bronze cast alloys. An investigation was then conducted to study the effects of eddy current signals and their potential in detecting, both linear and cluster type defects which were predominantly interdendritic with some reported as intergranular in nature. For inspecting Cupro Nickel Chromium castings two successful eddy current methods have been developed. Detection of surface flaws was achieved by high frequency [2MHzj examination and subsurface flaws by using low frequencies [1--'IKHz] but using specifically developed sensors that provided good penetration but maintained sensitivity to the fine defects. In the case of Nickel Aluminium Bronze material, the investigation was to look at electromagnetic techniques, which best utilizes the inherent feature of permeability/conductivity associated with this non- ferromagnetic material and any changes that phase selective corrosion may produce. Some meaningful results were obtained using a combination of edd'y current excitation with detection via magneto -re s istive sensors. Testing through 30-40mm of material to detect small magnetic variation produced by only 1-2 mm of corrosion penetration was difficult to quantify. Detection and assessment however appeared hopeful when examination was carried out from the corroded surface. With quantifiable samples a meaningful technique using eddy current excitation and magneto-resistive sensor for detection can be developed.

Using piezoelectric materials to harvest energy from human movement provides a potential power source to wearable devices and electronic textiles in everyday life. Two common comerical piezoelectric material: lead zirconate titante (PZT) and polyvinylidene fluoride (PVDF) are unsuitable for human body energy harvesting applications due to the high hardness and fragility of PZT and the low piezoelectric coefficients of PVDF. Ferroelectret is a thin polymer foam that can store electric charges in its internal voids, have strong piezoelectric properties and low elastic modulus which would make them very desirable for human body energy harvesting. The piezoelectricity of ferroelectrets originates from the combination of the internally stored charges and the cellular structures. However, the resulting pizoelectric properties of commercialized ferroelectrets are limited by the random individual void geometry and irregular overall cellular structure due to its existing fabrication processes. This work develop a numerical model using finite element analysis (FEA) approach to design and optimize the structure of ferroelectret during fabrication. Based on the models, we used polydimethysiloxane (PDMS) materials to fabricate ferroelectrets with different internal structures. The fabrication is done by casting method with 3D-printed moulds and silicon moulds produced using MEMS processes. The piezoelectric properties of fabricated PDMS ferroelectret are investigated to further validate the accuracy of our proposed numerical model in the work. The designed PDMS ferroelectret presented a maximum piezoelectric coefficient d33 of 520 pC/N. It can provide the maximum output voltage of 13 V and average output of 2.73 μW when connected to a 65 MΩ resistive load under acompressive force of 800 N at human normal walking model. The optimization PDMS ferroelectret strucutre for human body energy harvesting is also evaluated. In addition, a method for further improving the PDMS ferroelectret piezoelectric stability is proposed.

Doutoramento em Fisica
This thesis presents the results of perturbed angular correlation (PAC) experiments , an experimental technique which measures the hyperfine interaction at probes (radioactive ions implanted in the materials to study), from which one infers local information on an atomic scale. Furthermore, abinitio calculations using density functional theory electronic obtain results that directly complement the experiments, and are also used for theoretical research. These methods were applied in two families of materials. The manganites, with the possible existence of magnetic, charge, orbital and ferroelectric orders, are of fundamental and technological interest. The experimental results are obtained in the alkaline-earth manganites (Ca, Ba, Sr), with special interest due to the structural variety of possible polymorphs. With probes of Cd and In the stability of the probe and its location in a wide temperature range is established and a comparison with calculations allows the physical interpretation of the results. Calculations of hyperfine properties in rare-earth manganites are also presented. The second type of materials in which hyperfine properties were studied are the Manganese pnictides: MnAs, MnSb, and MnBi, compounds in which magnetism is fundamental. The experimental results obtained mainly consider the MnAs compound, whose magneto-structural transition is of great interest. The transition is analyzed in detail with the local resolution characteristic of the technique, obtaining information of the character of the transition also with complementary, more conventional techniques. The last work in this thesis uses only the first principles calculations, continuing the theme of the hyperfine interactions, but this time with respect to ferroelectrics. Several transition metal oxides with perovskite or distorted structures are considered. The electric field gradient which exists due to the quadrupole interaction in nuclei is related to the spontaneous electric polarization, the main quantity measured in ferroelectrics. This study provides a fundamental theoretical basis for previous empirical studies, suggesting new directions for research in ferroelectrics and multiferroics using techniques which measure the electric field gradient.
Esta tese apresenta os resultados de experiências de correlações angulares perturbadas (PAC), uma técnica experimental que mede as interacções hiperfinas em sondas - iões radioactivos implantados nos materiais a estudar, o que permite inferir informação local à escala de dimensões atómicas. Foram também utilizados cálculos ab-initio utilizando a teoria de funcionais da densidade electrónica, obtendo resultados que complementam directamente as experiências, e outros resultados também usados para investigação teórica. Estes métodos foram aplicados em duas famílias de materais. As manganites, com a possível existência de ordens magnéticas, de carga, orbital e ferroeléctrica, têm interesse fundamental e tecnológico. Cálculos iniciais na manganite de Ca provam a sua utilidade como complemento de experiências PAC neste tipo de materiais. Os resultados experimentais são depois obtidos nas manganites de terra-alcalina- Ba e Sr, com especial interesse estrutural devido à variedade de polimorfos possíveis. Com as sondas de Cd e In conseguiu-se estabelecer localização dos iões de sonda e a sua estabilidade num intervalo de temperatura grande, e uma comparação com os cálculos permite a interpretação mais aprofundada dos resultados. Cálculos das propriedades hiperfinas nas manganites de terras-raras também são apresentados. O segundo tipo de materiais em que foram estudadas as propriedades hiperfinas são os pnictídeos de Manganês: MnAs, MnSb, e MnBi. Os resultados experimentais obtidos consideram principalmente o MnAs, cuja transição magneto-estrutural tem maior interesse. A transição foi estudada em detalhe com a resolução local da técnica, com a obtenção de informação do carácter da transição, também com o complemento de outras técnicas mais convencionais. O último estudo desenvolvido nesta tese utiliza apenas os cálculos de primeiros princípios, continuando com o tema das interacções hiperfinas, mas desta vez em relação com a ferroelectricidade. São considerados vários óxidos com metais de transição com estruturas de perovskite ou distorcidas. O gradiente de campo eléctrico existente devido à interacção quadrupolar nos núcleos é relacionado com a polarização eléctrica espontânea, que é a principal quantidade medida em ferroeléctricos. Este estudo dá uma base fundamental teórica a alguns estudos empíricos antigos, sugerindo novas direcções de investigação em ferroeléctricos e multiferróicos utilizando técnicas de medida do gradiente de campo eléctrico.

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior
Neste trabalho, foram estudadas por espectroscopia MÃssbauer matÃrias primas de geopolÃmeros. Para motivar o trabalho sÃo apresentados resultados de espectroscopia MÃssbauer de um solo e uma concreÃÃo laterÃtica e os respectivos geopolÃmeros produzidos a partir deles. Para estudar a estrutura do ferro nas caulinitas e metacaulinitas, principais matÃrias primas geopolimÃricas, foram estudadas caulins vermelhos naturais com ocorrÃncia natural de ferro em sua estrutura e caulinitas brancas dopadas com ferro atravÃs de reaÃÃes de incorporaÃÃo em ambientes alcalinos. Os espectros MÃssbauer das amostras de caulim vermelho apresentaram um dubleto paramagnÃtico de Fe3+ octaÃdrico estrutural e uma fase amorfa. No processo de calcinaÃÃo houve o surgimento da hematita nos materiais devido aos ferros nÃo ligados à estrutura juntamente com os da fase amorfa. AlÃm disso observa-se o surgimento de um segundo dubleto paramagnÃtico consistente com Fe3+ estrutural em octaedros severamente deformados caracterÃsticos da metacaulinita. A caulinita branca dopada com ferro apresentaram somente um dubleto com desdobramento quadrupolar ligeiramente acima daqueles obtidos nos caulins vermelhos antes da queima. A queima resultou na transformaÃÃo de uma fraÃÃo da caulinita em metacaulinita com a consequente distorÃÃo dos sÃtios octaÃdricos alÃm do aparecimento de hematita em razÃo do ferro nÃo incorporado à estrutura da argila. Nos espectros das amostras moÃdas em jarras de aÃo inoxidÃvel observou-se uma reduÃÃo do desdobramento quadrupolar sugerindo uma acomodaÃÃo dos Ãons de Fe3+ nos octaedros da caulinita, alÃm do aparecimento de um segundo dubleto com desdobramento quadrupolar maior associado à deformaÃÃo dos octaedros de ferro causada pela moagem. O espectro da amostra moÃda em jarra de aÃo carbono apresentou contaminaÃÃo por ferro metÃlico, o que nÃo houve na moagem em aÃo inoxidÃvel. AlÃm da contaminaÃÃo, a moagem tambÃm induziu à formaÃÃo de uma fraÃÃo de Fe2+ octaÃdrico. A calcinaÃÃo desta amostra transformou o ferro metÃlico em hematita e oxidou o Fe2+ de volta para Fe3+. CalcinaÃÃo de todas as amostras moÃdas induziu o aparecimento de hematita e o aumento do desdobramento quadrupolar dos dubletos como resultado da distorÃÃo da caulinita. Esses resultados mostraram que à possÃvel dopar caulinita com ferro e obter metacaulinita com ferro estrutural atravÃs de moagem mecÃnica e calcinaÃÃo. Com suas vantagens e desvantagens as duas argilas sÃo apropriadas para utilizaÃÃo como matÃrias primas de geopolÃmeros.
In this work, geopolymeric precursor materials were studied by MÃssbauer spectroscopy. To motivate the work, results of MÃssbauer spectroscopy on lateritic soil and concretion and geopolymers produced from them are presented. To study the structure of iron in kaolinites and metakaolinites, geopolymeric most important precursor materials, natural red kaolins with naturally occurring structural iron and white kaolinite doped through iron incorporation reactions in alkaline environments. The MÃssbauer spectra of samples of red kaolin showed a doublet of paramagnetic octahedral Fe$^{3+}$ and an amorphous phase. In the calcination process the emergence of hematite due to burning of non-structural iron along with the amorphous phase is observed. In addition, it is also observed the appearance of a second doublet consistent with paramagnetic octahedral Fe$^{3+}$ characteristic of severely deformed metakaolinite. White kaolinite doped with iron showed only a doublet with quadrupole splitting slightly above those obtained in the red kaolin before burning. Burning resulted in the transformation of a fraction of kaolinite in metakaolinite with consequent distortion of the octahedral sites. It is also observed the appearance of hematite due to the existence of iron not incorporated into the clay structure. The spectra of samples milled in stainless steel jars showed a reduction in quadrupole splitting suggesting an accommodation of ions Fe$^{3+}$ octahedra in the kaolinite structure, and the appearance of a second doublet with quadrupole splitting associated with a milling induced larger deformation of the octahedral iron. The spectrum of the sample ground in carbon steel jar showed contamination by metallic iron, which was not seen in the sample ground in the stainless steel jar. In addition to contamination, milling also induced the formation of a fraction of octahedral Fe$^{2+}$. Calcination of this sample transformed metallic iron into hematite and oxidized the Fe$^{2+}$ back to Fe$^{3+} $. Calcination of all ground samples induced the appearance of hematite and the increase of the quadrupole splitting of doublets as a result of kaolinite distortions. These results showed that it is possible to dope kaolinite with iron and to obtain metakaolinite with structural iron through mechanical milling and calcination. With its advantages and disadvantages, both clays are suitable for use as geopolymers precursor materials.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
No presente trabalho foram preparados pós cerâmicos de Bi4Ti3O12 estequiométrico, com excesso de bismuto e com excesso dopados com nióbio pelo método dos precursores poliméricos. As fases cristalinas foram obtidas por calcinação a 700 °C-4h com 10% excesso Bi nas composições Bi4Ti3-xNbxO12 (x = 0; 0,1; 0,2 e 0,4 mol% Nb). Os pós obtidos foram caracterizados quanto ao tamanho das partículas, difratometria de raios X, espectroscopias Raman, no infravermelho e UV-vis indicando pós nanométricos com fase ortorrômbica predominante, ordenados a curta e longa distância e com alta cristalinidade. As cerâmicas foram compactadas e sinterizadas em forno convencional e microondas a 800 °C, além de caracterizadas por medidas de condutividade elétrica, constante e perda dielétricas, histerese e microscopia eletrônica de varredura. A condutividade elétrica sofreu decréscimo nas cerâmicas dopadas com nióbio, apresentando constante dielétrica de 170 na temperatura ambiente, baixos valores de polarização remanescente e densidade relativa máxima de 93% para cerâmicas sinterizadas em microondas. Cerâmicas funcionais texturizadas foram obtidas empregando-se a técnica de tape casting (colagem de folhas), onde partículas templates do BIT sintetizadas via método dos sais fundidos e com alta orientação na direção do eixo c foram adicionados as barbotinas aquosas do titanato de bismuto. As medidas de caracterização indicaram grau de texturização das cerâmicas de até 80% na direção do eixo c, com aumento da densidade relativa (97%) , da polarização remanescente (3,4 µC/cm2 ) além de menor condutividade elétrica, boa resposta dielétrica e microestrutura com grãos orientados, em comparação às cerâmicas policristalinas
In the present study were prepared stoichiometric Bi4Ti3O12 ceramic powders, with excess bismuth and niobium doped from polymeric precursor method. The crystalline phases were obtained by calcination at 700 °C for 4h with 10% excess Bi in the compositions Bi4Ti3- xNbxO12 (x = 0, 0.1, 0.2 and 0.4 mol% Nb). The powders were characterized for particle size, X-ray diffraction, Raman, IR and UV-vis spectroscopy indicating a predominant nanosized orthorhombic phase ordered at short and long distances, with high crystallinity. The ceramics were compacted and sintered in a conventional and microwave oven at 800 °C, and characterized by measurements of electrical conductivity, dielectric constant and loss, hysteresis, and scanning electron microscopy. The electrical conductivity decreased in the niobium-doped ceramics, with dielectric constant of 170 at room temperature, low remanent polarization and relative density of up to 93% for ceramics sintered in the microwave oven. Functional textured ceramics were obtained using the tape casting methodology where particles of the BIT templates synthesized from the molten salts method presented high orientation in the c-axis direction were added to the aqueous slurry of bismuth titanate. Characterization measures indicated texturing degree of ceramics up to 80% along the c- axis, with increasing in relative density (97%), in the remanent polarization (3.4 µC/cm2) and lower electrical conductivity, good dielectric response and microstructure with grain oriented compared to polycrystalline ceramics

Doutoramento em Física
The present PhD work aims the research and development of materials that exhibit multiferroic properties, in particular having a significant interaction between ferromagnetism and ferroelectricity; either directly within an intrinsic single phase or by combining extrinsic materials, achieving the coupling of properties through mechanic phenomena of the respective magnetostriction and piezoelectricity. These hybrid properties will allow the cross modification of magnetic and electric polarization states by the application of cross external magnetic and/or electric fields, giving way to a vast area for scientific investigation and potential technological applications in a new generation of electronic devices, such as computer memories, signal processing, transducers, sensors, etc. Initial experimental work consisted in chemical synthesis of nano powders oxides by urea pyrolysis method: A series of ceramic bulk composites with potential multiferroic properties comprised: of LuMnO3 with La0.7Sr0.3MnO3 and BaTiO3 with La0.7Ba0.3MnO3; and a series based on the intrinsic multiferroic LuMn1-zO3 phase modified with of Manganese vacancies. The acquisition of a new magnetron RF sputtering deposition system, in the Physics Department of Aveiro University, contributed to the proposal of an analogous experimental study in multiferroic thin films and multilayer samples. Besides the operational debut of this equipment several technical upgrades were completed like: the design and construction of the heater electrical contacts; specific shutters and supports for the magnetrons and for the substrate holder and; the addition of mass flow controllers, which allowed the introduction of N2 or O2 active atmosphere in the chamber; and the addition of a second RF generator, enabling co-deposition of different targets. Base study of the deposition conditions and resulting thin films characteristics in different substrates was made from an extensive list of targets. Particular attention was given to thin film deposition of magnetic phases La1-xSrxMnO3, La1-xBaxMnO3 and Ni2+x-yMn1-xGa1+y alloy, from the respective targets: La0.7Sr0.3MnO3, La0.7Ba0.3MnO3; and NiGa with NiMn. Main structural characterization of samples was performed by conventional and high resolution X-Ray Diffraction (XRD); chemical composition was determined by Electron Dispersion Spectroscopy (EDS); magnetization measurements recur to a Vibrating Sample Magnetometer (VSM) prototype; and surface probing (SPM) using Magnetic-Force (MFM) and Piezo-Response (PFM) Microscopy. Results clearly show that the composite bulk samples (LuM+LSM and BTO+LBM) feat the intended quality objectives in terms of phase composition and purity, having spurious contents below 0.5 %. SEM images confirm compact grain packaging and size distribution around the 50 nm scale. Electric conductivity, magnetization intensity and magneto impedance spreading response are coherent with the relative amount of magnetic phase in the sample. The existence of coupling between the functional phases is confirmed by the Magnetoelectric effect measurements of the sample “78%LuM+22%LSM” reaching 300% of electric response for 1 T at 100 kHz; while in the “78%BTO+22%LBM” sample the structural transitions of the magnetic phase at ~350 K result in a inversion of ME coefficient the behavior. A functional Magneto-Resistance measurement system was assembled from the concept stage until the, development and operational status; it enabled to test samples from 77 to 350 K, under an applied magnetic field up to 1 Tesla with 360º horizontal rotation; this system was also designed to measure Hall effect and has the potential to be further upgraded. Under collaboration protocols established with national and international institutions, complementary courses and sample characterization studies were performed using Magneto-Resistance (MR), Magneto-Impedance (MZ) and Magneto-Electric (ME) measurements; Raman and X-ray Photoelectron Spectroscopy (XPS); SQUID and VSM magnetization; Scanning Electron Microscopy (SEM) and Rutherford Back Scattering (RBS); Scan Probe Microscopy (SPM) with Band Excitation Probe Spectroscopy (BEPS); Neutron Powder Diffraction (NPD) and Perturbed Angular Correlations (PAC). Additional collaboration in research projects outside the scope of multiferroic materials provided further experience in sample preparation and characterization techniques, namely VSM and XPS measurements were performed in cubane molecular complex compounds and enable to identify the oxidation state of the integrating cluster of Ru ions; also, XRD and EDS/SEM analysis of the acquired targets and substrates implied the devolution of some items not in conformity with the specifications. Direct cooperation with parallel research projects regarding multiferroic materials, enable the assess to supplementary samples, namely a preliminary series of nanopowder Y1-x-yCaxØyMn1O3 and of Eu0.8Y0.2MnO3, a series of micropowder composites of LuMnO3 with La0.625Sr0.375MnO3 and of BaTiO3 with hexagonal ferrites; mono and polycrystalline samples of Pr1-xCaxMnO3, La1-xSrxMnO3 and La1-xCaxMnO3.
O trabalho de doutoramento presente tem por objectivo a pesquisa e desenvolvimento de materiais que manifestem propriedades multiferróicas, em particular com uma significativa interacção entre os fenómenos de ferromagnetismo e ferroelectricidade; seja de forma intrínseca em determinados materiais singulares, ou extrínseca ao combinar materiais que apresentam respectivamente fenómenos magnetoestritivo e de piezoelectricidade e em que geralmente o acoplamento se processa mecanicamente entre as fases. Esta hibridação de propriedades permite a modificação dos estados de polarização magnética ou eléctrica por aplicação dos campos externos complementares (eléctricos e/ou magnéticos), dando origem a uma vasta área de investigação científica e potenciais aplicações tecnológicas numa nova geração de dispositivos electrónicos como memórias, processadores, transdutores, sensores, etc. O trabalho experimental inicial consistiu na síntese química de óxidos sob a forma de pós nanométricos, pelo método de pirólise da ureia; As séries de compósitos maciços com potenciais propriedades multiferróicas compreendem: LuMnO3 com La0.7Sr0.3MnO3 e BaTiO3 com La0.7Ba0.3MnO3; e uma série baseada na modificação com lacunas de Manganésio da fase multiferróica intrínseca LuMn1-zO3. A aquisição de um novo sistema de deposição por RF sputtering, no Departamento de Física da Universidade de Aveiro, contribuiu para a proposta de estudo análogo de amostras multiferróicas sob a forma de filmes finos e multicamadas. Além da estreia operacional do equipamento foram efectuadas algumas melhorias técnicas e funcionais de que se destacam: o desenho e construção das ligações eléctricas do aquecedor; de portadas, protecções e respectivos suportes para os magnetrões e para o “porta substratos”; a adição de dois controladores de fluxo de gás permitindo a introdução controlada de Árgon e de atmosfera activa de O2 ou N2 durante a deposição; e a adição de uma segunda fonte e controlador RF permitindo a co-deposição simultânea de filmes a partir de dois alvos diferentes. O estudo base sobre as condições de deposição e das características dos filmes finos resultantes em diferentes substratos foi efectuada a partir de uma extensa lista de alvos. Atenção particular foi dada à deposição de filmes finos das fases magnéticas de La1-xSrxMnO3, La1-xBaxMnO3 e da liga Ni2+x-yMn1-xGa1+y a partir dos correspondentes alvos La0.7Sr0.3MnO3; La0.7Ba0.3MnO3 e NiGa com NiMn. A caracterização estrutural das amostras foi efectuada com Difractometria por Raios-X (XRD) convencional e de elevada resolução; determinação da composição química foi essencialmente realizada por Espectroscopia de Dispersão de Electrões (EDS); medidas de magnetização foram executadas com recurso a um protótipo de Magnetometro por Vibração da Amostra (VSM) e as medidas de análise de superfície utilizaram Microscopia de Ponta (SPM) nas vertentes de piezo resposta (PFM) e de força magnética (MFM). Os resultados obtidos nos compósitos maciços (LuM+LSM e BTO+LBM) demonstram claramente que as amostras satisfazem os objectivos propostos em termos de composição pureza das fases, com eventual conteúdo em óxidos espúrios inferior a 0.5%. Imagens obtidas por SEM confirmam a compactação dos grãos e distribuição de tamanhos em torno dos 50 nm. Condutividade eléctrica, intensidade da magnetização e a dispersão da resposta em Magneto-Impedância são coerentes com a proporção relativa da fase magnética em cada amostra. A existência de um acoplamento entre as fases funcionais é evidenciada por medidas de efeito Magneto-Eléctrico na amostra “78%LuM+22%LSM” que apresenta uma resposta eléctrica de ~300% para 1 Tesla a 100 kHz; enquanto que na amostra “78%BTO+22%LBM” se assinala a transição estrutural da fase magnética a ~350 K resulta na inversão do comportamento do coeficiente ME. Um sistema de Medidas de Magneto-Resistência foi totalmente desenvolvido e montado desde a fase conceptual até ao estado operacional; permite testar amostras de 77 a 350 K em função do campo magnético até 1 Tesla, e rotação horizontal de 360º; o sistema foi também desenhado para poder efectuar medidas de efeito de Hall e permitir upgrades. Ao abrigo de protocolos de colaboração estabelecidos com diversas instituições nacionais e internacionais, foram realizados cursos de formação complementar e caracterização de amostras em técnicas como Magneto Resistência (MR), Magneto Impedância (MZ) e efeito Magneto Eléctrico (ME); Espectroscopia Raman e Fotoelectrónica de Raios-X (XPS); Magnetização via sistemas SQUID e VSM; Microscopia de Ponta em Piezo resposta (PFM) e Espectroscopia de excitação em largura de banda (BEPS); Espectroscopia de Rutherford por Retro dispersão (RBS); Difracção de Neutrões em pós (NPD) e Correlações de Perturbação Angular (PAC) Colaboração em projectos de investigação fora do âmbito dos materiais multiferróicos permitiu ampliar e versatilizar experiencia em técnicas de preparação e caracterização de amostras, nomeadamente medidas de VSM e XPS permitiram identificar os estados de oxidação dos clusters de iões de Ruténio que integram complexos moleculares utilizados em catalisadores; A certificação por XRD e SEM/EDS do conjunto dos alvos e amostragem dos substratos adquiridos implicou a devolução de alguns itens com por falta de conformidade com as especificações. Cooperação directa em projectos de investigação paralelos sobre materiais multiferróicos permitiu o acesso a amostras suplementares, nomeadamente a uma série nano pós de Y1-x-yCaxØyMn1O3 e de Eu0.8Y0.2MnO3; a series de compósitos microestruturados de LuMnO3 com La0.625Sr0.375MnO3 e de BaTiO3 com ferrites hexagonais; e a diversas amostras poli- e mono-cristalinas de Pr1-xCaxMnO3, La1-xSrxMnO3 e La1-xCaxMnO3.
FCT - SFRH/BD/25011/2005

Orientador: Maria Helena Robert
Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica
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Resumo: Este trabalho apresenta o projeto e construção de um equipamento para a compofundição de ligas não ferrosas de médio ponto de fusão. O equipamento é constituído de um forno para a fusão e processamento do compo-fundido, com capacidade de aquecimento de até 1073K (800°C) e capacidade de carga de. 800g de AI, de um rotor provido de pás para promoção de agitação da liga durante a solidificação e sistema de refrigeração do lingote produzido. O trabalho descreve os diferentes constituintes do equipamento construído e apresenta resultados de seu comportamento mecânico, elétrico e térmico quando em operação. O trabalho apresenta ainda resultados de produtos reofundidos e compo-fundidos obtidos no equipamento construido. O equipamento mostrou-se eficiente na obtenção de pastas reofundidas da liga Al-3, 4Si-2,8Cu e de compósitos desta liga reforçada com 1,25 e 2,5% em peso de grafite ou negro de fumo na forma de pós. As condições utilizadas foram: velocidade de agitação de 800 a 1000 rpm, temperatura de processamento de 853K (580°C), pré-agitação para homogenização do material de 3 minutos e agitação com adição de reforço de 5 minutos. O reofundido obtido apresentou fase sólida perfeitamente globularizada e os compósitos obtidos apresentaram boa incorporação e dispersão dos reforços adicionados. O equipamento, portanto, mostrou-se adequado à compo-fundição
Abstract: This work presents the development of an equipment for compo-casting of medium melting point non ferrous alloys. The equipment holds a melting and processing fumace, with heating capacity of 1073K(800º C)and mass capacity of 800g Al, stirring device and cooling coil. The work describes the cornponents of such equipment and presents results concerning its performance during operation. The work also presents results concerning its suitability to produce rheocast slurries and composites. Results showed that the equiprnent is efficient in producing Al-3, 4Si-3Cu rheocastig slurries as well as composites with graphite or carbonblack as reinforcement. Conditions used are as follows: stirring speed 800-1000 rprns, stirring temperature 853 K (580º C), total stirring time Smim and amount of reinforcement 1,25 and 2,50%wt. Obtained rheocast slurries showed globularized solid phase and obtained composites showed good incorporation and dispersion of reinforcernent for both carbon-black and graphite. Therefore, the equiprnent is appropriate for compo-casting
Mestrado
Materiais e Processos de Fabricação
Mestre em Engenharia Mecânica

Ferroic materials, as notable members of smart materials, have been widely used in applications that perform sensing, actuation and control. The macroscopic property change of ferroic materials may become remarkably large during ferroic phase transition, leading to the fact that the macroscopic properties can be tuned by carefully applying a suitable external field (electric, magnetic, stress). To obtain an enhancement in physical and/or mechanical properties, different kinds of ferroic composites have been fabricated. The properties of a ferroic composite are determined not only by the properties and relative amounts of the constituent phases, but also by the microstructure of individual phase such as the phase connectivity, phase size, shape and spatial arrangement.

This dissertation mainly focuses on the computational study of microstructure – property – mechanism relations in two representative ferroic composites, i.e., two-phase particulate magnetoelectric (ME) composite and polymer matrix ferroelectric composite. The former is a great example of ferroic composite exhibiting a new property and functionality that neither of the constituent phases possesses individually. The latter well represents the kind of ferroic composites having property combinations that are better than the existing materials.

Phase field modeling was employed as the computing tool, and the required models for ferroic composites were developed based on existing models for monolithic materials. Extensive computational simulations were performed to investigate the microstructure-property relations and the underlying mechanism in ferroic composites. In particulate, it is found that for ME composite 0-3 connectivity (isolated magnetostrictive phase) is necessary to exhibit ME effect, and small but finite electrical conductivity of isolated magnetic phase can beneficially enhance ME effect. It is revealed that longitudinal and transverse ME coefficients of isotropic 0-3 particulate composites can be effectively tailored by controlling magnetic domain structures without resort to anisotropic two-phase microstructures. Simulations also show that the macroscopic properties of the ferroelectric- polymer composites critically depend on the ferroelectric phase connectivity while are not sensitive to the sizes and internal grain structures of the ceramic particles. Texturing is found critical to exploit the paraelectric↔ferroelectric phase transition and nonlinear polarization behavior in paraelectric polycrystal and its polymer matrix composite. Additionally, a Diffuse Interface Field model was developed to simulate packing and motion in liquid phase which is promising for studying the fabrication of particulate-polymer composites.

Nenhuma
A espectroscopia Mössbauer de 57Fe é uma técnica nuclear, não-destrutiva, utilizada na investigação das propriedades estruturais, magnéticas e hiperfinas de diferentes materiais sólidos. Trata-se, portanto, de uma poderosa ferramenta de caracterização de materiais na física, metalurgia, geologia e biologia, particularmente em materiais magnéticos, ligas metálicas e minerais contendo Fe. Na atualidade, a Espectroscopia Mössbauer de Elétrons de Conversão (CEMS) é amplamente utilizada no estudo de filmes finos e ultrafinos, bem como outros materiais nanoestruturados. No caso de nanoestruturas magnéticas, estudos a baixas temperaturas (LT) são particularmente importantes devido à possibilidade de efeitos oriundos do fenômeno do superparamagnetismo. Neste trabalho foi desenvolvido um sistema de medição CEMS a baixas temperaturas (< 20 K) utilizando um Channeltron (multiplicador de e-) e um Criostato ótico (Modelo SVT-400 da Janis Research Co, EUA) tendo como base um detector originalmente desenvolvido no Departamento de Física Aplicada / Espectroscopia Mössbauer da Universidade de Duisburg-Essen, Alemanha. O detector LTCEMS foi construído, testado e aplicado com sucesso num estudo preliminar de caracterização de bicamadas Fe/(EuxPb1-x)Te(111) com uso de camada sonda de 57Fe de apenas 15Å, obtendo resultados a temperaturas de até 8 K na amostra.
The 57Fe Mössbauer spectroscopy is a nuclear, non-destructive technique used for the investigation of structural, magnetic and hyperfine properties of several materials. It is a powerful tool in characterizing materials in physics, metallurgy, geology and biology field areas, especially magnetic materials, alloys and minerals containing Fe. Lately, the Conversion Electron Mössbauer Spectroscopy (CEMS) is widely used in making studies on ultra-thin magnetic films, as well as other nanoestructured materials. In case of magnetic nanostructures, low temperature (LT) studies are especially important due to the possibility of dealing with superparamagnetic effects. In this work it was developed a CEMS measurement system for low temperatures (< 20K) based on a solid-state electron multiplier (Channeltron) and an optical cryostat (Model SVT-400, Janis Research Co, USA), from which the project was originally conceived at the Applied Physics / Mössbauer Spectroscopy Department from University of Duisburg-Essen, Germany. The LT-CEMS system was fully built, tested and successfully applied in a preliminary characterization of Fe/(EuxPb1-x)Te(111) bilayers with use of a 15 Å, 57Fe probe layer, with reasonable results at sample temperatures as low as 8 K.

Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro Tecnológico. Programa de Pós-Graduação em Ciência e Engenharia de Materiais.
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Este trabalho apresenta um estudo sobre o efeito de variações de Si, de teores residuais de Cu e Mn e da prática de pós-inoculação sobre a tenacidade em ensaio Charpy de Ferros Nodulares Ferríticos no estado bruto de fundição. Também são discutidos os efeitos sobre a microestrutura e demais propriedades mecânicas. Adotou-se o método Taguchi (DOE) para o projeto dos experimentos e a técnica ANOVA para interpretação dos resultados. Estudou-se o efeito de variações de Si entre 2,2-2,4% e 2,1-2,7%, Cu entre 0,04-0,08% e 0,05-0,12%, Mn entre 0,13-0,20% e 0,15-0,30% e da adição de 0,1% de pós-inoculante. Si e pós-inoculação apresentaram forte efeito ferritizante e de aumento no número de nódulos. Cu e Mn apresentaram efeito perlitizante. Apesar do efeito fragilizante, o aumento nos teores de Si contribuíram para a elevação da energia absorvida. A pós-inoculação apresentou efeito mais significativo no aumento da energia absorvida em temperaturas de ensaio mais baixas. Aumentos nos teores de Cu e Mn resultaram em redução da energia absorvida. Com os resultados obtidos constatou-se que propriedades de tenacidade otimizadas podem ser alcançadas com baixos teores de elementos residuais, teores de Si em uma faixa de 2,4 a 2,7% de forma a garantir uma estrutura predominantemente ferrítica, além de uma eficiente prática de pós-inoculação que resulte em um elevado número de nódulos.

Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro Tecnológico, Programa de Pós-Graduação em Engenharia Mecânica, Florianópolis, 2017.
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Nos últimos anos ocorreu um aumento significativo nas pesquisas relacionadas ao desenvolvimento de materiais que apresentem baixo coeficiente de atrito, principalmente por permitirem um aumento no tempo de vida dos componentes de máquinas-ferramentas e na redução do consumo de energia. Dentre todos os processos de fabricação, os processos de usinagem desempenham um papel de grande importância para a indústria metal-mecânica, sendo empregados na manufatura de muitos componentes para os mais variados segmentos industriais. No entanto, algumas dificuldades são encontradas na usinagem de materiais autolubrificantes, como por exemplo a alta taxa de deformação durante a usinagem, podendo obstruir os poros que contém o lubrificante sólido. Nesse contexto, o objetivo desta pesquisa é analisar as componentes da força de usinagem, os cavacos e o fator de recalque durante o torneamento externo longitudinal de um aço sinterizado autolubrificante de matriz metálica fabricado por duas rotas distintas de fabricação. Os ensaios foram realizados a seco em um torno CNC utilizando ferramentas de metal-duro da classe P20 com revestimento em Ti(C,N) + Al2O3 + TiN. As componentes da força de usinagem foram monitoradas através de uma plataforma piezelétrica da empresa Kistler Instrumente. Os parâmetros de corte variados foram a velocidade de corte, o avanço e a profundidade de corte. Independentemente dos parâmetros de corte analisados, a rota de fabricação dos aços autolubrificantes sinterizados influenciou significativamente na força de corte e na força de avanço. O aumento da velocidade de corte não apresentou um efeito significativo sobre a força de usinagem, para ambas as rotas de fabricação dos aços sinterizados. Porém, verificou-se que o aumento da profundidade de corte ou do avanço acarreta um aumento nas componentes da força de usinagem, independentemente da rota de fabricação dos materiais. Verificou-se também a influência dos parâmetros de corte sobre o tipo e a forma dos cavacos obtidos durante a usinagem. O tipo de cavaco obtido durante a usinagem manteve-se constante do tipo lamelar, entretanto, a forma variou com a variação dos parâmetros de corte nas formas de arco espiral e espiral. As rotas de fabricação dos aços, outro fator analisado, apresentou, também, influência significativa no fator de recalque do cavaco.
Abstract : In the last few years occurred a significant increase in the research of new materials with low friction coefficient, mainly because they allow an increase in the life cycle of equipment components and a decrease in energy consumption. Amidst all manufacturing process, machining process have a big role for the metal-mechanic industry. Being employed in the manufacturing of a big number of components in various industry fields. Although there some difficulties in the machining of self-lubricating materials, like the high deformation rate during the machining process, which can obstruct lubricating holding pores. In these context, this research objective is machining force components analysis, wear mechanisms, chip analysis and shear rate of external turning of a sintered self-lubricating steel of metal matrix. The tests were made without lubricating fluid in CNC turning machine using hard metal tools class P20 with Ti(C,N) + Al2O3 + TiN coating. The force components were monitored by a piezoelectric platform from Kistler Instrumente Company. The cutting parameters tested were cutting speed, feed and cutting depth. Despite the cutting parameters tested, the manufacturing route of the sintered self-lubricating steels significant influenced in the cutting and feed forces. The increase in cutting speed didn?t significant influence the machining force, for both sintered steels manufacturing routes. Although, could be seen that an increase in cutting depth or feed can increase the machining forces, despite materials manufacturing route. Also the influence of cutting parameters over tool wear mechanisms and type and chip shape were analyzed. The chip type produced was a constant, but the shape changed with the cutting parameters. The manufacturing routes also significant altered the shear rate.

This thesis set out to investigate lead free ferroic materials with perovskite and tungsten bronze type structures, primarily focussing on the relationship between composition, temperature and crystal structure. A combination of diffraction techniques were employed to investigate the crystal structures. Additionally, other techniques including XANES, SEM, TGA, DSC and ferroic peroperty measurements were also employed to further illuminate these compounds. The first system investigated was the defect perovskite Sr0.8Ti0.6-yZryNb0.4O3, 0.0 ≤ y ≤ 0.6. It was found that neutron powder diffraction data were essential for determining the phase boundary composition. Second order compositional and temperature phase transitions were observed. Increasing the zirconium content increased octahedral tilting and led to higher transition temperatures. Local ordering was determined to be highly probable and it was found that the presence of vacancies extended the range of the high symmetry phase. The second system investigated was the BaxSr3-xTi1-yZryNb4O15, 0.0 ≤ x ≤ 3.0, 0.0 ≤ y ≤ 1.0, tungsten bronze type system. Barium rich compositions were found to adopt a tetragonal structure, while strontium rich compositions adopted an orthorhombic structure. Increasing the zirconium content of samples was seen to make the orthorhombic phase persist further. A large focus was placed on determining the structure of Sr3TiNb4O15 as a model for all orthorhombic compounds. A new structural model was proposed for Sr3TiNb4O15 distinct from those previously published. All orthorhombic compositions were observed to undergo first order phase transitions to the tetragonal structure on heating. The barium and strontium atoms were found to order onto two crystallographically distinct A sites. It was found that the tungsten bronze tolerance factor could be used as a predictive tool for the crystal symmetry of these materials. All compounds in this system for which ferroelectric measurements were performed displayed ferroelectric hysteresis behaviour.

Tese (doutorado) - Universidade Federal de Santa Catarina, Centro Tecnológico, Programa de Pós-Graduação em Ciência e Engenharia de Materiais, Florianópolis, 2016.
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Esta tese visou o desenvolvimento de um material autolubrificante volumétrico de matriz ferrosa contendo MoS2 como elemento lubrificante majoritário. Estudos demonstram a dificuldade em se produzir este tipo de compósito, devido a reação do MoS2 com a matriz ferrosa durante a sinterização. Desta forma, a pesquisa desenvolvida nesta tese buscou soluções para evitar ou reduzir esta reação, avaliando a influência de parâmetros da matéria-prima da matriz e da fase lubrificante (tamanho de partícula, adição de outros elementos e teor de lubrificantes), bem como parâmetros de processamento (taxa de aquecimento, temperatura, formação de fase líquida, tempo de patamar e atmosfera de sinterização). Os resultados mostraram que a temperatura influiu de forma preponderante na reação, mas não a taxa de aquecimento e que o uso de um pó de Fe de menor tamanho de partícula acelera-a; o melhor desempenho está associado ao MoS2 de maior tamanho de partícula (d50=32µm) e 9% em volume é o teor limite; a adição de grafite ou h-BN retarda a reação, porém apenas compósitos com MoS2+grafite apresentaram coeficiente de atrito abaixo de 0,2 associado a um baixo desgaste. A adição de elementos de liga modificou a forma como o MoS2 reagiu com a matriz ferrosa e o desempenho tribológico do compósito, sendo que alguns apresentaram resultados similares ao Fe puro (Ni misturado e P pré-misturado), outros possuem caráter deletério (Cr e Mo misturados e Mo pré-ligado) e alguns apresentaram caráter benéfico (C e P misturados e Cr pré-ligado). É viável sinterização de amostras em temperaturas entre 800 e 850 °C, porém as abordagens visando a intensificação da densificação e propriedades mecânicas não foram bem sucedidas. Através da definição e controle da matéria prima inicial (nomeadamente tamanho de partícula da matriz e do MoS2), composição do compósito e parâmetros de processamento (temperatura, tempo e atmosfera de sinterização) foi possível a produção de materiais autolubrificantes de matriz ferrosa contendo MoS2 como elemento lubrificante majoritário que apresentam baixo coeficiente de atrito a seco (0,06-0,08) associado a uma baixa taxa de desgaste (2,0-3,5 x 10-6 mm³.N-1.m-1).

Abstract : This thesis aimed the development of a self-lubricating composite containing MoS2 dispersed in an iron matrix produced by powder metallurgy. Previous studies demonstrate that MoS2 reacts with iron matrices during sintering, making the production of Fe-MoS2 composites rather difficult. Therefore the research developed within this thesis focused on the possible solutions to avoid or reduce this reaction, evaluating the influence of raw material (particle size, amount and type of lubricants) and processing (heating rate, temperature, dwell time, liquid phase formation and atmosphere) parameters. The results have shown that temperature has a major influence on the reaction, but not the heating rate; the use of a small Fe particle size accelerates the reaction; better performance was achieved by using the d50=32µm MoS2 and 9% in volume is the limit amount; the addition of graphite or h-BN slows the reaction, but only MoS2+graphite composites presents friction coefficient below 0,2 associated with low wear rate. The addition of alloying elements modified how MoS2 interacts with the iron matrix and the composite friction coefficient, some of which had a beneficial effect (admixed C and P, and pre-alloyed Cr alloy), while others (admixed Cr and Mo, and pre-alloyed Mo alloy) are harmful. It is possible to produce iron samples by low temperature sintering (800-850 °C), however the approaches to improve densification and mechanical properties were not successful. By means of defining and adequate control of the raw material (namely particle size of matrix and lubricants), composition and processing parameters (sintering temperature, time and atmosphere) it was possible to produce self-lubricating iron based composites containing MoS2, which presented low dry friction coefficient (0,06-0,08) and low wear rate (2,0-3,5 x 10-6 mm³.N-1.m-1).

O mercado de minérios de ferro e aço está extremamente aquecido nesta primeira década do século XXI, e como mostram os especialistas neste assunto deverá permanecer desta forma por no mínimo mais 5 ou 10 anos. Com o aumento substancial de preços das \"commodities\", principalmente os minérios de ferro, nesta década há nas indústrias ou corporações uma alta disponibilidade de recursos para bons projetos. Desta forma, a empresa que tiver condições de tomar decisões estratégicas melhores, mais rápidas e mais fundamentadas garantirá a perpetuidade do negócio neste mundo competitivo. O principal objetivo desta dissertação é o desenvolvimento e aplicação de um método de tomada de decisão, que utilize simulação-otimização durante o processo de planejamento do negócio. Este método será aplicado na cadeia produtiva de minérios de ferro da Samarco Mineração S/A, com o propósito de melhorar a qualidade das informações do processo de escolha da melhor alternativa de investimentos para os próximos 05 anos. Este método demonstrou uma melhora na qualidade do processo decisório de escolha dos investimentos, além disso, observou-se que o desdobramento em fases garantido pelo método proposto, converge diversos fatores, simplificando e otimizando a tomada de decisão gerencial. Ao avaliar e confrontar os conceitos de simulação e otimização, observou-se que existe um grande conjunto de experiências bem explorado de técnicas para resolução de problemas no sentido de aprimorar, em cada uma das áreas de conhecimento (simulação e otimização) separadamente a busca da melhor solução, deixando de se aproveitar o potencial que se pode conseguir com a integração dessas técnicas. Neste sentido procurou-se evidenciar que não era objetivo desta pesquisa analisar qual é a melhor técnica a ser empregada em cada problema que afeta os sistemas logísticos em geral, e sim potencializar a discussão, assim como muitos autores apresentados neste trabalho, que estas técnicas são complementares e que o sucesso da solução do problema ou oportunidade é proporcional a correta aplicação destas técnicas em seus pontos fortes de resolução de problema. E os casos apresentados e o método aqui proposto reforçam que a aplicação destas técnicas em conjunto garantem um melhor resultado do que o emprego destas ferramentas separadamente.
World demand for iron ore and steel industries are extremely high in the very beginning of the 21st century, and the analysts are foreseeing that it will last for a long period. Likewise the commodities in general, the prices of iron ore have been increasing considerably, mainly because of the disarticulation through this industry supply chain. Considering the systemic aspects of this particular market, the decisions to invest in upstream capacities to supply the demand is very complex and risky. The complexity is related with assets intensiveness, competitor\'s movements, time between decision to implant a project and startup, and the demand-price ups and downs cycles. The companies that make the right strategic decisions, at the right time, are the ones that will succeed in this competitive and global market. The objective of this dissertation is to develop a methodology, using simulationoptimization techniques that support strategic investments decisions. In the research part of this dissertation, a sort of concepts and techniques of simulation, heuristics and optimization were explored and it was possible to identify an opportunity to explore the potential integration of techniques. In particular, this dissertation aims to clarify that this techniques may be complementary, and the success if very much related with the correct approach to combine them considering the particularities of the studied problem. The results have shown that the proposed method clarify that the right combination of techniques, in this case, simulation-optimization, is produces better results and individual application of each one of them. The method was applied at Samarco in its business planning process, and it has been useful to support better investments decisions.

Mestrado em Engenharia de Materiais
O presente trabalho relata o trabalho desenvolvido num estágio na empresa Duritcast, a par da vivência das operações rotineiras do processo de fundição em areia ambicionou-se desenvolver soluções para duas das preocupações do setor. A primeira relacionada com o descarte dos revestimentos refratários dos equipamentos de fusão, e a segunda com a preparação das moldações utilizando modelos em poliestireno expandido (EPS). Os fornos de fundição, são revestidos com uma camada de refratário que se consome por corrosão pela escória ou por abrasão/reação aos elementos presentes no processo. Os revestimentos em fim de vida são depositados em aterros após o abatimento dos fornos mas a importância crescente das questões ambientais impõe a procura de possíveis vias de reutilização. O nome comercial do material refratário usado no revestimento dos fornos da Duritcast é “Coral SLX” e é constituído essencialmente por alumina e magnésia (espinela) é um granulado denso e seco e aplica-se por compactação. Neste trabalho pretendeu-se estudar a recuperação da fração não contaminada do refratário na forma de granulados com uma escoabilidade adequada para a conformação de acessórios para fundição de aço. Recorrendo ao EMMA (Elkem Materials Mix Analyzer) um programa de avaliação do empacotamento de partículas através do controlo da distribuição granulométrica, foi possível criar a nova mistura de pós auto-escoante. Manipulando as classes granulométricas para se obter um pó com escoamento ótimo deve-se adicionar 38,3% da classe (2000-106 μm), 29,7% da classe (2000-500 μm), 17,8% da classe (1000-500 μm) e 14,2% da classe (106-63 μm). No segundo caso, a facilidade de modelagem oferecida pelo EPS é contrabalançada pela libertação de gases (CO2) emitidos para a atmosfera durante a combustão do polímero e pelos defeitos provocados pela dificuldade de remoção do EPS não consumido da superfície da peça. O objetivo deste trabalho foi estudar a remoção do EPS através da sua dissolução por um solvente orgânico, amigo do ambiente, R-limoneno. Foi estudado o melhor método de aplicação do solvente, tendo-se concluído que o mais eficaz seria com a pipeta pois a reação dá-se de uma forma mais extensa. A solubilização do EPS foi testada em moldações de tamanhos diferentes, pelo que conclui-se que este processo só é viável quando se pretende obter peças menores que 1 Ton. Durante o estágio foram realizados outros trabalhos, nomeadamente na área da qualidade e acompanhamento do processo produtivo de ferro nodular. A realização destas atividades permitiu o enquadramento no processo produtivo e o ganho de autonomia na prática laboratorial.
This document describes the work carried out during an internship at the Duritcast company. Along with the experience of daily operations of the sand casting process, the main aim was to develop solutions for two industry concerns. The first related to the disposal of refractory linings of fusion equipment, and the second with the preparation of patterns using models of expanded polystyrene (EPS). In the first case, after the furnace lining is dismantled, the spent refractories are landfilled, but the growing importance of environmental issues requires looking for possible ways to reuse them. The reuse potential of the uncontaminated fraction of the refractory was investigated, in the form of loose aggregates with the flowability adequate to manufacture steel casting accessories. Using the EMMA program, it was possible to study the particle size distribution and create a new blend with maximum flowability which should 38,3% of the class (2000-106 μm), 29,7% of the class (2000-500 μm), 17,8% of the class (1000-500 μm) and 14,2% of class (106-63 μm). In the second case, the ease of modeling offered by EPS is offset by the release of gases (CO2) emitted into the atmosphere during combustion of the polymer and the defects caused by the difficulty of removing unconsumed EPS left on the part’s surface. We intended to study the removal of EPS through dissolution by organic, environmentally friendly R-limonene solvent, was studied the solvent’s most effective application method was found to be the utilization of the pipette due to a more extensive reaction of EPS and R-Limone. Solubility of the EPS was tested in molds of different sizes and it was concluded that this process is only possible when applied on parts smaller than 1 ton. During the internship other activities were conducted particularly in the area of quality and monitoring the process of production of ductile iron. These activities promoted a better knowledge of the productive process and increased autonomy in laboratory practice.

Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro Tecnológico. Programa de Pós-graduação em Engenharia de Materiais
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Il mio progetto di ricerca ha avuto come focus il Salento nell’età del Ferro partendo dallo studio contestuale di un sito scoperto recentemente a Vaste, nel sud della provincia di Lecce. Si tratta di un sito inedito rivelatosi particolarmente importante perché è uno dei pochi contesti ritenuti cultuali documentati nel Salento per l’età del Ferro. Si tratta di una vasta area caratterizzata dalle presenza di buche terragne i cui depositi si sono rivelati di natura rituale. È stato uno dei pochi contesti salentini che ha restituito materiale iapigio integro. La cronologia del contesto è prima metà del VII sec. a.C. L’analisi del contesto di Vaste è stata preceduta da una schedatura dei siti dell’età del Ferro editi nel Salento. L’altra parte importante del progetto è stata l’analisi chimica tramite tecnica XRF svolta presso il CEDAD su un campione di ceramica d’importazione databile tra fine VIII e VII sec. a.C. proveniente da alcuni siti salentini (Vaste, Otranto e San Vito dei Normanni) e della Basilicata (Policoro e Torre di Satriano). Il lavoro ha permesso di stabilire i luoghi di produzione delle varie classi ceramiche analizzate.
My research project will focus on the Salento region during the Iron Age; beginning with the study of a site that was recently discovered in Vaste, in the Southern province of Lecce. Little is known or has been published about the site, but as studies of the area continue it was discovered to have been one of the few sites to be officially religious in Salento during the Iron Age. Interestingly, it is a vast area characterised by the presence of ‘earth pits’, which are earthy deposits of a ritualistic nature. It is also one of the few areas in Salento where undamaged ‘Iapygian’ artefacts have been discovered. This period chronologically dates from the 7th century B.C. Further studies for this project have been done using chemical analysis (an XRF technique done in CEDAD laboratories) on pottery samples dating from the 8th to the 7th century B.C. from various sites in Salento, such as, Vaste, Otrano and San Vito dei Normanni and sites in Basilicata, such as, Policoro and Torre di Satriano.

Il mio progetto di ricerca ha avuto come focus il Salento nell’età del Ferro partendo dallo studio contestuale di un sito scoperto recentemente a Vaste, nel sud della provincia di Lecce. Si tratta di un sito inedito rivelatosi particolarmente importante perché è uno dei pochi contesti ritenuti cultuali documentati nel Salento per l’età del Ferro. Si tratta di una vasta area caratterizzata dalle presenza di buche terragne i cui depositi si sono rivelati di natura rituale. È stato uno dei pochi contesti salentini che ha restituito materiale iapigio integro. La cronologia del contesto è prima metà del VII sec. a.C. L’analisi del contesto di Vaste è stata preceduta da una schedatura dei siti dell’età del Ferro editi nel Salento. L’altra parte importante del progetto è stata l’analisi chimica tramite tecnica XRF svolta presso il CEDAD su un campione di ceramica d’importazione databile tra fine VIII e VII sec. a.C. proveniente da alcuni siti salentini (Vaste, Otranto e San Vito dei Normanni) e della Basilicata (Policoro e Torre di Satriano). Il lavoro ha permesso di stabilire i luoghi di produzione delle varie classi ceramiche analizzate.
My research project will focus on the Salento region during the Iron Age; beginning with the study of a site that was recently discovered in Vaste, in the Southern province of Lecce. Little is known or has been published about the site, but as studies of the area continue it was discovered to have been one of the few sites to be officially religious in Salento during the Iron Age. Interestingly, it is a vast area characterised by the presence of ‘earth pits’, which are earthy deposits of a ritualistic nature. It is also one of the few areas in Salento where undamaged ‘Iapygian’ artefacts have been discovered. This period chronologically dates from the 7th century B.C. Further studies for this project have been done using chemical analysis (an XRF technique done in CEDAD laboratories) on pottery samples dating from the 8th to the 7th century B.C. from various sites in Salento, such as, Vaste, Otrano and San Vito dei Normanni and sites in Basilicata, such as, Policoro and Torre di Satriano.

Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro Tecnológico, Programa de Pós-Graduação em Ciência e Engenharia de Materiais, Florianópolis, 2013.
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A metalurgia do pó ferrosa é um processo que oferece inúmeras soluções na indústria, principalmente devido a economia de escala. Este processo tem algumas limitações, como o tamanho e a geometria dos corpos a serem produzidos. No intuito de investigar outras soluções para a metalurgia do pó, principalmente no condicionante a componentes, tem-se o processo de brasagem, que é a união de dois ou mais corpos, de modo a formar um corpo final único. O intuito deste trabalho é realizar a união durante a sinterização, em processo definido como sinterbonding. Para tal, estudou-se ligas de ferro cobre, com percentuais de 0 a 20% de adição de cobre, no intuito de formar fase líquida durante o processo descrito anteriormente e promover a junção de dois sólidos através do posicionamento de topo, em condições de processamento semelhantes as já aplicadas na indústria (pressão de compactação e temperatura). No intuito de caracterizar a união as amostras foram preparadas metalograficamente, para verificar a continuidade da linha da junção e também comparadas mecanicamente através de ensaio uniaxial de tração em relação a uma amostra padrão. Para melhorar os resultados também utilizou- se a técnica de recompactação. Foram obtidos tensões de ruptura 20% inferiores em relação a amostra de referência, porém com significativa redução da capacidade de deformação, de 70 a 90%.

Abstract : Metal powder metallurgy is a process that offers numerous solutions in the industry, mainly due economies of scale. But this process has some limitations, such as the size and geometry of the green bodies to be produced. In order to determinate other solutions for this process, especially concerning into the geometry, it has been applied the brazing process which is the union of two or more bodies, so as to form a single body end. The aim of this work is to provide the union during the sintering process, which is defined as sinterbonding. Iron-copper alloys, with a range from 0-20% of copper where studied, in order to form a liquid phase during the process and promote the joining by top-of-body positioning, under similar conditions of those already applied in industry (pressing pressure and temperature). To characterize the union, samples were prepared metallographically to verify the continuity of the junction and also compared mechanically through tensile-strength test in reference to a standard sample. To improve the results the double pressing technique also was used. It was observed that to the samples with higher content of copper and double-pressed it was obtained better results, but if compared with a standard sample, lower mechanical strenght, a great loss in elongation and low impact resistance were obtained.

O Brasil é um dos grandes produtores mundiais de minério de ferro e exporta a maior parte da sua produção. No comércio internacional é importante assegurar a comparabilidade dos resultados analíticos obtidos em diferentes laboratórios. Uma variação de 0,1 % na média do teor de ferro pode aumentar ou diminuir em muito o valor de um grande carregamento de minério. Assim, os sistemas de garantia da qualidade dos laboratórios necessitam de materiais de referência. Este trabalho estudou a preparação de um lote de minério de ferro (pelotizado) como material de referência, certificando os teores de vários constituintes por meio de um programa interlaboratorial. Treze laboratórios participaram do programa e dezoito componentes do minério tiveram seus teores certificados: Fetotal (65,1%), SiO2 (2,76%), Al2O3 (0,46%), TiO2 (0,056%), P (0,026%), S (0,003%), MnO (0,094%), CaO (3,31%), MgO (0,043%), K2O (0,013%), Ba (0,004%), Zn (13 mg/kg), Cu (10 mg/kg), Co (12 mg/kg), Cr (56 mg/kg), Pb (15 mg/kg), Ni (14 mg/kg), V (48 mg/kg).
Brazil is one of the great worldwide iron ore producers and exports most of its production. In the international trade it is important to make sure the comparison of the analytical results among different laboratories. A variation of 0,1% in the average of the iron content can increase or decrease the value of a large ore shipment. Thus, the quality guarantee systems of the laboratories need certified reference materials. The aim of this work was the preparation an amount of iron ore (pellets) as reference material, being certified content of some constituents through an interlaboratory program. Thirteen laboratories participated of the program and eighteen components of the ore had its content certified: Fetotal (65,1%), SiO2 (2,76%), Al2O3 (0,46%), TiO2 (0,056%), P (0,026%), S (0,003%), MnO (0,094%), CaO (3,31%), MgO (0,043%), K2O (0,013%), Ba (0,004%), Zn (13 mg/kg), Cu (10 mg/kg), Co (12 mg/kg), Cr (56 mg/kg), Pb (15 mg/kg), Ni (14 mg/kg), V (48 mg/kg).

O presente trabalho apresenta um estudo do efeito do hidrogênio, a influência da temperatura e do tempo no processo de pós-oxidação por plasma pulsado na liga ferrosa AISI 1045 previamente nitretada a plasma. O estudo das fases cristalinas presentes no sistema foi realizado pela técnica de difração de raios X (DRX). O método de refinamento por Rietveld foi utilizado para quantificar o conteúdo de fases presentes. A estrutura eletrônica da superfície oxidada foi estudada por espectroscopia de fotoelétron induzidos por raios X (XPS). A morfologia e espessura da camada do óxido foram avaliadas por microscopia eletrônica de varredura (MEV) e microscopia de força atômica (AFM). As propriedades mecânicas foram estudadas mediante ensaios de nanoindentação. Ensaios de névoa salina foram executados com o intuito de estudar a resistência à corrosão acelerada do sistema tratado. O hidrogênio controla a formação das fases oxidadas (hematita (α-Fe2O3) e magnetita (Fe3O4)). Uma concentração de 25% de H2 na mistura gasosa oxidante proporciona uma camada de óxido livre de hematita. Por um lado, a espessura do óxido segue um comportamento exponencial tipo Arrhenius em função da temperatura de tratamento típico de um processo termicamente induzido, com uma energia de ativação de 68±5 kJ/mol. Por outro lado, a espessura de óxido segue um comportamento tipo-parabólico com o tempo de tratamento típico de um processo de reação-difusão. Baixas temperaturas e curtos tempos de processo proporcionam camadas de óxidos mais homogêneas, compactas e com maior dureza. Os ensaios de corrosão mostraram que superfícies sem estruturas globulares, mais compactas e com poros fechados possuem uma maior resistência à corrosão, porém ainda não atende a especificação mínima para possível substituição do cromo duro em ligas ferrosas.
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This work shows the hydrogen effect and the influence of processing temperature and time in the post-oxidation treatment by pulsed plasma on nitrided AISI 1045 ferrous alloy. The crystalline structure was analyzed by X-ray diffraction (XRD). The Rietveld refinement method was used in order to quantify the present phases in the system. The electronic structure of the oxide layer was studied by X-ray photoemission electron spectroscopy (XPS). The morphology and oxide layer thickness were analyzed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The mechanical properties were studied by nanoindentation tests. In an effort to know the corrosion resistance of our systems, salt spray tests were executed. Hydrogen controls the formation of oxide phases (hematite (α-Fe2O3) and magnetite (Fe3O4)). A 25 % H2 concentration in the oxidation gas mixture leads to obtain a hematite-free oxide layer. On one hand, the oxide layer thickness follows an exponential Arrhenius-like behavior with processing temperature which is characteristic of a thermally induced-process with activation energy of 68±5kJ/mol. On the other hand, the oxide layer thickness follows a parabolic-like behavior with processing time which is characteristic of the reaction-diffusion process. Lower temperatures and shorter times of processing render more homogenous and compacts oxide layers with higher hardness. Although, corrosion tests show that surfaces without globular structures, more compacts and with closed-pores have higher corrosion resistances, our system does not attend the minimal specification in order to substitute hard chromium in ferrous alloys.

Filmes de benzotriazol (BTAH) formados sobre aços carbono e inoxidável 316L foram estudados em meios de ácido sulfúrico, ácido clorídrico e cloreto de sódio a 25°C. Os seguintes aspectos foram considerados: as condições de formação do filme, sua eficiência, sua resistência em meios não contendo o inibidor,a presença de aditivos e o efeito do transporte de massa sobre o mecanismo da reação. Foram empregadas como técnicas: transitórios de potencial de circuito aberto, ensaios gravimétricos, curvas de polarização potenciostáticas e potenciodinâmicas com eletrodo parado e de disco rotativo, cronoamperometria, espectroscopia de impedância eletroquímica, microscopia ótica, microscopia eletrônica de varredura e análise da superfície por dispersão de energia. O BTAH se mostrou inibidor na grande maioria dos meios para os dois materiais estudados. A resistência dos filmes formados não existe ou é parcial quando as superfícies metálicas revestidas com o filme são imersas nos meios estudados sem inibidor. A adição de Cu(II) aumenta a resistência dos filmes, para determinadas relações [BTAH]/[Cu(II)] que estabilizem o intermediário Cu(I). A presença de íons provenientes da dissolução do aço inoxidável 304 em H2SO4 0,50 mol.L-1 contendo BTAH, eleva significativamente a resistência dos filmes formados, quando estes são expostos aos meios sem inibidor. O cloreto de trimetildodecil amônio exerce sinergismo sobre a ação do BTAH como inibidor de corrosão do aço carbono 1010 em meios ácidos. Superfícies de aço carbono previamente reduzidas são mais eficientes na formação de filmes resistentes aos meios sem inibidor. O transporte de massa do BTAH é uma etapa cinética importante no mecanismo de formação do filme sobre aço inoxidável 316L em meio de HCI 2,0 mol.L-1. O BTAH se mostrou inibidor para a corrosão do aço quando revestido pelo \"primer\" da tinta epóxi, quando adicionado à tinta ou quando o filme é formado antes da aplicação do \"primer\".
Benzotriazole (BTAH) films formed on carbon steel and 316L stainless steel have been studied in sulfuric and chloridric acids and in sodium choride solutionsat 25°C. Different aspects were considered: the film formation conditions, its efficiency, its resistance, the presence of additives and the effect of mass transport on the reaction mechanism. Open circuit potential measurements, weight loss experiments, potenciostatic and potentiadynamic polarization curves using stationary and rotating disc electrode, chronoamperometry, electrochemical impedance spectroscopy, optical and scanning electron microscopies and energy dispersive surface analysis have been used as techniques. BTAH have shown inhibitive effect over the majority of the systems studied. The film resistance depends on the presence of the inhibitor in the solution but the result is different if the film is formed in solution containing additives as copper (II) ions or cations obtained from 304 SS dissolution in H2SO4 media; in this case the films resist to chloridric acid media without BTAH. Dodecyltrimetilammonium chloride presents synergism on the inhibitive BTAH action forcarbon steel in acid solution. The BTAH mass transport represents an important step on the film formation mechanism. BTAH is also an effective inhibitor for carbon steel covered by epoxy primer when it is added to the primer or when the film is formed on the carbon steel surface from a H2SO4 solution containing BTAH.

Existem diversos componentes produzidos por metalurgia do pó que necessitam utilizar uma matéria prima nobre devido a aplicações que causam desgaste em áreas específicas. Desta forma faz-se necessário o desenvolvimento de um material tornando o projeto mais atraente economicamente. O objetivo deste trabalho é analisar e discutir o efeito da densidade nas propriedades mecânicas e microestruturais de materiais com gradiente de função, compostos por metade de ferro comercialmente puro e a outra metade de um material mais nobre, que contém elementos de liga específicos para tratamento de sinterhardening. Corpos de prova foram compactados variando-se a densidade, posteriormente sinterizados e revenidos. Ensaios mecânicos e análise microestrutural foram realizados. Foi possível verificar, de acordo com os resultados, que o aumento da densidade promove o aumento das propriedades mecânicas. Além disso, um pequeno incremento na densidade do componente proporciona a formação do dobro de martensita. Desta forma, é possível fabricar componentes com esta composição levando-se em consideração a distância referente a zona de transição para que as propriedades necessárias estejam presentes nas regiões críticas.
There are several components produced by powder metallurgy that need to use a noble raw material due to applications that cause wear in specific areas. In this way it is necessary to develop a material made the project more economically attractive. The objective of this work is to analyze and discuss the effect of density on the mechanical and microstructural properties of functionally gradient materials composed of half of commercially pure iron and the other half of a more noble material containing specific alloying elements for the treatment of sinterhardening. Test specimens were compacted by varying the density, sintered and tempered. Mechanical tests, metallographic analysis and hardness were performed. It was possible to verify, according to the results, that the increase of the density promotes the increase of the mechanical properties. In addition, a small increase in component density gives the formation of twice martensite.In this way, it is possible to fabricate components with this composition taking into account the distance of the transition zone so that the necessary properties are present in the critical regions.

Multiferroics are currently intensely investigated because the coexistence and coupling of ferroic arrangements brings about new physical effects and, for the few room-temperature examples, interesting prospects for applications in various fields. This interest is illustrated by the recent publication of several articles on multiferroics in high impact reviews over the last five years. The main goal of the thesis was to look for new multiferroics by exploiting overlooked and original polar and magnetic arrangements. We more precisely investigated compounds based on lead iron tungsten PbFe2/3W1/3O3 (PFW) and lead zirconate PbZrO3 (PZO) oxides. PFW displays long- and short-range both polar and magnetic orders (ferroelectric-relaxor and antiferromagnetic-spin-glass) while PZO is antiferroelectric with antiferrodistorsivity (oxygen tilts) and existence of ferroelectric instabilities. Combining various techniques from synthesis to electric, magnetic and structural characterizations, we demonstrated that it is possible to get a multiferroic compound (50%PFW-50%PZO) with coexistence of multiple ferroic and structural arrangements with room temperature properties of practical interest. This work opens new prospects in this rich field of multiferroics in peculiar by using antiferroelectrics.

Low-dimensional materials with novel electronic and ferroic properties play a crucial role in the development of next-generation nanoscale functional devices and have drawn extensive research attentions. By using state-of-art first-principles calculations, Monte Carlo simulations, and structural revolution algorithms, four new low-dimensional materials were predicted showing promising applications in electronics or spintronics and two strategies were proposed to introduce ferroelectricity and realize strong electromagnetic coupling in experimentally fabricated low-dimensional materials, which may accelerate the discovery and design of novel functional low-dimensional materials.