No description available.

No description available.

Revealing the prior austenite grain boundaries from a martensitic structure is well known to be very difficult and dependent on the chemical composition and the thermomechanical processing of the steel. In the present study, four different chemical etching reagents and additional thermal etching have been conducted for thermomechanical simulated tool steels Orvar Supreme and Stavax ESR. The etching results have been characterized using light optical microscopy and electron backscattered diffraction. The obtained results show that saturated aqueous picric acid, oxalic and sodium bisulfite based acid reveals prior austenite grain boundaries well for Orvar Supreme. For Stavax ESR, only aqueous CrO3-NaOH-picric acid provides good results in revealing the prior austenite grain boundaries. Thermal etching shows good potential and if conducted properly, thermal etching is a good alternative to the chemical reagents from a health- and environmental perspective.

This study focuses on the laser powder bed fusion processing of NiTi alloys and the feasibility of fabricating very thin stent structures for biomedical applications. A comprehensive correlation between the process and the material’s-structure and properties is established to facilitate the fabrication of NiTi alloys with tailored properties. In the first step, the impact of LPBF processing parameters and post-treatments on evolving the microstructure, texture, superelasticity, and asymmetry is examined. Subsequently, the feasibility of manufacturing very thin mesh structured stents is scrutinized followed by in-depth investigations into differently designed stents considering properties such as surface characteristics, mechanical properties, superelasticity, and recoverability. The obtained results and the represented discussions offer imperative insights, helping to better understand the complexity of the LPBF process and the present challenging aspects. Moreover, detailed contributions are made with the goal of paving the road ahead for the production of patient-specific NiTi stents with enhanced properties. / Thesis / Doctor of Philosophy (PhD)

Conventional thermobarometry in metamorphic systems has been primarily limited to constraining peak temperature (or pressure) along a generalized P-T loop. This is largely attributed to the assumption that mineral assemblages and chemistries achieve a state closest to equilibrium with the maximum thermal (and therefore energetic) input at these peak conditions. However, this traditional approach is limited in providing much information about the evolution of a metamorphic terrane, which is modified by tectonic (kinematic) forces, fluid and component mobility, and heating duration. The ubiquity of quartz in the continental crust has driven much interest in using the phase for thermobarometric purposes. In this dissertation, I discss the application of elastic theory in reconstructing conditions of inclusion encapsulation through inclusion pressure estimation with Raman spectroscopy. In some instances, overpressuring of quartz inclusions in garnet give evidence for high-pressure formation conditions. When analyses are collected from garnet core to rim, pressure paths along garnet growth can be inferred (if temperature can be reasonably estimated). In high-T, low-P terranes, quartz may become dilated if the inclusion adheres to the host. If a quartz inclusion is sufficiently stretched, transformation to a low-density polymorph may occur. Trace element uptake, particularly Ti, have been characterized in quartz and understood to be the result of a temperature- (and to a lesser extent, pressure-) sensitive substitution for Si4+. However, the application of the Ti-in-quartz thermobarometer in quartz mylonites has led to mixed results due to the low-Ti resetting that occurs with dynamic recrystallization. We applied defect energy simulations and took a global assessment of deformed quartz trace element chemistries to infer that sweeping grain boundaries provide short pathways that allows localized re-equilibration with a Ti-undersaturated medium, resulting in Ti removal from the quartz lattice. In addition, thermodynamic pseudosection modeling has provided a method to assess Ti activity as a dynamic parameter – one that evolves as the phase stability changes through prograde and retrograde metamorphic reactions. With this understanding, better growth-composition models can be derived to infer complex pressure-temperature-time-deformation (P-T-t-D) histories of metamorphic rocks. These techniques and results are coupled with conventional thermobarometry techniques to provide a more comprehensive picture of the conditions experienced by a rock through the evolution, from burial to exhumation to the Earth's surface. The thermal evolution is used to provide conceptual thermal-kinematic models to explain tectonic evolution and heat advection in the continental lithosphere in ancient mountain belts. / Ph. D.

No description available.

Les aciers multiphasés à très haute résistance mécanique destinés à l’industrie automobile font l’objet d’importantes activités de recherche et développement dans le contexte de l’allègement des structures. L’obtention de meilleurs compromis entre résistance et ductilité nécessite de comprendre l’influence du couple composition chimique nominale – paramètres du procédé d’élaboration sur la formation des microstructures.La présente étude s’inscrit dans cette démarche de compréhension et porte en particulier sur les mécanismes se produisant lors du recuit des nuances d’aciers Dual Phase de haut grade microalliés au Ti et au Nb, dont la microstructure initiale laminée à froid est composée de bainite et de martensite. Ces mécanismes (précipitation des éléments de microalliage Ti, Nb et Mo, recristallisation de la ferrite et formation de l’austénite) présentent des interactions complexes. Le scénario des évolutions microstructurales lors du recuit est caractérisé à l’aide d’une étude expérimentale s’appuyant sur des techniques d’analyses complémentaires à différentes échelles (DRX in situ, MEB, MET, SAT). L’influence respective des éléments de microalliage Ti, Nb et Mo et des paramètres du recuit sur ce scénario est clarifiée à l’aide d’une caractérisation systématique des évolutions microstructurales couplée à la mise en œuvre d’une démarche de modélisation des mécanismes et de leurs interactions. / To meet the need for weight reductions in the automotive industry, new advanced high-strength steels are being developed. The achievement of a better balance between high strength and high formability requires a deep understanding of both the effect of chemical composition and processing parameters on the formation of microstructures. The present work contributes to such an objective and deals with the mechanisms occurring during annealing of Dual Phase steels microalloyed with Ti and Nb. Microstructural changes during this stage include precipitation of microalloying elements, ferrite recrystallization and austenite formation. These mechanisms are investigated using complementary experimental techniques at different scales such as in situ XRD, SEM, TEM and APT in various Dual Phase steel grades having the same bainite-martensite initial cold-rolled microstructure. Using combined experimental and modeling approaches, the present work clarifies the separate influence of microalloying elements Ti, Nb and Mo and heating rate on the mechanisms occurring during annealing and their interactions.

No presente trabalho estudou-se a recristalização do aço de alta resistência baixa liga (ARBL) microligado ao nióbio (160 ppm em peso) da Companhia Siderúrgica Nacional 2336 utilizado na fabricação de reforços estruturais para a indústria automobilística. A grande utilização deste tipo de aço pelas indústrias tem motivado o desenvolvimento de novas ligas capazes de atender a requisitos críticos de estampagem combinado com alta resistência mecânica. Amostras deste aço no estado laminado a quente foram deformadas posteriormente a frio em escala piloto com reduções de 50 e 70%, reduções típicas na indústria, e recozidas em banho de sal em temperaturas variando entre 600 e 700ºC em diferentes tempos. A evolução microestrutural das amostras no estado encruado e na condição recozida foi acompanhada utilizando-se as técnicas de microscopia ótica e eletrônica de varredura. As texturas de deformação e de recristalização foram determinadas via difração de raios X. A fração volumétrica recristalizada (Xv) e o tamanho de grão foram determinados com o auxílio de metalografia quantitativa nas amostras recozidas. Medidas de microdureza Vickers foram utilizadas para construir as curvas de encruamento e da cinética de amolecimento em função da temperatura de recozimento e comparadas com curvas construídas pelo primeiro método. Os resultados mostram que a recristalização ocorre em temperaturas acima de 650°C. Com auxílio de um gráfico de Xv contra A (fração amolecida), podemos observar a ocorrência de um desvio da idealidade a 650°C e 700°C. A explicação mais provável é a ocorrência de precipitação, especialmente para o aço menos deformado. Os valores do expoente de Avrami obtidos a partir das duas abordagens (medidas de microdureza e metalografia quantitativa) são apresentados e discutidos. / The recrystallization of a high strength low alloy steel (HSLA) containing niobium (160 wt-ppm) was investigated. The HSLA steel, named CSN 2336, is used in the manufacture of structural parts for automotive industry. The increasing use of this application type of steels in automotive industries has motivated the development of new alloys able to gather the critical requirements for deep drawing combined with high strengths. Samples of this steel in hot-rolled condition were cold-rolled with reductions of 50% and 70%, commonly used in most of applications, and isothermally annealed in salt bath at temperatures between 600 and 700ºC. The microstructure of the samples in both coldworked and annealed states was imaged using light optical (LOM) and scanning electronic microscopies (SEM). Deformation and recrystallization textures were determined by X-ray diffraction. The recrystallized volume fraction (Xv) and the mean grain size were determined by quantitative metallography in the annealed samples. Vickers microhardness testing was used to determine the work hardening and the softening kinetics behaviors. The results show that recrystallization occurs at temperatures above 650°C for the most deformed steel. By plotting Xv against A (softening fraction), we observe the occurrence of a deviation from ideality at 650°C and 700°C, likely caused by solid-state precipitation, especially for the less deformed steel. The values of n (Avrami exponent) obtained from both approaches (softening curves and quantitative metallography) are presented and discussed.

Materiais magnetostrictivos, como o TERFENOL-D (Tb0,27-0,30Dy0,73-0,70Fe2) e o GALFENOL (Fe72-82Ga18-28), são aplicados em diversos tipos de atuadores, sensores e coletores de energia. Contudo, existe a necessidade de novos materiais que sejam mais baratos, ambientalmente amigáveis e com melhores propriedades mecânicas. Por essa razão, as ligas de Fe-Al são uma alternativa, já que o alumínio é mais abundante na natureza e é sete vezes mais barato que o gálio. O objetivo desse trabalho foi estudar a influência de dois tratamentos termomecânicos nas propriedades magnéticas das ligas (Fe1-xAlx)98,4B1,6, onde x = 0,18; 0,13 e 0,21. No primeiro processamento, as ligas foram submetidas a um tratamento térmico sob compressão para introduzir uma anisotropia magnetocristalina extrínseca. Para compressões de até 180 MPa, as ligas tratadas sob tensão obtiveram valores de magnetostricção e dos coeficientes piezomagnéticos maiores que o das ligas sem tratamento. Ou seja, este processamento aumentou a sensibilidade das ligas como atuador (d33) e sensor (d33 *). No segundo processamento termomecânico, amostras com formato de chapa foram laminadas e tratadas termicamente para induzir um crescimento anormal de grãos e consequentemente uma textura. Embora não tenha ocorrido crescimento de grão anormal durante o tratamento térmico, os valores de magnetostricção foram maiores que o das amostras como fundidas. Ambos processamentos termomecânicos foram efetivos para melhorar as propriedades magnéticas e a liga (Fe0,87Al0,13)98,4B1,6 foi a que obteve os maiores valores de magnetostricção e dos coeficientes piezomagnéticos. Em outras palavras, dentre as ligas estudadas, esta composição foi mais promissora para ser aplicada em atuadores e sensores. / Magnetostrictive materials, like TERFENOL-D (Tb0.27-0.30Dy0.73-0.70Fe2) and GALFENOL (Fe72-82Ga18-28), are applied in several types of sensors, actuators and energy harvesting. Nevertheless, there is the necessity of new materials that are cheaper, environmentally friendly and with good mechanical properties. For that reason, the Fe-Al alloys are an alternative, since the aluminum is more abundant in nature and is seven times cheaper than gallium. The goal of this work is to study the influence of two thermomechanical proceeding at magnetic properties of the (Fe1- xAlx)98.4B1.6 alloys, which x = 0.18; 0.13 e 0.21. At the first proceeding, the alloys were submitted to a stress annealing to introduce an extrinsic magnetocrystalline anisotropy. Up to 180 MPa of compression stress, stress annealed alloys have magnetostriction and piezomagnetic coefficient values higher than the alloys without annealing. In other words, this proceeding increased the alloys sensibility to be applied like actuators (d33) and sensors (d33 *). At the second thermomechanical proceeding, samples with sheet format were rolled and annealed to induce an abnormal grain growth and, consequently, a texture. Although the annealing not produced an abnormal grain growth, the magnetostriction values are higher than for the as-cast samples. Both proceedings were efficient to improve the magnetic properties and the (Fe0.87Al0.13)98.4B1.6 alloy achieved the higher values of magnetostriction and piezomagnetic coefficient. In another words, between the studied alloys, this composition was the most promising to be applied like actuators and sensors.

No presente trabalho foram estudados os fenômenos de encruamento e, principalmente, a formação e reversão da martensita alfa-linha (a\', cúbica de corpo centrado, CCC, ferromagnética) induzida por deformação em um aço inoxidável dúplex UNS S31803 e um super dúplex UNS S32520. Inicialmente, as microestruturas dos dois materiais na condição solubilizada foram caracterizadas com auxílio de várias técnicas complementares de análise microestrutural. Foram determinadas fração volumétrica, estrutura cristalina, composição química, tamanho e morfologia das duas fases (ferrita e austenita). Posteriormente, os dois aços foram deformados por dois métodos: a laminação a frio, dividida em vários estágios, com menores graus de deformação e a limagem, sendo que o cavaco limado resultante apresenta altos graus de deformação. Algumas amostras deformadas foram recozidas. Os fenômenos de encruamento, formação e reversão de martensita induzida por deformação na austenita, recuperação, recristalização da austenita e da ferrita no cavaco limado foram estudados predominantemente por difratometria de raios X e usando o método de Rietveld. A difratometria de raios X também foi utilizada para determinação das microdeformações residuais e tamanhos de cristalito (subgrão), calculadas a partir do alargamento dos picos de difração causado pelas deformações. Desta forma, puderam-se comparar os níveis de deformação da laminação e limagem. Qualitativamente, a formação e reversão da martensita induzida por deformação também foi estudada por meio de medidas magnéticas utilizando-se dados de saturação magnética das curvas de histerese obtidas com o auxílio de um magnetômetro de amostra vibrante. Observou-se que para o aço inoxidável dúplex, tanto a laminação quanto a limagem causaram a formação de martensita induzida por deformação e para o aço inoxidável super dúplex, apenas a limagem promoveu essa transformação. Em comparação com o aço dúplex, o aço super dúplex apresentou maior resistência à formação de martensita induzida por deformação, pois apresenta uma austenita mais rica em nitrogênio e uma maior propensão à formação de fase sigma durante o recozimento, pois apresenta uma ferrita mais rica em cromo e nitrogênio. / In the present work the phenomena of strain hardening, formation and reversion of the strain induced alpha-prime martensite (a\', body centered cubic, BCC, Ferromagnetic) in an UNS S31803 duplex and UNS S32520 super duplex stainless steels have been studied. Firstly, the microstructures of both materials in the solution annealed condition were characterized with the aid of several microstructural analysis complementary techniques. The volume fraction, crystalline structure, chemical composition, size and morphology of the two phases (ferrite and austenite) have been determined. Further, both steels were deformed by two methods: cold rolling, divided into several stages, with lower strain levels than filing, which the chips resulting had higher strain levels. The phenomena of strain hardening, formation and reversion of strain induced martensite in the austenite phase, recovery and recrystallization of austenite and ferrite phases have been studied, mainly using X-ray diffraction and the Rietveld method. X-ray diffraction was also used to determine the residual microstrain and crystallite size (sub grain), calculated from the diffraction peak broadening caused by straining. Thus, the levels of cold rolling and filing strains could be compared. Qualitatively, the formation and reversion of strain induced martensite was also studied by magnetic measurements using data from magnetic saturation of hysteresis curves obtained with the aid of a vibrating sample magnetometer. It has been observed that for the duplex stainless steel, both filing as well as cold rolling promoted strain induced martensite. On the other hand, for the super duplex stainless steel, just filing promoted this transformation. In the comparing with duplex, the super duplex stainless steel austenite is more stable that is why is richer in nitrogen, so, the strain induced martensite formation is more difficult. The easier sigma phase precipitation during annealing as well in the super duplex stainless steel is due higher levels of chrome and molybdenum than the duplex stainless steel.