The hot forming-quenching (HFQ) process has introduced grains and subgrain growth, accompanied with modification of the intermetallic particle distribution in AZ31 magnesium alloys. Each region of the HFQ component represents significant grain structure variation and surface conditions that contributed to the corrosion susceptibility. The homogeneous grain structure significantly ruled the corrosion propagation features by filiform-like corrosion. Immersion of AZ31 alloys in 3.5 wt.% NaCl indicated higher corrosion rate of HFQ TRC (corrosion rate: 10.129 mm/year), a factor of 10 times, higher than the rolled alloy (corrosion rate: 0.853 mm/year) and a factor of 2 times, higher than the corrosion rate of MCTRC alloy (corrosion rate: 5.956 mm/year). Much lower corrosion rate was indicated in the as-cast TRC and MCTRC alloys, compared to the alloys after HFQ process that revealed the contribution of network or continuous distribution of β-Mg17Al12 phase particles to reduce the corrosion driven in chloride solution. In contrast, discontinuous distribution of cathodic β-Mg17Al12 phase particles increases the corrosion rate of HFQ TRC alloy by promoting the cathodic reaction and intense filament propagation resembling the coarse interdendritic and grain boundaries attack. The presence of high population densities of cathodic Al8Mn5 particles in HFQ rolled AZ31B-H24 alloy significantly reduced the corrosion driven for intense corrosion attack on the rolled alloy. The surface preparation by mechanical grinding process induced MgO and Zn-enrichment layer, accompanied with near surface deformed layer that consisted of nanograins in the range size of 40 to 250 nm. The grinding process refined the surface by removing the cutting damage and marks that formed during the thermomechanical process and led to stable potential of the HFQ AZ31 alloys, in the range of -1.59 to -1.57 V, during open circuit potential (OCP) measurement. The surface regularity with grinding path causing the filament to propagate following the grinding direction. The as-received surface contained many cutting damages and deep scratch marks from the rolling and casting processes that could introduce many corrosion initiation sites. The absence of the grinding direction on the as-received surface could control intense corrosion susceptibility, due to the non-linear filament propagation. The surface irregularity on chromic acid cleaned surface of HFQ rolled AZ31B-H24 alloy also contributed to low corrosion potential of the rolled alloy during OCP and potentiodynamic polarization measurement.

Spark Plasma Sintering (SPS) is a promising rapid consolidation technique that allows a better understanding and manipulating of sintering kinetics and therefore makes it possible to obtain Si3N4-based ceramics with tailored microstructures, consisting of grains with either equiaxed or elongated morphology. The presence of an extra liquid phase is necessary for forming tough interlocking microstructures in Yb/Y-stabilised α-sialon by HP. The liquid is introduced by a new method, namely by increasing the O/N ratio in the general formula RExSi12-(3x+n)Al3x+nOnN16-n while keeping the cation ratios of RE, Si and Al constant. Monophasic α-sialon ceramics with tailored microstructures, consisting of either fine equiaxed or elongated grains, have been obtained by using SPS, whether or not such an extra liquid phase is involved. The three processes, namely densification, phase transformation and grain growth, which usually occur simultaneously during conventional HP consolidation of Si3N4-based ceramics, have been precisely followed and separately investigated in the SPS process. The enhanced densification is attributed to the non-equilibrium nature of the liquid phase formed during heating. The dominating mechanism during densification is the enhanced grain boundary sliding accompanied by diffusion- and/or reaction-controlled processes. The rapid grain growth is ascribed to a dynamic ripening mechanism based on the formation of a liquid phase that is grossly out of equilibrium, which in turn generates an extra chemical driving force for mass transfer. Monophasic α-sialon ceramics with interlocking microstructures exhibit improved damage tolerance. Y/Yb- stabilised monophasic α-sialon ceramics containing approximately 3 vol% liquid with refined interlocking microstructures have excellent thermal-shock resistance, comparable to the best β-sialon ceramics with 20 vol% additional liquid phase prepared by HP. The obtained sialon ceramics with fine-grained microstructure show formidably improved superplasticity in the presence of an electric field. The compressive strain rate reaches the order of 10-2 s-1 at temperatures above 1500oC, that is, two orders of magnitude higher than that has been realised so far by any other conventional approaches. The high deformation rate recorded in this work opens up possibilities for making ceramic components with complex shapes through super-plastic forming.

The unique features of the Spark plasma sintering (SPS) were used to investigate the sintering and deformation behaviour of titanium and titanium–titanium diboride composites, and to control the sintering and grain growth of ferroelectric Na0.5K0.5NbO3 (NKN) and of hydroxyapatite (HAp). In the SPS the samples experience a temperature different from that recorded by the thermocouple (pyrometer) used and this temperature difference has been estimated for Ti and NKN.   Sintering and deformation of titanium was investigated. Increasing heating rate and/or pressure shifted the sintering to lower temperatures, and the sintering and deformation rates changed when the α→β phase transition temperature was passed. Fully dense Ti/TiB2 composites were prepared. The Ti/TiB2 composites could be deformed at high temperatures, but the hardness decreased due to the formation of TiB.    The kinetic windows within which it is possible to obtain fully dense NKN and HAp ceramics and simultaneously avoid grain growth are defined. Materials have a threshold temperature above which rapid and abnormal grain growth takes place. The abnormal grain growth of NKN is due to a small shift in the stoichiometry, which in turn impairs the ferroelectric properties. Fully transparent HAp nanoceramics was prepared, and between 900 and 1050 oC elongated grains are formed, while above 1050 oC abnormal grain growth takes place.NKN samples containing grains of the sizes 0.35–0.6 µm yielded optimum ferroelectric properties, i.e. a high remanent polarization (Pr = 30 µC/cm2) and high piezoelectric constant (d33= 160 pC/N). The ferroelectric domain structure was studied, and all grains exhibited a multi-domain type of structure. / At the time of doctoral defense the following articles were unpublished and had a status as follows: Article 4: Manuscript; Article 5 : Manuscript

Static abnormal grain growth (SAGG) was studied in Al-Mg alloy AA5182 sheet by varying four processing parameters: deformation temperature, strain rate, annealing temperature, and annealing time. SAGG is a secondary recrystallization process related to geometric dynamic recrystallization (GDRX) and requires both deformation at elevated temperature and subsequent static annealing. A minimum temperature is required for both SAGG and GDRX. Recrystallized grains only develop at strains larger than the critical strain for SAGG, [epsilon]SAGG. The size of the recrystallized grains is inversely related to and controlled by the density of SAGG nuclei, which increases as local strain increases. The results of this study suggest that SAGG is controlled by two thermally-activated mechanisms, dynamic recovery and recrystallization. During deformation, dynamic recovery increases as deformation temperature increases or strain rate decreases, increasing the critical strain for SAGG. SAGG is subject to an incubation time that decreases as annealing temperature increases. SAGG can produce grains large enough to reduce yield strength by 20 to 50 percent. The results of this study suggest strategies for avoiding SAGG during hot-metal forming operations by varying processing conditions to increase [epsilon]SAGG. / text

This work concerns the microstructure of CSS-grown CdTe layers used for CdTe/CdS solar cells. Particular attention is given to how the development of microstructure on annealing with CdCl(_2) may correlate with increases in efficiency. By annealing pressed pellets of bulk CdTe powder, it is shown that microstructural change does occur on heating the material, enhanced by the inclusion of CdCl(_2) flux. However, the temperature required to cause significant effects is demonstrated to be higher than that at which heavy oxidation takes place. The dynamics of this oxidation are also examined. To investigate microstructural evolution in thin-films of CdTe, bi-layers of CdTe and CdS are examined by bevelling, thus revealing the microstructure to within ~1 µm of the interface. This allows optical microscopy and subsequent image analysis of grain structure. The work shows that the grain- size, which is well described by the Rayleigh distribution, varies linearly throughout the layer, but is invariant under CdCl(_2) treatment. Electrical measurements on these bi-layers, however, showed increased efficiency, as is widely reported. This demonstrates that the efficiency of these devices is not dictated by the bulk microstructure. Further, the region within 1 µm of the interface, of similar bi-layers to above, is examined by plan-view TEM. This reveals five-fold grain-growth on CdCl(_2) treatment. Moreover, these grains show a considerably smaller grain size than expected from extrapolating the linear trend in the bulk. These observations are explained in terms of the pinning of the CdTe grain size to the underlying CdS, and the small grain size this causes. A simple model was proposed for a link between the grain-growth to the efficiency improvement. The study also examines the behaviour of defects within grains upon CdCl(_2) treatment provided the first direct evidence of recovery on CdCl(_2) treatment in this system. Finally, a computer model is presented to describe the evolution of microstructure during growth. This is shown to be capable of reproducing the observed variation in grain size, but its strict physical accuracy is questioned.

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A aplicação de modelos matemáticos baseados em técnicas numéricas aumentou com o avanço da informática através da criação de microprocessadores mais velozes e periféricos de armazenamento de dados com grande capacidade. Buscando uma maior produtividade e a melhoria da qualidade final do produto solidificado, propõe-se neste trabalho, desenvolver um modelo computacional de origem físico para o crescimento de grão no Lingotamento Contínuo. O modelo é simulado utilizando o Método de Monte Carlo juntamente com o Método das Diferenças Finitas, com o objetivo de obter e caracterizar a transição colunar-equiaxial através desse método. As simulações foram realizadas utilizando a programação Fortran 90/95 no ambiente Linux através do software Developer Studio e aplicados nos aços SAE 1015 e 1020. A seguir, foram realizadas comparações entre as macroestruturas simuladas e as macroestruturas das amostras dos aços obtidas pelo Laboratório de Fundição (LAFUN) da UFRGS. Destas simulações observou-se que o modelo oferece a possibilidade da simulação de diferentes condições operacionais para prever a evolução macroestrutural de lingotes. / The application of mathematical models based on numerical techniques increased with the advancement of information technology by creating faster microprocessors and peripherals with high data storage capacity. Seeking for a major productivity and the improvement of the final quality of the solidified product. In this assignment, the development of a computational model with a physical origen for the growth of the continuous casting, is proposed. The model is simulated by using the Monte Carlo Method with the Finite Differences Method, the goal is to obtain and characterize the columnar-equiaxed transition through this method. The simulations were performed using the Fortran 90/95 programming in Linux environment using the Developer Studio software and applied to the steel SAE 1015 and 1020. Following it, comparisons were made between the macro and simulated macrostructures of the samples obtained by the Laboratory of Steel Casting - Laboratório de Fundição (LAFUN) at UFRGS. From these simulations, it was observed that the modified model offers the possibility of simulating different operating conditions to predict the evolution of macrostructural ingots.

Les alliages ODS (Oxides Dispersion Strengthened), sont principalement étudiés pour leur capacité à répondre favorablement au cahier des charges de la fonction de gainage combustible pour les réacteurs nucléaire de type RNR-Na (Réacteur à Neutrons Rapides à caloporteur sodium). Elaborés par métallurgie des poudres, mécanosynthèse puis extrusion, ils affichent des propriétés mécaniques, et notamment en fluage, extrêmement intéressantes. Néanmoins, la voie élaboration utilisée induit une forte anisotropie microstructurale. Cette anisotropie se retrouve au niveau de leurs propriétés mécaniques et conduit à une fragilité dans le sens de sollicitation transverse. Le but de cette thèse est d'étudier l'évolution microstructurale de ces matériaux. Les aciers ODS présentent des microstructures ultra fines en termes de grains, de précipités, et de formation d'amas qui conduisent à de grandes difficultés pour en obtenir la recristallisation. De plus, les microstructures obtenues présentent souvent une recristallisation avec croissance anormale. De telles évolutions demandent des investigations à très fine échelle et ont été relativement peu examinées dans le domaine des alliages ODS. Il faut en effet être capable d'une étude structurale la plus quantitative possible de la microstructure des nanograins, ainsi que de la précipitation afin d'étudier les mécanismes d'interaction précipitation / joints de grain. Ceci n'est possible que par un couplage de différentes méthodes : la microscopie électronique en transmission (en particulier avec l'utilisation des outils récemment développés pour l'étude de la nanotexturation, i.e. ACOM-TEM); la diffusion centrale des neutrons ou des rayons X; et enfin la sonde atomique tomographique, à la fois pour apporter les informations sur la morphologie et la chimie des amas et nanoprécipités mais surtout sur la composition chimique aux joints de grains. A partir de l'identification des mécanismes contrôlant la croissance anormale, une modélisation permettant de prédire son apparition dans la microstructure est confrontée à cette caractérisation microstructurale poussée. Cette modélisation prête une attention particulière à la migration des joints de grains couplée à la diffusion et effets d'ancrage préférentiel des joints triples par les précipités ainsi qu'à l'énergie motrice stockée sous forme de densité de dislocation. / Oxide Dispersion Steels (ODS) alloys are mainly studied for their ability to fulfil the technical specifications required for Sodium Fast Reactor (SFR) fuel cladding application. Their processing involves powder metallurgy, mechanical alloying and extrusion. Therefore, despite their interesting mechanical creep properties, the extrusion processing involves a high microstructural anisotropy. These particular feature leads to poor mechanical properties in the transverse direction which are worsen by the occurrence of abnormal grain growth. Unfortunately, since internal pressure increases in the tube with the accumulation of gas fission products, the major stress component is precisely applied in the transverse direction. As a result, the material faces a critical risk of failure and control of the microstructure is a key issue. The aim of this thesis is to study the microstructural evolution of ODS ferritic steels. ODS ferritic steels show ultrafine microstructures in terms both grains and precipitates which made the recrystallization very difficult and allow for abnormal grain growth. To observe such evolutions, fine scale microstructure characterization are necessary. This is only possible by coupling different characterization methods: transmission electronic microscopy (in particular with the new developed tools for nanotexturation studies, i.e. ACOM-TEM); neutron and X-ray small angle scattering; and atomic probe tomography. Based on the mechanisms that lead to and control the abnormal grain growth, a model to predict the occurrence of abnormal grain growth is confronted to the experimental results. This model that takes a particular attention to the dislocation stored energy effect to adequately reproduce the observed characterization results.

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