The aim of this work was to systematically study how the microstructure evolution is affected by the carbon activity in WC-Ni cemented carbides. Seven WC-9.59at%Ni alloys with different carbon activity were sintered at 1500 °C. From investigating these alloys, the carbon window has been experimentally evaluated using light optical microscopy and compared to theoretical carbon window calculated using Thermo-Calc. The overall microstructure of cross sections and raw surfaces have been investigated using scanning electron microscopy. Finally, the WC grain size and distribution have been evaluated using electron backscatter diffraction. It was found that the experimental carbon window was slightly wider than the theoretical carbon window. The WC grain size increased and the grain size distribution got wider with increasing carbon activity. In addition, the largest WC grains showed the largest grain growth by increasing carbon activity. By comparing the present results of grain size and distribution of WC-Ni to previous results of WC-Co, it was found that the WC grain growth was more pronounced and more influenced by the carbon activity.

This thesis consists of a thermodynamically based kinetic model that more accurately predicts grain boundary mobility (GBM) over a large range of thermodynamic states including changes in temperature, pressure and shear stress. The form of the model was validated against calculated GBM values for Al bicrystals via molecular dynamics (MD) simulations. A total of 98,786 simulations were performed (164 different GBs, each with a minimum of 250 different thermodynamic states, and 2 different driving forces). Methodology for the computation of the GBM via MD simulations is provided. The model parameters are directly linked to extensive thermodynamic quantities and suggest potential mechanisms for GBM under combined thermal and triaxial loads. This thesis also discusses the influence of GB character on the thermodynamic mobility parameters. The resulting insights about GB character and thermodynamic state on GBM suggest an opportunity to achieve designed microstructures by controlling thermodynamic state during microstructure evolution.

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No description available.

Tato doktorská práce se zabývala mikrostrukturálním vývojem vybraných oxidových keramických materiálů během konvenčního slinování (CS), rychlého slinování (RRS), flash slinování (FS) a slinování pomocí plazmatu (SPS). S ohledem na keramiku pro strukturální aplikace byly pomocí RRS připraveny relativně velké (1 cm3), bez defektní a téměř hutné pelety oxidu hlinitého a yttriem stabilizovaného oxidu zirkoničitého (YSZ) s homogenní mikrostrukturou. RRS bylo také shledáno jako optimální metoda pro přípravu vysoce hutné bezolovnaté piezoelektrické keramiky s podobnými vlastnostmi, jako byly získány po časově a energeticky náročnějším CS. Metoda SPS dále zlepšila vlastnosti bezolovnaté piezoelektrické keramiky a produkovala plně hutné vzorky, což je dobrým předpokladem pro translucenci a z níž vyplývajícím optoelektrickým vlastnostem. Nejoptimálnějších výsledků – plné hustoty a vysokých piezoelektrických vlastností – bylo dosaženo kombinací SPS a RRS. Analýzy provedené v této studii také poukázaly na důležitost eliminace těkavých nečistot před rychlým ohřevem. Jinak totiž dochází k zachycení těchto látek ve slinuté keramice, což ve výsledku limituje její konečnou hustotu. Ukázalo se, že nízké konečné hustoty RRS YSZ jsou spojeny se zachycením zbytkového chloru pocházejícího ze syntézy prášku. Pokud byl zbytkový chlor odstraněn vysokoteplotním žíháním keramických kompaktů před zahájením RRS, byly touto metodou získány téměř plně hutné YZS vzorky. Negativní vliv zbytkového chloru na zhutnění byl viditelný také u flash slinovaných YSZ vzorků. Navíc FS YSZ často vede ke zrychlení růstu zrn v jádře vzorku, v důsledku vyšší teploty a elektrochemické redukce. Ve spektru procesních parametrů použitých v rámci této práce dokonce došlo k abnormálnímu růstu zrna (AGG). Silně bimodální distribuce velikosti zrn ukázaná v této práci nebyla dříve nalezena u flash slinutého YSZ. AGG byl vysvětlen dvěma přispívajícími faktory – relativně velkou velikostí vzorku, která vedla k lokalizaci elektrického proudu a vzniku horkých míst (z angl. hot-spots), a celkově akcelerovanou kinetikou růstu zrn v jádře vzorku způsobenou elektrochemickou redukcí.

La taille de grains dans le manteau terrestre a des implications cruciales sur les processus à grande échelle, telles que la propagation des ondes sismiques, la perméabilité et la rhéologie des roches. Cependant, la taille de grains évolue constamment avec le temps, car la croissance de grains statique induit une augmentation de la taille moyenne tandis que la recristallisation dynamique contribue à sa décroissance. La croissance d’olivine au sein d’agrégats mantelliques dans un milieu inter-granulaire sec, en présence de liquide magmatique ou dans des conditions sursaturées en eau a été modélisée dans le cadre de cette thèse. En s’appuyant sur la théorie de croissance cristalline ainsi que sur des expériences à 1-atmosphère et hautes températures précédemment publiées, la loi de croissance d’olivine sèche a été déterminée. Le facteur limitant est, dans ce cas, la diffusion du silicium aux joints de grains à travers une épaisseur effective de 30 nm. La croissance d’agrégats en présence de liquide magmatique et fluide aqueux a été contrainte par de nouvelles expériences haute pression/haute température. Ces données indiquent que les taux de croissance sont significativement plus importants que dans des conditions sèches et sont limités par des réactions aux interfaces cristal/liquide. Nous proposons une loi de croissance générale régulée par une combinaison de joints de grains secs et mouillés, grâce aux paramètres de contiguité et de mouillabilité. Cette loi de croissance unifiée est fondamentale pour extrapoler les tailles de grains expérimentales à des échelles de temps, des profondeurs et des quantités de liquides relatives au manteau supérieur. / Grain size in the Earth’s mantle is a fundamental parameter that has crucial implications on large-scale processes, such as seismic wave propagation, the permeability and the rheology of rocks. However, grain size is constantly evolving with time, where static grain growth implies an increase of the average grain size whereas dynamic recrystallization contributes to its decrease. Static grain growth of olivine-rich mantle aggregates in an intergranular medium being dry, melt-bearing and water-oversaturated has been here modeled. By using the appropriate theoretical background, the dry olivine grain growth law has been established from previously published experimental grain growth data at 1-atmosphere and high-temperature conditions. Grain growth rates for these samples are limited by silicon diffusion at grain boundaries through an effective width of 30 nm. Grain growth for melt- and water-bearing aggregates was, however, constrained by new high-pressure and high-temperature experiments. This data indicates that grain growth rates for liquid-bearing samples are significantly faster than for dry samples and are limited by precipitation reactions at the crystal/liquid interface rather by diffusion through the liquid phase. We propose a general grain growth law, which takes into account dry grain boundaries as well as wetted grain-grain interfaces, through the contiguity and wetness parameters. This unified law is fundamental to extrapolate experimental grain sizes to time scales, depths and liquid contents that are relevant of the upper mantle.

O Processamento e Análise Digital de Imagens é utilizado cada vez mais para agilizar processos, aumentar a precisão, segurança e confiabilidade de dados extraídos de imagens nas mais diversas áreas de pesquisa. No entanto, muitas vezes é necessário que o pesquisador faça, ele próprio, o pré-processamento das imagens, mesmo não sendo um especialista nesta área. Isto coloca em risco o próprio objetivo do uso do Processamento e Análise Digital de Imagens. Este trabalho analisa a relação dos dados extraídos de uma imagem (micrografia) através do software livre ImageJ com relação ao seu processamento final desejado, avaliando assim, a necessidade ou não, de uma ou mais sequencias de pré-processamento para adequar a imagem para o processamento final, indicando ainda quais fatores de influência apresentam informações irrelevantes ou incompletas para o processamento final utilizando ferramentas da Lógica Paraconsistente Anotada. Os resultados obtidos mostram que esta abordagem carece de informações diversificadas sobre a imagem original capturada que possam subsidiar a tomada de decisão quanto aos procedimentos necessários e, para o pré-processamento adequado ao objetivo desejado. / Processing and Analysis of Digital Images is increasingly used to streamline processes, improve accuracy, safety and reliability of data extracted from images in various research areas. However, it is often necessary for the researcher to make himself, the preprocessing of images, although not an expert in this area. This puts at risk the very purpose of using the Processing and Analysis of Digital Images. This paper analyzes the relationship of the data extracted from an image (micrograph) through the free software ImageJ, with respect to its desired final processing. Thus, evaluating the necessity or not, of one or more sequences of preprocessing to adjust the image to the final processing, further indicating which factors influence presents incomplete or irrelevant information for final processing using tools of Annotaded Paraconsistent Logic. The results show that this approach lacks diversified information about the original image captured that can support decision making about procedures for appropriate preprocessing to the desired goal.

<p>Cemented carbides (WC-Co) are powder metallurgical products produced by liquid phase sintering. WC-Co is widely used for making a large variety of cutting tools, such as drills and inserts turning applications, due to its great mechanical properties, where the hardness of the WC grains is combined with the toughness of the of the Co binder. WC grain size and grain size distribution are the two most important factors to control the mechanical properties of the products.</p><p>This study examined the grain growth dependence of different milling and sintering times. The resulting grain size and grain size distribution were measured using image analysis on scanning electron microscopy images (SEM) and by using electron backscatter diffraction (EBSD). In addition, the correlation between hardness and coercivity, the most common indirect measures of grain size, and different methods of calculating average grain radius were investigated. An attempt was also made to study the contribution of defects to grain growth. This work also includes an overview of various grain growth equations and a numerical implementation of these.</p><p>Experimental results show that for shorter sintering times, powders milled for short times (15 min and 1 h) have larger average grain radii. There is a crossover after 6 to 8 h of sintering, where the powders milled for a long time (40 h and 200 h), have larger average radii. The measured hardness values correlate well with the average grain radius calculated from the grain surface area and the coercivity correlates with the established equations. EBSD measurements detected boundaries that could not be detected by image analysis, and that were not Sigma 2 boundaries. It is likely that these boundaries are either low energy boundaries or boundaries between grains that are very closely oriented. Comparing heat-treated powder with the untreated resulted in a lower average grain size after sintering for the heat-treated powder. None of the growth equations investigated in this work could fully describe the experimental grain growth.</p><p>Through increased understanding of the grain growth, the growth can be controlled and the end product can have the desired tool properties. The occurrence of abnormal grains in cutting tool applications can cause breakage, which is especially important to avoid in applications such as PCB drills. A correlation between hardness and grain size provides further means for cheap and fast indirect measures of the grain size in production.</p> / <p>Hårdmetall är ett pulvermetallurgiskt material som tillverkas genom smältfassintring och som kännetecknas av hårdhet, styvhet och god slitstyrka. Volframkarbidens (WC) kornstorlek och kornstorleksfördelning är två viktiga faktorer för att kontrollera de mekaniska egenskaperna i hårdmetall.</p><p>I den här studien har korntillväxtens beroende på malning och sintring undersökts. WC-Co maldes och sintrades fyra olika tider och kornstorleksfördelningen mättes med bildanalys på svepelektronmikroskopbilder samt med ``electron backscatter diffraction'' (EBSD). I arbetet har även korrelationen mellan hårdhet, koercivitet och olika sätt att beräkna medelkornstorleken undersökts. Ett försök har också genomförts för att studera hur defekterna i det malda pulvret påverkar korntillväxten. I arbetet har även ett flertal olika tillväxtekvationer modellerats numeriskt och för och nackdelar med de olika tillväxtekvationerna har vägts mot varandra.</p><p>En lång maltid (40 h och 200 h) visade sig ge liten kornstorlek för sintring kortare än 6 h, men för sintringar längre än 8 h gav istället kort malning (15 min och 1 h) den mindre kornstorleken. Det visade sig att uppmätt hårdhet korrelerar bäst med den medelkornstorleksradie som räknats fram från kornytan. I EBSD mätningarna kunde man observera ett flertal korngränser, utöver Sigma 2 korngränser, som inte hade detekterats med bildanalys. Värmebehandlingen av det malda pulvret minskade korntillväxten under efterföljande sintring. Ingen av de undersökta tillväxtekvationerna kunde beskriva de experimentella resultaten fullt ut.</p><p>Genom ökad förståelse för korntillväxt kan man kontrollera tillväxten och slutprodukten kan få önskade egenskaper. Förekomsten av abnorm korntillväxt i skärverktyg i hårdmetall är en av de vanligaste kritiska defekterna och det är speciellt viktigt är undvika korntillväxt i tillverkning av små verktyg, som till exempel kretskortsborrar. Hårdhet och koercivitet är de vanligaste indirekta mätmetoderna för att mäta kornstorlek i produktion. En bra korrelation mellan kornstorlek och indirekta mätmetoder ger utökade verktyg för snabba och billiga mätningar.</p>

O Processamento e Análise Digital de Imagens é utilizado cada vez mais para agilizar processos, aumentar a precisão, segurança e confiabilidade de dados extraídos de imagens nas mais diversas áreas de pesquisa. No entanto, muitas vezes é necessário que o pesquisador faça, ele próprio, o pré-processamento das imagens, mesmo não sendo um especialista nesta área. Isto coloca em risco o próprio objetivo do uso do Processamento e Análise Digital de Imagens. Este trabalho analisa a relação dos dados extraídos de uma imagem (micrografia) através do software livre ImageJ com relação ao seu processamento final desejado, avaliando assim, a necessidade ou não, de uma ou mais sequencias de pré-processamento para adequar a imagem para o processamento final, indicando ainda quais fatores de influência apresentam informações irrelevantes ou incompletas para o processamento final utilizando ferramentas da Lógica Paraconsistente Anotada. Os resultados obtidos mostram que esta abordagem carece de informações diversificadas sobre a imagem original capturada que possam subsidiar a tomada de decisão quanto aos procedimentos necessários e, para o pré-processamento adequado ao objetivo desejado. / Processing and Analysis of Digital Images is increasingly used to streamline processes, improve accuracy, safety and reliability of data extracted from images in various research areas. However, it is often necessary for the researcher to make himself, the preprocessing of images, although not an expert in this area. This puts at risk the very purpose of using the Processing and Analysis of Digital Images. This paper analyzes the relationship of the data extracted from an image (micrograph) through the free software ImageJ, with respect to its desired final processing. Thus, evaluating the necessity or not, of one or more sequences of preprocessing to adjust the image to the final processing, further indicating which factors influence presents incomplete or irrelevant information for final processing using tools of Annotaded Paraconsistent Logic. The results show that this approach lacks diversified information about the original image captured that can support decision making about procedures for appropriate preprocessing to the desired goal.

The content of this thesis is about preparation and processing of lead-free piezoceramic materials with perovskite structure. Potassium sodium niobate (KNN) powder was prepared by solid state reaction (SSR) and liquid phase reaction (sol-gel reaction). The powders were formed by uniaxial and isostatic pressing and further sintered. The density, grain size and morphology were determined on the sintered samples. The powder, synthesised by SSR and sintered in a conventional furnace, was chosen as a standard. The maximum density achieved on samples after optimization of sintering cycle was 93 %TD. The sintering optimization involved a homogenization step at 950 °C, which promotes the correct development of the phase composition and microstructure, followed by sintering at 1120 °C. The same approach and sintering cycle were used for sintering the samples, prepared by sol-gel synthesis. The maximum density of the samples prepared by sol-gel reaction and sintered in a conventional way, was 92 %TD. For further comparison, both of the synthesised powders were sintered using SPS (spark plasma sintering), which increased their final density up to 97 %TD. The approximate value of the piezoelectric coefficient d33 (pC/N) has been measured on selected SSR samples with pure phase composition ((K0,5Na0,5)NbO3). The best measured value of d33 was around 100 pC/N.