Over the past decades, microwave sintering has been investigated, and the effects of microwave sintering have been demonstrated, however there is still uncertainty as to what is causing the enhancements known as the microwave effect . For a better understanding of the microwave effect , the effect of microwaves on the pore size distribution during densification has been investigated for submicron-sized zinc oxide (ZnO), which was sintered with conventional heating and varying amounts of microwave power but always maintaining exactly the same time-temperature profile. Initially, the density of the sintered samples was measured and compared; this proved that the densification of the hybrid sintered samples was increased and that the higher the level of microwaves used, the more it enhanced the densification. After this, the porosity was investigated through the use of nitrogen adsorption analysis, mercury porosimetry and Field Emission Gun Scanning Electron Microscopy (FEGSEM). Initially, it was found that sintering with microwaves reduces pores faster than for conventional sintering as expected. However, the experiments also revealed that the mechanisms of the reduction in the porosity were not different for microwave sintering compared to conventional sintering. When the porosity was compared at equivalent densities, it was observed that there was no significant difference, either in terms of the amount of porosity or the microstructure development. Since the structural development was the same for both conventional and hybrid sintering, it was concluded that the cause for the enhancement of the densification was enhanced diffusion caused by an additional driving force induced by the microwave field. The investigation of the solid-state reaction between zinc oxide and alumina was designed to investigate whether the diffusion associated with reactions was also enhanced by the use of microwaves. Therefore, zinc oxide and alumina samples were reacted as diffusion couples using conventional and hybrid heating, the latter with varying amounts of microwave power. The analyses of the reaction layer using FEGSEM showed an increase in the reaction product layer thickness when hybrid heating was used, with a higher level of microwaves yielding more growth. These results supported the view that the enhanced reaction rates were caused by enhanced diffusion, again caused by an additional driving force induced by the microwave field. For both the densification and reaction cases, the most likely additional driving force is considered to be the ponderomotive effect.

As técnicas de sinterização convencional de zircônia tetragonal parcialmente estabilizada com ítria (Y-TZP) vêm apresentando limitações quanto ao tempo e temperatura de sinterização, aumentando o custo do produto biocerâmico. Assim, a sinterização por micro-ondas se torna uma alternativa apropriada promovendo rápido aquecimento, elevadas densidades, controle de tamanho de grão, reduzindo o tempo total para produzir o material cerâmico desejado. O objetivo do presente trabalho foi comparar o efeito da sinterização por micro-ondas de cerâmicas comerciais Y-TZP pré-sinterizadas (grupos V-M e LP-M) e outra produzida a partir de pós sintetizados pela técnica de coprecipitação (grupo CP-M). Valores de densidade, tenacidade à fratura, tamanho de grão, translucidez e quantificação das fases cristalinas de amostras sinterizadas, antes e após envelhecimento em reator hidrotérmico, foram relatados. Os grupos V-M e CP-M de amostras foram sinterizados a 1450°C e 1350°C por 15 e 30 minutos e o grupo LP-M, sinterizado apenas a 1450°C, nos mesmos tempos. Os grupos sinterizados a 1450°C por 15 e 30 minutos apresentaram os maiores valores de densidade (média de 98% em relação à densidade teórica). O tamanho médio de grão das amostras de maior densificação variou de 309 a 355 nm. Os resultados de translucidez (ΔE) são próximos aos divulgados na literatura. A quantificação de fases por difratometria de raios X das amostras não envelhecidas, indicou que em sua maioria, são formadas por 89% de fase tetragonal e 11% fase cúbica. Os ensaios de envelhecimento hidrotérmico permitiram verificar o comportamento de degradação de fases das amostras sinterizadas em micro-ondas, demonstrando que, no caso das cerâmicas comerciais, essa técnica é uma alternativa viável para produção de cerâmicas Y-TZP mais resistentes à degradação. / Conventional sintering techniques of yttria-tetragonal zirconia polycrystals (Y-TZP) ceramics have presented limitations regarding the sintering time and temperature, increasing the cost of the final dental and biomedical products. Herein, microwave sintering comes to be an interesting alternative by providing fast heating, high densification and grain size control, reducing the overall processing time to produce the desired ceramic material. The aim of this study was to compare the effect of microwave sintering of a pre-sintered Y-TZP dental ceramics (V-M and LP-M groups) and other prepared from powders synthesized in a laboratorial scale by the precipitation route (CP-M group). Values of densification, fracture toughness, grain size, translucency and crystalline phases quantification of aged and non-aged sintered samples were reported. The groups V-M and CP-M were sintered at 1450°C and 1350°C for 15 and 30 minutes and the group LP-M was sintered at 1450°C at the same times. The sintered samples at 1450°C for 15 and 30 minutes presented the highest density values (around 98% related to theoretical density). The average grain size of highest density samples varied between 309 a 355 nm. The translucency (ΔE) results were similar to the reported literature. The X-ray diffraction crystalline phase quantification analysis indicated that the majority of the non-aged samples were formed by 89% tetragonal phase and 11% cubic phase. The hydrothermal tests allowed to verify the phase degradation behavior under wet environment of microwave sintered samples, indicating that in the case of commercial ceramics, this technique as an viable alternative for production of better degradation resistance Y-TZP ceramics.

In this study, prealloyed austenitic stainless steel and premixed soft magnetic Ni-Fe permalloy compacts were consolidated through microwave and conventional sintering routes at combinations of various sintering temperatures and compaction pressures. Sintered alloys were characterized in terms of their densification, microstructural evolution as well as mechanical and magnetic properties. The effect of sintering method in terms of the applied sintering parameters on the final properties of the compacts were investigated in a comparative manner. It was determined that microwave sintered permalloys are superior compared to their conventionally sintered counterparts in densification response, microstructural characteristics such as pore shape and distribution as well as mechanical properties for both austenitic stainless steel and permalloy compacts. However, permeability of the microwave sintered permalloys was inferior to their conventionally sintered counterparts in some cases due to microstructural refinement associated with microwave sintering route.

Made available in DSpace on 2014-12-17T14:07:11Z (GMT). No. of bitstreams: 1 JotaCL_TESE.pdf: 5010463 bytes, checksum: 1561e00830959256c5a6c3c69602a56b (MD5) Previous issue date: 2012-08-30 / O processamento t?rmico de materiais cer?micos via energia de microondas, no est?gio atual, vem ganhando cada dia mais import?ncia, tendo em vista suas in?meras aplica??es, como por exemplo: aplica??o de microondas na ?rea de processamento mineral (aquecimento de min?rios antes da moagem, secagem, redu??o carbot?rmica de ?xidos minerais, lixivia??o, fus?o, pr?-tratamento de min?rios e concentrados de ouro refrat?rio, regenera??o de carv?o, etc. de acordo com Kigman & Rowson, 1998). Em virtude de uma s?rie de vantagens em potencial, frente aos m?todos convencionais de aquecimento, como redu??o no tempo de processamento; economia de energia; diminui??o do di?metro m?dio das part?culas e melhoramento nas propriedades tecnol?gicas em geral, esta tecnologia vem se destacando. Neste contexto, o objetivo geral deste trabalho, ? desenvolver uma pesquisa visando identificar e caracterizar novas op??es de mat?rias-primas cer?micas como argilas, feldspatos e caulins que sejam eficazes para definir a formula??o de uma ou mais massas para produ??o de componentes de cer?mica estrutural com propriedades f?sicas, mec?nicas e est?ticas adequadas ap?s passarem por sinteriza??o convencional e por energia de microondas destacando as vantagens desta ?ltima. Al?m dos requisitos t?cnicos e de processo, as formula??es apresentadas dever?o atender ?s expectativas de pre?o e de log?stica de fornecimento. No estudo foram conformados corpos-de-prova por extrus?o e prensagem, sinterizados em fornos microondas e convencional, sob ciclos de queima mais r?pidos que os atualmente praticados. As mat?rias-primas foram caracterizadas e analisadas, utilizando as t?cnicas de fluoresc?ncia por raios X (FRX), difra??o por raios X (DRX), an?lise t?rmica diferencial (DTA), an?lise t?rmica gravim?trica (DTG), an?lise granulom?trica (AG), microscopia eletr?nica de varredura (MEV), absor??o d agua (AA), massa especifica aparente (MEA), porosidade aparente (PA), retra??o linear (RL) e tens?o de ruptura e flex?o (TRF). Os resultados obtidos indicaram que as propriedades tecnol?gicas de Absor??o de ?gua (AA) e Tens?o de Ruptura e flex?o (TRF), proposto no trabalho foram adquiridos com sucesso e est?o bem al?m do limite exigido pelas especifica??es das normas da ABNT NBR 15.270/05 e 15.310/09

This diploma thesis deals with the study of microstructure development during the final stage of sintering of two zirconia based ceramic materials (tetragonal ZrO2 doped with 3 mol% of Y2O3 and cubic ZrO2 doped with 8 mol% of Y2O3). Conventional, microwave and SPS sintering methods were used. Achieved relative densities and mean grain sizes were evaluated for sintered materials. It was found that the non-conventional sintering methods are capable of rapid processing of ceramics with improved microstructure compared to conventional sintering.

ABSTRACT MICROWAVE SINTERING AND CHARACTERIZATION OF ALUMINA AND ALUMINA MATRIX CERAMIC NANOCOMPOSITES Kayiplar, Burcu M.S., Department of Metallurgical and Materials Engineering Supervisor: Assist. Prof. Dr. Arcan F. Dericioglu April 2010, 106 pages Efficiency of microwave heating on the sintering of ceramic materials has been investigated in comparison to conventional processing. Monolithic alumina with or without sintering additives such as MgO, CaO, Y2O3 were fabricated by both conventional and microwave sintering at temperatures ranging from 1000&deg / C to 1600&deg / C with a constant soaking time of 1 hour. Based on the densification results on monolithic alumina, nanometer-sized SiC or stabilized ZrO2 particle-dispersed alumina matrix ceramic nanocomposites were sintered by both methods at 1300&deg / C and 1500&deg / C for 1 hour. Sintered ceramic materials were characterized in terms of densification, microstructural evolution, chemical composition and mechanical properties such as hardness and indentation fracture toughness. Microwave sintering was determined to be a remarkably effective method in the production of Al2O3 ceramics at considerably low temperatures (&amp / #8804 / 1400&deg / C) compared to conventional sintering in achieving enhanced relative densities reaching to ~97% with improved microstructural characteristics and mechanical properties. Usage of sintering additives at temperatures higher than 1400&deg / C was determined to be effective in densifiying Al2O3 by both methods. Second phase particle incorporation yielded poor densification resulting in a decrease of hardness of the fabricated ceramic nanocomposites / however, their fracture toughness improved considerably caused by the crack deflection at the dispersed particles and grain boundaries reaching to ~4 MPa&middot / m1/2 in the case of SiC particledispersed nanocomposites. Compared to conventional sintering, microwave sintering is more effective in the processing of alumina and alumina matrix nanocomposites leading to similar densification values along with improved microstructural and mechanical characteristics at lower temperatures in shorter soaking periods.

[EN] Zirconia has become a widely utilized structural ceramic material with important applications in dentistry due to its superb mechanical properties, biocompatibility, aesthetic characteristics and durability. Zirconia needs to be stabilized in the t-phase to obtain improved mechanical properties such as hardness and fracture toughness. Fully dense yttria-stabilized tetragonal zirconia polycrystalline (Y-TZP) materials are normally consolidated through the energy-intensive processing of powders at very high temperatures (>1000 °C). Innovative non-conventional approaches are being developed to reduce time and energy consumption and, consequently, environmental impact in ceramic powder processing. Microwave sintering is one such approach aimed at fully-densifying ceramics by using a different heating mechanism based on the material's inherent dielectric properties. The main purpose of this work is to obtain highly dense Y-TZP dental materials from commercial and lab-prepared sources via microwave sintering with mechanical and microstructural qualities that are similar or even improved with respect to their conventionally sintered counterparts. Therefore, its effect on important aspects related to dental applications has been studied. First, Y-TZP ceramics have been characterized upon sintering to determine whether the resulting properties meet the minimum mechanical requirements for structural dental applications. Second, the influence of microwave sintering on hydrothermal degradation, a spontaneous ageing phenomenon that affects zirconia materials in wet conditions, has been investigated. And third, the behavior under fretting wear conditions of microwave and conventionally sintered materials has been assessed to evaluate their durability and performance. The main conclusions indicate that microwave sintering allows proper consolidation of dental Y-TZP materials resulting in a finer microstructure due to shorter processing time and mechanical properties comparable, and in some cases enhanced, to those obtained in conventional sintered materials at lower dwell temperatures. Additionally, a higher resistance to hydrothermal degradation has been determined for microwave sintered materials due to a finer grain size and lower sintering temperatures that reduce the presence of cubic phase, which is responsible for destabilizing neighboring tetragonal phase grains. Finally, a similar wear rate has been obtained between microwave and conventional sintering of zirconia materials under fretting wear conditions. In addition, humidity can reduce the wear volume loss due to the lubricative effect of water and wear of degraded materials might increase the resistance due to the formation of a protective debris layer. In general, microwave sintering can be an interesting alternative for obtaining fully-densified Y-TZP dental materials providing certain advantages over conventional methods. Nonetheless, more studies are still necessary to have a better understanding of the advantages and disadvantages of microwave sintering of zirconia ceramics. / [ES] La circona es un material ampliamente utilizado como cerámica estructural con aplicaciones en el ámbito dental debido a sus propiedades mecánicas, biocompatibilidad, características estéticas y durabilidad. Para poder aprovechar las altas propiedades mecánicas de la circona, es necesario estabilizarla en su fase tetragonal. Los materiales de circona policristalina estabilizada con itria (Y-TZP) se consolidan normalmente a través de polvos mediante procesos energéticamente intensivos a altas temperaturas (>1000 °C). Actualmente, se están desarrollando técnicas basadas en métodos no convencionales para reducir el tiempo y el consumo energético en el procesado de polvos cerámicos. La sinterización por microondas tiene por objetivo la densificación completa mediante la utilización de mecanismos de calentamiento basados en las propiedades dieléctricas del material. El objetivo principal es la obtención de materiales dentales de Y-TZP altamente densos mediante la sinterización por microondas con propiedades mecánicas y microestructurales similares, o incluso por encima de las obtenidas por el método convencional. Para ello, se estudian aspectos relevantes al ámbito dental. En primer lugar, los materiales son caracterizados con el fin de determinar si las propiedades finales cumplen con los requisitos mecánicos para aplicaciones dentales. Además, se ha investigado la influencia de la sinterización por microondas en la degradación hidrotérmica, un fenómeno espontáneo de envejecimiento que afecta a los materiales de circona en condiciones de humedad. Finalmente, se ha evaluado el comportamiento en condiciones de desgaste fretting de los materiales sinterizados para determinar su durabilidad. Las conclusiones principales indican que la sinterización por microondas permite la consolidación adecuada de estos materiales, resultando en una microestructura más fina debido a los tiempos más cortos de procesado y en propiedades mecánicas comparables a las de materiales obtenidos mediante el método convencional, incluso a temperaturas más bajas. Una mayor resistencia a la degradación hidrotérmica se ha determinado en materiales sinterizados por microondas. Al emplear temperaturas más bajas se reduce la presencia de fase cúbica, la cual es responsable por la desestabilización de granos adyacentes de fase tetragonal. Tasas de desgaste similares han sido observadas entre materiales sinterizados por microondas y convencionalmente bajo condiciones de desgaste fretting. Adicionalmente, la humedad puede reducir sustancialmente la pérdida de volumen de desgaste debido al efecto lubricante del agua y los materiales degradados pueden aumentar la resistencia a este tipo de desgaste como consecuencia de la formación de una capa protectora de material que se desprende más fácil. En general, la sinterización por microondas es una alternativa interesante para obtener materiales dentales de Y-TZP altamente densos con ciertas ventajas sobre los métodos convencionales pero deben considerarse también las desventajas de esta técnica. / [CAT] La circona és un material àmpliament utilitzat com a ceràmica estructural amb aplicacions en l'àmbit dental a causa de les seues propietats mecàniques, biocompatibilidad, característiques estètiques i durabilitat. Per a poder aprofitar les altes propietats mecàniques de la circona, és necessari estabilitzar-la en la seua fase tetragonal. Els materials de circona policristalina estabilitzada amb itria (Y-TZP) es consoliden normalment mitjançant processos energèticament intensius a altes temperatures (>1000 °C). Actualment, s'estan desenvolupant tècniques basades en mètodes no convencionals per a reduir el temps i el consum energètic en el processament de la pols ceràmicas. La sinterització per microones té per objectiu la densificació completa mitjançant la utilització de mecanismes d'escalfament basats en les propietats dielèctriques del material. L'objectiu principal d'aquesta tesi és l'obtenció de materials dentals de Y-TZP altament densos mitjançant la sinterització per microones amb propietats mecàniques i microestructurals superiors a les obtingudes per mètodes convencionals. En primer lloc, els materials seràn caracteritzats per a determinar si les propietats finals compleixen amb els requisits mecànics per a aplicacions dentals. En segon lloc, s'investigarà la influència de la sinterització per microones en la degradació hidrotèrmica, un fenomen espontani d'envelliment que afecta als materials de circona en condicions d'humitat. I en tercer lloc, s'avaluarà el comportament en condicions de desgast fretting dels materials sinteritzats per a determinar la seua durabilitat. Les conclusions principals indiquen que la sinterització per microones permet la consolidació adequada i millorada de materials de Y-TZP, amb una microestructura més fina a causa dels temps més curts de processament i propietats mecàniques comparables a les de materials obtinguts mitjançant el mètode convencional, fins i tot a temperatures més baixes. Un factor positiu ha sigut la major resistència a la degradació hidrotèrmica en materials sinteritzats per microones. A més, al emprar temperatures més baixes es redueix la presència de fase cúbica, la qual és la responsable de la desestabilització de grans adjacents de fase tetragonal. Finalment, sota condicions de desgast fretting, s'han observat taxes de desgast similars entre materials sinteritzats per microones i via convencional. Addicionalment, en condicions de 100% d'humitat es pot reduir substancialment la pèrdua de volum de desgast a causa de l'efecte lubrificant de l'aigua i materials degradats, els quals poden augmentar la resistència a aquest tipus de desgast com a conseqüència de la formació d'una capa protectora de material que es desprèn amb més facilitat. En general, la sinterització per microones és una alternativa molt interessant per a obtindre materials dentals Y-TZP òptims i amb certes avantatges sobre els mètodes convencionals, però han de considerar-se també algunes desavantatges d'aquesta tècnica. / Presenda Barrera, Á. (2016). ADVANCED CERAMIC MATERIALS FOR DENTAL APPLICATIONS SINTERED BY MICROWAVE HEATING [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/68510 / TESIS

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Le frittage par micro-ondes est une nouvelle technologie de chauffage rapide utilisée pour l’élaboration de matériaux par le procédé de métallurgie des poudres. Cette méthode de frittage est non seulement économique en temps et en énergie, mais peut aussi permettre d’améliorer les propriétés finales du matériau. Cependant, l’effet bénéfique que peut apporter le chauffage par rayonnement micro-ondes n'est pas encore complètement compris.Dans ce cadre, cette thèse porte sur la mise en œuvre et les comparaisons des comportements en frittages conventionnel et micro-ondes multimodes (2,45 GHz) de l’alumine. La densification et l'évolution de la microstructure des échantillons frittés ont été analysés et comparés entre ces deux processus de chauffage en relation avec la nature des poudres de l'alumine : surface spécifique et teneur en dopant magnésie.A partir du suivi dilatométrique du frittage au cours des traitements conventionnel et micro-ondes, nous déterminons en anisotherme les énergies d’activation apparentes, qui sont considérées comme les paramètres importants de la thermodynamique de frittage : les valeurs trouvées sont toujours plus faibles dans le cas du frittage sous champ électromagnétique, preuve que les diffusions conduisant à la densification sont favorisées. Le suivi in situ permet aussi de déterminer les mécanismes de frittage (étude cinétique), par exploitation des courbes obtenues en traitement isotherme : la diffusion aux joints de grains reste le mécanisme dominant dans la plupart des cas, sauf pour une nanopoudre où la réaction d’interface devient le mécanisme limitant sous champ micro-ondes, preuve là encore de l’influence du champ électromagnétique sur la diffusion.Nous avons ainsi mis en évidence et expliqué les effets d’un champ électromagnétique sur le phénomène de densification, contribuant à terme à la maîtrise de l’application du rayonnement micro-ondes dans l’industrie céramique. / Microwave energy has been successfully applied as a heating source in the field of powder metallurgy. Compared with conventional heating techniques, microwave sintering has a high potential to reduce the processing time as well as temperature, and to optimize functional properties. However, the detailed explanation of this enhanced effect underlying microwave sintering is still under debate.Taking into account those issues, the objective of this work was to investigate comparatively conventional and 2.45 GHz microwave multimode sintering of alumina. The densification behavior and microstructure evolution of alumina powders with different MgO doping levels as well as specific surface areas have been systematically and quantitatively studied.By the way of dilatometric measurements in both conventional and microwave processes, studies in terms of thermodynamics were carried out in non-isothermal conditions. The apparent activation energy values are significantly lowered when microwave is applied, indicating a microwave-induced enhancement on diffusion. Furthermore, densification kinetics was isothermally taken in order to study in more detailed manner the mechanism(s) involved during microwave sintering. It suggests that the grain boundary diffusion is the dominant mechanism in most cases, except for a nanopowder. In the case of fine-grained alumina, it was assumed that microwave-assisted densification is controlled by in-series “interface-reaction / grain-boundary diffusion” mechanism. But anyway, grain-boundary diffusion has been always enhanced by microwave non-thermal effect.This work will be meaningful to develop the in-depth understanding of the microwave sintering process at both the fundamental and the applied levels.

Procédé de moulage par injection de poudres est constitué de quatre étapes principales: la préparation des matières premières, moulage par injection, le déliantage et le frittage. Cette thèse présente les recherches sur deux aspects principaux: la micro-injection et frittage par micro -ondes. Les contributions principaux peuvent être conclues dans les quatre aspects suivants: Modification et complément de l'algorithme précédent pour la simulation du procédé de moulage par injection; L'évaluation et la mise en œuvre de l'effet de tension de surface en simulation pour micro-injection; Micro-ondes expériences de frittage de compacts basés sur l'acier inoxydable 17-4PH; Réalisation de la simulation de frittage à micro-ondes avec couplage de la multi-physique, y compris le chauffage à micro-ondes classique, le transfert de chaleur, et le supplément de modèle pour la densification de frittage de la poudre compacté / Powder Injection molding process consists off our main stages: feedstock preparation, injection molding, debinding and sintering. The thesis presents the research on two main aspects: micro injectionmolding and microwave sintering. The main contributions can be concluded in thefollowing four aspects: Modification and supplement of previous algorithm for the simulation ofinjection molding process; Evaluation and implementation of surface tension effect in simulation for micro injection; Microwave sintering experiments of compacts based on 17-4PH stainles ssteel; Realization of the microwave sintering simulation with the coupling of multi-physics,including the classic microwave heating, heat transfer, and the supplement of model for sintering densification of powder impacts