The thesis studies the sintering behaviours and mechanical properties of perovskite-structured Ba0.5Sr0.5Co0.8Fe0.2O3-δ (BSCF) ceramics. The sintering behaviours of BSCF are studied by sintering BSCF powder using a series of sintering temperatures and dwell times. Under all circumstances, only a cubic perovskite structure is identified in as-sintered samples. The relative density of BSCF increases with increasing sintering temperature and dwell time, but shows a more significant increase with increasing temperature. While the grain size increases with increasing sintering temperature and dwell time, it is found that the increasing temperature contributes much more significantly than increasing dwell time in grain growth. The shape of grain size distribution profile is independent of sintering temperature and dwell time, but the profile shifts with different sintering conditions. The grain maintains an aspect ratio of 1.8 irrespective of sintering conditions. Similar findings are also made on the Ni-doped BSCF, but it is found that Ni doping inhibits the grain growth and retards the densification of BSCF while it has little influence on the grain size distributions and grain aspect ratio distributions. The grain growth exponent (n) and apparent activation energy (Q) are also systematically studied. It is found that grain boundary diffusion is the dominant controlling mechanism for BSCF while both grain boundary and lattice diffusions are the equally dominant controlling mechanisms for BSCF-Ni8. The fracture stress of BSCF is measured by both three-point and ring-on-ring bending tests at room and high temperatures. The fracture stress determined by three-point bending tests is consistently higher than that value measured by ring-on-ring tests for a given temperature. By utilising Weibull statistics a close prediction is made of the three-point values from the ring-on-ring values. Compared with the Young’s modulus of BSCF obtained from three-point bending tests between RT and 800 °C, the values determined from ring-on-ring tests shows a fairly good agreement. However, the Young’s modulus measured by both bending tests is lower than that value determined by micro-indentation tests. Hardness and fracture toughness are independent of grain size and grain orientation. Porosity is the dominant factor in Young’s modulus, hardness and fracture toughness of BSCF. The intrinsic hardness, intrinsic Young’s modulus and intrinsic fracture toughness of BSCF are also determined. The subcritical crack growth (SCG) of BSCF is also studied using constant load method at RT and constant stress rate method at 800 °C. It is found that that BSCF is not susceptible to SCG at RT but becomes relatively sensitive to SCG at 800 °C. The results are subsequently used as a basis for a strength–probability–time (SPT) lifetime prediction. Ni doping increases the Young’s modulus, hardness and fracture toughness of BSCF determined micro-indentation tests at RT. Both hardness and Young’s modulus show a non-monotonic trend with Ni doping content, which is attributed to the porosity and secondary phase. The intrinsic hardness, intrinsic Young’s modulus and intrinsic fracture toughness of 8 mol% Ni-doped BSCF are determined. Dopants have little influence on grain orientation and the distribution of grain boundary misorientation angles of BSCF.

Orientador: Guilherme de Siqueira Ferreira Anzaloni Saavedra / Co-orientador: Flávia Pires Rodrigues / Banca: Estevão Tomitsu Kimpara / Banca: Carlos Eduardo Francci / Resumo: O objetivo deste trabalho foi avaliar o efeito do método de sinterização, convencional e por meio de energia micro-ondas, sobre as características microestruturais e propriedades mecânicas de cerâmicas à base de zircônia Y-TZP. A hipótese nula foi que a sinterização realizada por forno de micro-ondas não influencia na resistência à flexão biaxial de discos Y-TZP, tanto dos discos envelhecidos por meio de uma cicladora termomecânica, quanto nos grupos não-ciclados. Cem amostras em forma de discos de cerâmica VIPI Block Zirconn (12 x 1,2 mm) foram usinados de acordo com as normas ISO 6872 para o ensaio de flexão biaxial e foram separados em grupos de acordo com o método de sinterização e de envelhecimento termomecânico: Grupo I: Sinterização convencional e sem ciclagem mecânica; Grupo II: Sinterização convencional + ciclagem termomecânica; Grupo III: Sinterização em micro-ondas e sem ciclagem termomecânica; Grupo IV: Sinterização em micro-ondas + ciclagem termomecânica. Os corpos de prova foram submetidos à flexão biaxial após a sinterização para os grupos não ciclados e após a ciclagem para os grupos os quais foram submetidos ao envelhecimento (1.200.000 ciclos, carga de 45 N e frequência de 2,8 Hz, biaxial, imersos em água 37 °C). Foi realizada análise qualitativa das amostras por meio de um microscópio eletrônico de varredura e difração de raios-X em oito amostras (n = 2) para todos os grupos. Para a análise estatística foi utilizado o módulo Weibull (m), sendo que não houve diferença significativa quando comparado à ciclagem, porém houve quando comparado o método. O mesmo ocorreu quando foi aplicada a análise de variância (α = 5%). Conclui-se que o protocolo de sinterização praticado neste estudo não teve sucesso na sinterização da zircônia odontológica, e o termociclagem não afeta as características microestruturais e mecânicas da Y-TZP / Abstract: The objective of this study was to evaluate the impact of the sintering method, conventional and through microwave energy on the microstructural characteristics and mechanical properties of ceramics based on Y- TZP zirconia. The null hypothesis is that sintering is carried out by microwave oven has no effect on the biaxial flexural strength Y- TZP disc, both discs aged by means of a thermo cycler, and in the non- cycled groups. One hundred samples in the form of VIPI Block Zirconn ceramic discs (12 x 1.2 mm) were machined in accordance with ISO 6872 standards for biaxial bending test and were divided into groups according to the method of sintering and thermomechanical aging: Group I: conventional and without mechanical cycling sintering ; Group II : conventional + thermomechanical cycling sintering ; Group III: microwave sintering and without thermomechanical cycling ; Group IV: in microwave sintering + thermomechanical cycling . The specimens were subjected to biaxial bending after sintering for non-cycled groups and after cycling for groups which were submitted to aging ( 1,200,000 cycles, 45 N load and frequency of 2.8 Hz, biaxial, immersed in water 37 °C). Qualitative analysis was performed on samples using a scanning electron microscope and X-ray diffraction samples in eight samples(n = 2) for all groups. For statistical analysis the Weibull modulus (m) was used, and there was no significant difference when compared to cycling, but there was compared the method. The same happened when the analysis of variance (α = 5%) was applied. It follows that sintering protocol performed in this study had no success in dental zirconia sintering and thermal cycling does not affect the microstructure and mechanical properties of Y- TZP / Mestre

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Submitted by Marcus Nathan Silvestre null (silvestre.nathan@gmail.com) on 2016-08-15T19:33:33Z No. of bitstreams: 1 OBTENÇÃO DA LIGA NITI POR METALURGIA DO PÓ.pdf: 7180947 bytes, checksum: fb85ad122507b1a567ca667e4e2ee8fa (MD5) / Approved for entry into archive by Ana Paula Grisoto (grisotoana@reitoria.unesp.br) on 2016-08-17T13:10:34Z (GMT) No. of bitstreams: 1 silvestre_mn_me_guara.pdf: 7180947 bytes, checksum: fb85ad122507b1a567ca667e4e2ee8fa (MD5) / Made available in DSpace on 2016-08-17T13:10:34Z (GMT). No. of bitstreams: 1 silvestre_mn_me_guara.pdf: 7180947 bytes, checksum: fb85ad122507b1a567ca667e4e2ee8fa (MD5) Previous issue date: 2016-07-29 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / O nitinol (NiTi) é uma das ligas mais empregadas entre aquelas que apresentam o efeito de memória de forma. A produção da liga por metalurgia do pó é uma alternativa às limitações das ligas fundidas, mas apresenta algumas limitações. O objetivo deste trabalho foi obter a liga NiTi via metalurgia do pó, combinando temperatura e tempo de sinterização para produzir uma liga com baixo volume de fases secundárias e óxidos e a martensita como fase principal à temperatura ambiente. Os pós de níquel e titânio foram pesados na proporção 50,5% Ni - 49,5% Ti (% at) e misturados mecanicamente por 2 horas. A mistura foi compactada uniaxialmente sob três tensões consecutivas: 1000, 750 e 500 MPa, relaxando o sistema em cada carga. Em seguida as amostras foram sinterizadas a 930°C, por períodos de 20, 30, 40 ou 50 horas. Após a determinação da melhor rota de sinterização, as amostras foram submetidas à deformação mecânica a quente, utilizando deformações reais de 31% ou 98%. As amostras foram submetidas a alguns tratamentos térmicos: o recozimento foi realizado a temperaturas de 500 °C e 700 °C e a solubilização a 930 °C. A caracterização das amostras foi realizada por microscopia óptica e MEV, difração de raios X, calorimetria exploratória diferencial e ensaio de microdureza. Em relação à rota de sinterização, o melhor resultado foi obtido utilizando-se tempo de sinterização de 50 horas, com a fase martensítica predominante e ausência de pó residual. As fases intermetálicas secundárias observadas foram Ni3Ti e Ni4Ti3. A densidade das amostras sinterizadas não variou significativamente com o tipo de compactação ou tempo de sinterização. A temperatura de transformação de fase martensítica foi satisfatória para o processo. Em relação à conformação mecânica, o valor de densidade aumentou significantemente, como o esperado. Com o recozimento das amostras, a microestrutura não foi alterada, entretanto os intermetálicos se formaram. Os valores de dureza nas amostras são consideravelmente altos para a composição utilizada e estão relacionados à contaminação por oxigênio, à precipitação da fase Ni4Ti3 e à presença de austenita. / Nitinol (NiTi) is one of the most used alloys that exhibit the shape memory effect and powder metallurgy is an alternative to overcome the casting limitations, but some details need to be checked. The aim of this work is to obtain NiTi by powder metallurgy, determining the best combination of sintering time and sintering temperature to produce an alloy with low volume fraction of secondary intermetallic phases and oxides and martensite as the main phase at room temperature. Ni and Ti elemental powders were weighted in order to get the 49.5% Ti – 50.5%Ni (% at) composition and mechanically mixed for 2 hours. The mixed powder was then uniaxially die compacted under the following condition: 1000 MPa, 750 MPa and 500 MPa. After every stress was applied, the system was relaxed. The sintering was performed under an argon atmosphere at 930°C for: 20, 30, 40 and 50 hours. After determining the best sintering route, hot rolling was applied to the samples, using real deformation of 31% and 98%. The samples were submitted to heat treatments: annealing was performed at 500 °C and 700 °C and solubilization was performed at 930 °C. The samples were characterized using optical microscopy, scanning electron microscope, x-ray diffraction and differential scanning calorimetry (DSC). The best route obtained was 50 hours of sintering time, which resulted in the lowest volume of secondary intermetallic phases and no unreacted powder. The intermetallic phases formed were Ni3Ti and Ni4Ti3. The density did not vary with the type of compacting or sintering time. The start temperature of martensite transformation was considered reasonable regarding the process used. After hot rolling, the microstructure did not change significantly. The phases detected after rolling were the same detected previously. About the heat treatments, after the aging the microstructure remained unchanged, but intermetallic phases precipitated. The hardness values obtained were considerably high for the composition used and were attributed to the oxygen contamination, Ni4Ti3 precipitation and the presence of austenite.