Abstract The present work aimed at evaluating the microstructures and mechanical properties of spark plasma sintered WC-6 wt% Co ceramic composites doped with boron (0.2 and 0.5 wt%). W-50 at% C (W-6.13 wt% C) powders produced under different milling times (20, 60, 180, and 600 min) were used as starting materials and subsequently mixed with Co (6 wt%) and B (0.2 or 0.5 wt%) powders for 5 min. The resultant WC-Co-B powder mixtures were consolidated by spark plasma sintering at 1450 °C for 10 min at 40 MPa under vacuum in order to obtain the samples with 10 mm diameter and 3 mm thickness. The starting powders and the sintered samples were characterized by laser diffraction particle size analysis, X-ray diffraction with Rietveld refinement, relative density, scanning electron microscopy, energy dispersive spectrometry, Vickers hardness test, and diametral compression test. Supersaturated W solid solution (WSS) with a crystallite size of <50 nm was formed in W-50C (at%) powder mixtures. The relative density of the sintered composites increased with the increasing milling time up to 180 min from 79.7%±0.6% to 86.7%±0.5% for WC-6Co-0.2B and from 86.7%±0.6% to 90.9%±0.4% for WC-6Co-0.5B. Furthermore, the WC phase appeared as the matrix in the sintered samples, and W2CoB2 precipitated homogeneously around WC grain boundaries, mainly to those containing 0.5% B. The Vickers hardness values of the sintered WC-6Co-0.2B and WC-6Co-0.5B ranged from 1790±39 to 2158±25 HV and 1858±31 to 2182±28 HV, respectively. The fracture strength (determined by diametral compression test) varied between 144-353 MPa due to the porosity and precipitates in thin-thickness cylinder samples.

Abstract The fracture toughness of 3Y-TZP ceramics obtained from a nanocrystalline powder with an optimized microstructure and highly transformable tetragonal grains was investigated. Samples of ZrO2-3 mol% Y2O3 were sintered at temperatures between 1250 and 1400 °C, with isothermal holding times of up to 16 h. Samples sintered at 1250 °C exhibited relative densities ranging between 92% and 98%, which increased with increasing isothermal duration, while samples sintered at 1300, 1350, or 1400 °C achieved densification higher than 98% for all isothermal treatments. Crystallographic analysis indicated the presence of a highly transformable ZrO2-tetragonal phase ( c / a √ 2 = 1 . 0148 - 1 . 0154 ) for all conditions studied. The average grain size ranged from 0.18±0.04 mm (1250 °C-0 h) to 0.64±0.08 mm (1400 °C-16 h), indicating activation energy of 141.3 kJ/mol for grain growth and a growth exponent of 2.8. Both Vickers hardness (1025 to 1300 HV) and fracture toughness (4.0 to 7.8 MPa.m1/2) increased with increasing sintering temperature and time due to increased densification, reduced porosity, and maintenance of potentially high fracture toughness by the t→m phase transformation.

Resumo O objetivo deste estudo foi caracterizar e avaliar as propriedades físicas e mecânicas de uma zircônia experimental para aplicação odontológica e comparar os resultados da resistência à flexão biaxial com a simulação de elementos finitos (MEF). Amostras de zircônia tetragonal estabilizada com ítria (Y-TZP) foram sinterizadas a 1475 °C/2 h e caracterizadas por difração de raios X, microscopia eletrônica de varredura, densidade relativa, resistência à flexão usando teste de pistão em três bolas (P-3B) e módulo de Young. A partir dos resultados de resistência à flexão, foram realizadas simulações numéricas utilizando o software Abaqus. O modelo completo utilizou 70216 elementos. Os resultados apontaram para densificação total em amostras sinterizadas, ZrO2 tetragonal e cúbica como fases cristalinas, tamanho de grão de 0,6±0,2 μm, módulo de Young de 195±4 GPa, resistência à flexão de 1191±9 MPa e módulo de Weibull m=16,3. A simulação numérica indicou uma resistência à flexão próxima de 1100 MPa, com diferença menor que 7% em relação aos resultados experimentais. Os resultados foram comparados associando as propriedades físicas e mecânicas de Y-TZP com seus fenômenos intrínsecos, como a transformação tgm e o domínio ferroelástico.

Abstract The objectives of this study were to characterize and evaluate the physical and mechanical properties of an experimental zirconia for dental application and compare the biaxial flexural strength results with the finite element simulation (FEM). Yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic samples were sintered at 1475 °C/2 h and characterized by X-ray diffraction, scanning electron microscopy, relative density, flexural strength using piston-on-three balls (P-3B) test and Young’s modulus. From the flexural strength results, numerical simulations were performed using Abaqus software. The complete model used 70216 elements, considering the components of the test. The results indicated full densification of sintered samples, ZrO2-tetragonal and ZrO2-cubic as crystalline phases, and average grain size of 0.6±0.2 μm. Mechanical characterization of sintered samples indicated Young’s modulus of 195±4 GPa, flexural strength of 1191±9 MPa and Weibull modulus m=16.3. FEM simulation indicated a flexural strength close to 1100 MPa, with a difference lower than 7% in relation to the experimental results. The results were compared associating the physical and mechanical properties of Y-TZP with its intrinsic phenomena such as tgm transformation and ferroelastic domain.

Resumo Quatro porcelanas dentárias para cobertura de zircônia foram sinterizadas (queimadas) a 910-960 °C e caracterizadas, focando na análise de confiabilidade, propriedades físicas e mecânicas. Amostras com densidade relativa próxima de 99% apresentaram cristalização de leucita, além de fase amorfa residual. Dureza entre 491±23 e 575±32 HV foi diferente entre todas as cerâmicas. Tenacidade à fratura entre 1,13±0,11 e 1,42±0,25 MPa.m1/2 foi estatisticamente diferente. Os resultados de resistência à flexão não foram diferentes para as porcelanas (73±9 a 75±12 MPa), com a exceção de um grupo específico (62±4 MPa). A análise de Weibull indicou resistência à flexão entre 73 e 75 MPa, módulo de Weibull (m) entre 5,7 e 7,1, enquanto a cerâmica com resistência de 60 MPa apresentou m=13,6. O uso de teoria clássica da mecânica da fratura, associado aos resultados das propriedades obtidas neste trabalho, indicou tamanho crítico do defeito nestas cerâmicas entre 65 e 90 μm e a energia de fratura teórica das porcelanas foi de 10,5 a 16,3 J/m. Concluiu-se que as porcelanas têm diferentes comportamentos e parece não haver clara relação entre as propriedades estudadas.

Abstract Four dental porcelains for covering zirconia were sintered (fired) at 910-960 °C and characterized, focusing in analyzing reliability, physical and mechanical properties. Samples with relative density close to 99% presented leucite crystallization apart from residual amorphous phase. Hardness between 491±23 and 575±32 HV was different among all ceramics. Fracture toughness between 1.13±0.11 and 1.42±0.25 MPa.m1/2 was statistically different. Bending strength results were not different for three porcelain groups (73±9 to 75±12 MPa), with the exception of one specific group (62±4 MPa). Weibull analysis indicated bending strength between 73 and 75 MPa, Weibull modulus (m) between 5.7 and 7.1, while the ceramic with strength of 60 MPa presented m=13.6. The use of classical theory of fracture mechanics associated to the results of properties obtained in this work indicated the critical failure size in these ceramics lays between 65 and 90 μm and the theoretical fracture energy of porcelains is approximately from 10.5 to 16.3 J/m. It was concluded that the porcelains had different behavior, and it seems that there is no clear relationship among the studied properties.

Este trabalho foi proposto com objetivo de analisar a possibilidade da substituição de Y2O3 por CeO2 sinterização via fase líquida de nitreto de silício (Si3N4), visando obter um material com boas propriedades físicas, mecânicas e microestruturais, além da redução de custos de produção desta cerâmica. Para o desenvolvimento deste trabalho foram preparadas duas misturas de pós, variando-se as proporções entre alfa-Si3N4, Al2O3, AlN, Y2O3 e CeO2. As misturas de pós foram homogeneizadas em etanol, secas em evaporador rotativo e estufa, respectivamente. Em seguida, prensadas uniaxialmente (100 MPa) e isostaticamente a frio(300 MPa). As amostras foram sinterizadas à 1850 ºC durante 1 h, em forno com elemento resistivo de grafite sob atmosfera de nitrogênio. Após sinterização, as amostras apresentaram densidades relativas superiores a 97% do valor teórico. A tenacidade à fratura e a dureza foram superiores a 5,28 MPa.m½ e 17,12 GPa, respectivamente. As análises de fases por difração de raios X e microscopia eletrônica de varredura mostraram a presença das fases alfa-SiAlON e beta-Si3N4.

This work investigated the substitution of Y2O3 for CeO2 in liquid-phase sintered silicon nitride ceramics. Cost reduction as well as good physical, mechanical and microstructural properties are the main objectives of the present study. Two powder mixtures were prepared, varying the contents of alpha-Si3N4, Al2O3, AlN, Y2O3 and CeO2. The mixtures were homogenized in ethanol, dried in a rotating evaporator and kiln, respectively, and then uniaxially (100 MPa) and cold isostatically pressed (300 MPa). The samples were sintered at 1850ºC for 1 h in a graphite resistive furnace under nitrogen atmosphere. After sintering the density of the samples was higher than 97% of the theoretical value. The fracture toughness and hardness were higher than 5.28 MPa.m½ and 17.12 GPa, respectively. Phase analysis by X-ray diffraction and scanning electron microscopy revealed the presence of alpha-SiAlON and beta-Si3N4.

Nitreto de silício (Si3N4) é um material cerâmico covalente de elevada resistência à corrosão e estabilidade mecânica em temperaturas elevadas. Devido a essas propriedades, sua utilização em processos metalúrgicos, tais como em fundição de ligas metálicas, é crescente. Desta forma, a caracterização da interface entre Si3N4 e metais fundidos é de grande interesse para investigar possíveis interações as quais poderão deteriorar o material cerâmico e/ou contaminar o metal. Nesse trabalho o uso de Si3N4 como material base de cadinhos para fundição de alumínio foi estudado, pela investigação do ataque corrosivo de Al líquido a 1150 ºC durante 30 dias, ao ar. A interface foi caracterizada por difração de raios X, microscopia eletrônica de varredura e espectroscopia de energia dispersiva. É encontrado que devido à oxidação superficial dois óxidos se formam - SiO2 no Si3N4 e Al2O3 no Al - os quais evitam possíveis reações sob as condições estudadas, conferindo alta resistência à corrosão aos cadinhos de Si3N4.

Silicon nitride is a covalent ceramic material of high corrosion resistance and mechanical stability at elevated temperatures. Due to these properties, its use in metallurgical processes, such as the casting of alloys, is increasing. Therefore, the characterization of the interface between Si3N4 and the casted metal is of great importance to investigate possible interactions, which might deteriorate the ceramic mould or contaminate the metal. In this work, the use of Si3N4 as crucible material for Al-casting has been studied, by investigating the corrosion attack of liquid Al at a temperature of 1150 ºC during 30 days in air. The interface was characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy. It has been found that due to superficial oxidation two oxide layers form - SiO2 on Si3N4 and Al2O3 on Al - which effectively hinder further reactions under the conditions studied, confering high corrosion resistance to the Si3N4 crucible.