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Calcium cobaltite (Ca3Co4O9) is considered as one of the most promising thermoelectric p-type oxides for energy harvesting applications at temperatures above 500 °C. It is challenging to sinter this material as its stability is limited to 920 °C. To facilitate a practicable and scalable production of Ca3Co4O9 for multilayer generators, a systematic study of the influence of powder calcination, Bi doping, reaction sintering, and pressure-assisted sintering (PAS) on microstructure and thermoelectric properties is presented. Batches of doped, undoped, calcined, and not calcined powders were prepared, tape-cast, and sintered with and without uniaxial pressure at 900 °C. The resulting phase compositions, microstructures, and thermoelectric properties were analyzed. It is shown that the beneficial effect of Bi doping observed on pressureless sintered samples cannot be transferred to PAS. Liquid phase formation induces distortions and abnormal grain growth. Although the Seebeck coefficient is increased to 139 μV/K by Bi doping, the power factor is low due to poor electrical conductivity. The best results were achieved by PAS of calcined powder. The dense and textured microstructure exhibits a high power factor of 326 μW/m K2 at 800 °C but adversely high thermal conductivity in the relevant direction. The figure of merit is higher than 0.08 at 700 °C.
This study combines three different approaches to lower the sintering temperature of Sm-doped CaMnO3 to save energy in production and facilitate co-firing with other low-firing oxides or metallization. The surface energy of the powder was increased by fine milling, sintering kinetics were enhanced by additives, and uniaxial pressure during sintering was applied. The shrinkage, density, microstructure, and thermoelectric properties were evaluated. Compared to micro-sized powder, the use of finely ground powder allows us to lower the sintering temperature by 150 K without reduction of the power factor. By screening the effect of various common additives on linear shrinkage of CaMnO3 after sintering at 1100°C for 2 h, CuO is identified as the most effective additive. Densification at sintering temperatures below 1000°C can be significantly increased by pressure-assisted sintering. The power factor at room temperature of CaMnO3 nano-powder sintered at 1250°C was 445 μW/(m K2). Sintering at 1100°C reduced the power factor to 130 μW/(m K2) for CaMnO3 nano-powder, while addition of 4 wt. % CuO to the same powder led to ∼290 μW/(m K2). The combination of fine milling, CuO addition, and pressure-assisted sintering at 950°C resulted in a power factor of ∼130 μW/(m K2). These results show that nano-sized powder and CuO addition are successful and recommendable strategies to produce CaMnO3 with competitive properties at significantly reduced temperatures and dwell times.
Dielectric strength testing of ceramics can be performed with various setups and parameters. Comparisons of results from different sources are often not meaningful, because the results are strongly dependent on the actual testing procedure. The aim of this study is to quantify the influence of voltage ramp rate, electrode size, electrode conditioning, and sample thickness on the measured AC dielectric strength of a commercial alumina. Mean values, Weibull moduli, and failure probabilities determined in standardized short time tests are evaluated and related to withstand voltage tests. Dielectric strength values in the range from 21.6 to 33.2 kV•mm -1 were obtained for the same material using different testing procedures. Short time tests resulted in small standard deviations (< 2 kV•mm -1 ) and high Weibull moduli around 30, while withstand tests at voltage levels with low and virtual zero failure probability in short time tests resulted in large scatter of withstand time and Weibull moduli < 1. The strong decrease in Weibull moduli is attributed to progressive damage from partial discharge and depolarization during AC testing. These findings emphasize the necessity of a thorough documentation of testing procedure and highlight the importance of withstand voltage tests for a comprehensive material characterization.
<p>The relationship between fracture toughness and Yttria content in modern zirconia ceramics was revised. For that purpose, we evaluated here 10 modern Y<sub>2</sub>O<sub>3</sub>-stabilized zirconia (YSZ) materials currently used in biomedical applications, namely prosthetic and implant dentistry. The most relevant range between 2-5 mol% Y<sub>2</sub>O<sub>3</sub> was addressed by selecting from conventional opaque 3 mol% YSZ up to more translucent compositions (4-5 mol% YSZs). A technical 2YSZ was used to extend the range of our evaluation. The bulk mol% Y<sub>2</sub>O<sub>3</sub> concentration was measured by X-Ray Fluorescence Spectroscopy. Phase quantification by Rietveld refinement are supplied by considering only two tetragonal phases or an additional improbable cubic phase. A first-account of the fracture toughness (<i>K</i><sub>Ic</sub>) of the partly-sintered materials is given, which amounted to 0.4 – 0.7 MPaÖm. In the fully-densified state, an inverse power-law behavior was obtained between <i>K</i><sub>Ic</sub> and bulk mol% Y<sub>2</sub>O<sub>3</sub> content, whether using only our measurements or including literature data, challenging some established relationships.</p>
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