Al-contaminated Ta-substituted Li7La3Zr2O12 (LLZ:Ta), synthesized via solid-state reaction, and Al-free Ta-substituted Li7La3Zr2O12, fabricated by hot-press sintering (HP-LLZ:Ta), have relative densities of 92.7% and 99.0%, respectively. Impedance spectra show the total conductivity of LLZ:Ta to be 0.71 mS cm(-1) at 30 °C and that of HP-LLZ:Ta to be 1.18 mS cm(-1). The lower total conductivity for LLZ:Ta than HP-LLZ:Ta was attributed to the higher grain boundary resistance and lower relative density of LLZ:Ta, as confirmed by their microstructures. Constant direct current measurements of HP-LLZ:Ta with a current density of 0.5 mA cm(-2) suggest that the short circuit formation was neither due to the low relative density of the samples nor the reduction of Li-Al glassy phase at grain boundaries. TEM, EELS, and MAS NMR were used to prove that the short circuit was from Li dendrite formation inside HP-LLZ:Ta, which took place along the grain boundaries. The Li dendrite formation was found to be mostly due to the inhomogeneous contact between LLZ solid electrolyte and Li electrodes. By flatting the surface of the LLZ:Ta pellets and using thin layers of Au buffer to improve the contact between LLZ:Ta and Li electrodes, the interface resistance could be dramatically reduced, which results in short-circuit-free cells when running a current density of 0.5 mA cm(-2) through the pellets. Temperature-dependent stepped current density galvanostatic cyclings were also carried out to determine the critical current densities for the short circuit formation. The short circuit that still occurred at higher current density is due to the inhomogeneous dissolution and deposition of metallic Li at the interfaces of Li electrodes and LLZ solid electrolyte when cycling the cell at large current densities.
The sintering behavior of nanocrystalline ZnO was investigated at only 250 °C. Densification was achieved by the combined effect of uniaxial pressure and the addition of water both in a Field Assisted Sintering Technology/Spark Plasma Sintering apparatus and a warm hand press with a heater holder. The final pure ZnO materials present high densities (> 90 % theoretical density) with nano-grain sizes. By measuring the shrinkage rate as a function of applied stress it was possible to identify the stress exponent related to the densification process. A value larger than one points to non-linear relationship going beyond single solid-state diffusion or liquid phase sintering. Only a low amount of water (1.7 wt.%) was needed since the process is dictated by the adsorption on the surface of the ZnO particles. Part of the adsorbed water dissociates into H + and OH -ions, which diffuse into the ZnO crystal structure, generating grain boundaries/interfaces with high defect chemistry. As characterized by Kelvin Probe Force Microscopy, and supported by impedance spectroscopy, this highly defective grain boundary area presents much higher surface energy than the bulk. This highly defective grain boundary area with high potential reduces the activation energy of the atomic diffusion, leading to sinter the compound at low temperature.
Also several groups applied a similar approach to increase the open porosity of lters.10-13 Recently, this technology The production of highly porous titanium parts of has been used for biomedical applications,14 but until now complex shape by powder metallurgical technology is the technique was restricted to the production of parts with described. Well de ned porosity and pore sizes were simple geometry such as cylinders or bars. In contrast to achieved using a pore forming additive. This additive this, many titanium parts, for example surgical implants, also enhances the strength of unsintered compacts, have a high complexity in the shape. allowing machining in the green state. The require-The present work focuses on the development of a ments of the initial powders and pecularities of each suitable manufacturing route for net shape parts made of production step are discussed in detail. The microhighly porous titanium, while the mechanical properties structure of porous materials and examples of net and deformation behaviour of this material have already shape parts are given, aiming preferentially at biobeen published elsewhere.8,9 Considering that the quantity medical applications. The impurities of the obtained of implants with speci ed size is usually small, the applititanium parts are compared with the requirements of cation of special dies and automated equipment becomes the ISO standard for titanium implants.
Detailed insight into electrochemical reaction mechanisms and rate limiting steps is crucial for targeted optimization of solid oxide fuel cell (SOFC) electrodes, especially for new materials and processing techniques, such as Ni/Gd-doped ceria (GDC) cermet anodes in metal-supported cells. Here, we present a comprehensive model that describes the impedance of porous cermet electrodes according to a transmission line circuit. We exemplify the validity of the model on electrolyte-supported symmetrical model cells with two equal Ni/Ce0.9Gd0.1O1.95-δ anodes. These anodes exhibit a remarkably low polarization resistance of less than 0.1 Ωcm2 at 750 °C and OCV, and metal-supported cells with equally prepared anodes achieve excellent power density of >2 W/cm2 at 700 °C. With the transmission line impedance model, it is possible to separate and quantify the individual contributions to the polarization resistance, such as oxygen ion transport across the YSZ-GDC interface, ionic conductivity within the porous anode, oxygen exchange at the GDC surface and gas phase diffusion. Furthermore, we show that the fitted parameters consistently scale with variation of electrode geometry, temperature and atmosphere. Since the fitted parameters are representative for materials properties, we can also relate our results to model studies on the ion conductivity, oxygen stoichiometry and surface catalytic properties of Gd-doped ceria and obtain very good quantitative agreement. With this detailed insight into reaction mechanisms, we can explain the excellent performance of the anode as a combination of materials properties of GDC and the unusual microstructure that is a consequence of the reductive sintering procedure, which is required for anodes in metal-supported cells.
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