RESUMO
8 mol% Y2O3-stabilized ZrO2 (8YSZ) ceramics were prepared with KCl and LiF additions to obtain porous specimens with high skeletal density. Thermogravimetric and differential thermal analyses (TG/DTA) were carried out on 8YSZ and on 8YSZ mixed to 5 wt.% KCl or 5 wt.% LiF as sacrificial pore formers that were thermally removed during sintering. The melting and evaporation of the alkali halides were evaluated by differential thermal analysis. Dilatometric analysis was also carried out following the same TG/DTA temperature profile with results suggesting rearrangement of the 8YSZ particles during LiF and KCl melting. The dilatometric data of 8YSZ green pellets mixed to KCl or LiF exhibited an initial expansion up to the melting of the alkali halide, followed by shrinkage due to sintering evolution with grain growth and pore elimination. The time that the alkali halide molten phase was kept during sintering was found to be an important parameter for obtaining 8YSZ-sintered specimens with specific pore content; bulk density and open porosity could then be tuned by controlling the time the alkali halide remained liquid during sintering. Scanning electron microscopy images of the pellet fracture surfaces showed pores that contributed to increasing the electrical resistivity as evaluated by impedance spectroscopy analysis.
RESUMO
Understanding the physics behind changes in dielectric permittivity and mechanical response with temperature and frequency in lead-free ferroic materials is a fundamental key to achieve optimal properties and to guarantee good performance in the technological applications envisaged. In this work, dense [Formula: see text] (BNT) electroceramics were prepared through solid-state reaction of high-grade oxide reagents, followed by sintering at high temperature (1393 K for 3 h). In good agreement with previous reports in the literature, the thermal behaviour of dielectric response from these BNT materials showed the occurrence of a high-temperature diffuse-like permittivity peak, whose origin has been so far controversial. Thermally stimulated depolarization current, impedance and mechanical spectroscopies measurements were here conducted, over a wide range of temperature and frequency, to get a deep insight into the mechanism behind of this event. The approach included considering both as-sintered and reduced BNT samples, from which it is demonstrated that the broad high-temperature dielectric peak originates from interfacial polarization involving oxygen vacancies-related space-charge effects that develop at the grain-to-grain contacts. This mechanism, that contributes to the anomalous behavior observed in the mechanical response at low frequencies, could also be responsible for the presence of ferroelastic domains up to high temperatures.
