Zirconia-based cast refractories are widely used for glass furnace applications. Since they have to withstand harsh chemical as well as thermo-mechanical environments, internal stresses and microcracking are often present in such materials under operating conditions (sometimes in excess of 1700 °C). We studied the evolution of thermal (CTE) and mechanical (Young’s modulus) properties as a function of temperature in a fused-cast refractory containing 94 wt.% of monoclinic ZrO2 and 6 wt.% of a silicate glassy phase. With the aid of X-ray refraction techniques (yielding the internal specific surface in materials), we also monitored the evolution of microcracking as a function of thermal cycles (crossing the martensitic phase transformation around 1000 °C) under externally applied stress. We found that external compressive stress leads to a strong decrease of the internal surface per unit volume, but a tensile load has a similar (though not so strong) effect. In agreement with existing literature on β-eucryptite microcracked ceramics, we could explain these phenomena by microcrack closure in the load direction in the compression case, and by microcrack propagation (rather than microcrack nucleation) under tensile conditions.
18 April 2018 in Journal of the American Ceramic Society
Spark Plasma Sintering (SPS) has become a conventional and promising sintering method for powder consolidation. This study aims to well understand the mechanisms of densification encountered during SPS treatments, especially in the early stages of sintering. The direct current (DC) electrical behavior of copper granular medium is characterized. Their properties are correlated with their microstructural evolutions through post-mortem scanning electron microscope (SEM) observations to allow a thorough understanding of the involved Branly effect that is suspected to occur in SPS. The electrical response is studied by modifying the initial thickness of the oxide layer on particles surfaces and applying various mechanical loads on the granular medium. Without load and at low current, the measured quasi-reversible behavior is connected to the formation of spots at the microcontacts between the particles. By increasing the current, the Branly transition from an insulating to a conductive state suddenly occurs. The insulating oxide layer is destroyed, and micro-bridges are created. The application of a mechanical pressure strongly modifies the DC Branly effect. Increasing low stress leads to a strong decrease in the breakdown field. For high-applied pressure, successive drops in the electric field are detected during the electrical transition. These successive drops are induced by microcracking of the insulating oxide layer.