Preparation and thermal evolution of sol-gel derived transparent ZrO₂ and MgO-ZrO₂ gel monolith

Abstract

Transparent gel monoliths of pure and MgO-doped zirconia having dopant concentrations in the range 0 to 15 mol % were prepared by chemical polymerization of zirconium n-propoxide and magnesium acetate tetrahydrate using 2-methoxy ethanol as solvent. The thermal evolution of amorphous gels was studied by differential thermal analysis, X-ray diffraction and transmission electron microscopy. The crystallization of pure and doped zirconia gels occurred in the temperature range 360 to 450° C. The first crystalline phase to appear is tetragonal for pure and 2 mol % doped zirconia, and cubic for 3 to 15 mol % doped samples. Both crystallization and decomposition temperatures are found to increase with increasing dopant concentration, approaching a saturation value for 10 mol % doped samples. It has been established that the transformation of the cubic to the monoclinic phase takes place via a metastable tetragonal phase. A linear relationship between the lattice parameter of cubic zirconia and MgO concentration has been established. X-ray diffraction studies have also revealed that the entire amount of MgO used in preparing doped zirconia gels remains in a single MgO-ZrO₂ crystalline phase formed initially by thermal treatment.[/p]