Tetragonal to monoclinic transformation and microstructural evolution in ZrO2–9.7 mol% MgO during cyclic heating and cooling

The tetragonal (t) to monoclinic (m) transformation behaviour and its relationship to microstructural evolution were investigated by means of dilatometry and transmission electron microscopy for ZrO2–9.7 mol% MgO during cyclic heating and cooling between room temperature and 1490 K. In the as-sintered specimens, fine oblate ellipsoidal t-phase precipitates, 20–50 nm in diameter and 100–200 nm long, were distributed in the cubic (c)-phase matrix. They were below a critical size for transformation and exhibited no transformation in the first three cycles. In the fourth and further cycles, transformation occurred in two distinct stages. A low-temperature stage appeared at 850–1000 K on heating and at 400–700 K on cooling, while a high-temperature stage appeared at 1350–1400 K on heating and at 1000–1200 K on cooling. With the increasing number of cycles, at first the size of low-temperature stages increased and then decreased above ten cycles accompanying the development of the high-temperature stage. During cyclic heating and cooling, coarsening of ellipsoidal precipitates and decomposition of c- and t-phases occurred. As a result of the decomposition, MgO particles and a new m-phase containing a very low concentration of MgO were produced. The coarsened ellipsoidal t-phase precipitates were responsible for the low-temperature stage. The new m- or t-phase containing very low MgO produced by the decomposition was responsible for the high-temperature stage.