AEM investigation of ZrO2 solid solution formation in ZrO2/mullite composites

Zirconia (ZrO2) is often added to ceramic compacts to increase their toughness. The mechanisms by which this toughness increase occurs are generally accepted to be those of transformation toughening and microcracking. The mechanism of transformation toughening is based on the presence of metastable tetragonal ZrO2 which transforms to the monoclinic allotrope when stressed by a propagating crack. The decrease in volume which accompanies this transformation effectively relieves the applied stress at the crack tip and toughens the material; microcrack toughening arises from the deflection of a propagating crack around sharply angular inclusions.These mechanisms, however, do not explain the toughness increases associated with the class of composites investigated here. Analytical electron microscopy (AEM) has been used to determine whether solid solution effects could be the cause of this increased toughness. Specimens of a mullite (3Al2O3·2SiO2) + 15 vol. % ZrO2 were prepared by the usual technique of mechanical thinning followed by ion beam milling. All observations were made in a Philips EM400 TEM/STEM microscope fitted with EDXS and EELS spectrometers.