The kinetics of the tetragonal to monoclinic (t–m) transformation of zirconia in a hydrous environment at 134°C and 3 bar pressure was studied. As surface X-ray diffraction, which is conventionally used to explore the progress, has a very limited depth of information, it distorts the quantitative results in a layer-on-layer situation and by itself is ill suited for this reason. Analyzing cross sections is more suitable; therefore, focused ion beam techniques were used to prepare artifact-free cuts. The material was subsequently investigated by scanning electron microscopy, electron backscatter diffraction and Raman spectroscopy. Only the combination of methods makes it possible to resolve the quantifiable details of the process. The transformation starts in the near-surface areas, forms a layer, and the growth of this layer proceeds into the bulk material following a simple linear time law (0.0624 μm h−1 for material in the chosen condition), without apparent retardation or limit. The progress yields a gradientless layer with a fixed amount of residual tetragonal zirconia (∼27% for 3Y-TZP in the present conditions) separated from unaffected material by a boundary, which has a roughness only in the grain size range. The kinetics indicates a reaction rate control, where the hydration reaction is the key factor, but is modified by the stepwise access of water to the reaction front opened by the autocatalytic transformation of zirconia with a critical hydration level.
This paper was originally published in Acta Biomaterialia (2013) 9, 4826-4835.
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