3Y‐TZP In‐Depth Phase Transformation by Raman Spectroscopy: A Comparison of Three Methods

Zirconia phase transformation is usually studied on surface. For in‐depth study, three methods were proposed using Raman microspectroscopy quantitative evaluation: direct measurement on sample cross section, confocal Raman spectroscopy (CRS), and progressive pinhole aperture enlargement (PPAE). The aim of this study was to compare transformation profiles obtained with these three methods on the same sample. Three 3Y‐TZP samples were aged, respectively, for 25, 72, and 90 h in artificial saliva. Transformation profiles were determined with cross‐sectional measurement, CRS and PPAE. A transformation profile simulation model based on PPAE measurements is proposed, using the convolution of the excitation intensity profile and the Beer–Lambert law (optical properties of zirconia). The simulation model was validated with the determination of 3Y‐TZP transformation factor, T = 1.15 μm^?1, identical for the three aging durations. Both cross section and PPAE measured similar in‐depth transformation decrease, but with a 10 μm‐shift: transformed zirconia layer is more important in cross‐sectional protocol (36 μm with PPAE and 46 μm with cross‐sectional after 90 h aging). Complementary measurements on a 10 h aged sample, where transformation is initiated by Low‐Temperature Degradation, showed that sample preparation and polishing, necessary in the cross‐sectional method, were responsible for the higher transformation. PPAE method enables noninvasive in‐depth measurements with limited optical and mechanical biases.