Quantitative analysis of monoclinic phase in 3Y-TZP by Raman spectroscopy

Abstract

Standard mixtures of tetragonal and monoclinic zirconia powders have been carefully prepared in order to cover the complete weight range from 0% to 100% of monoclinic phase, and they have been analyzed by X-ray diffraction and Raman spectroscopy. Several equations given in the literature for determining the composition of monoclinic and tetragonal mixtures from Raman spectra have been used and the results compared with the actual compositions. The calibration constant for the ratio between the intensities of the monoclinic peaks at 181–190 cm−1 and the tetragonal peak at 147 cm−1 was estimated to be 2.07, while for the ratio between the intensities of the same monoclinic peaks and the sum of tetragonal peaks at 147 and 265 cm−1 was found to be 0.3. The first value is very close to that reported before in the literature, but the latter is significantly different from that most used in the literature for surface characterization of low-temperature degradation of 3Y-TZP in femoral heads and dental ceramics. The results are discussed in terms of the homogeneity of composition standards used for calibration Raman spectra.