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Raman Spectroscopy Evaluation of Subsurface Hydrothermal Degradation of Zirconia
Author(s) -
Wulfman Claudine,
Djaker Nadia,
Dupont Nathalie,
Ruse Dorin,
Sadoun Michaël,
la Chapelle Marc Lamy
Publication year - 2012
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/j.1551-2916.2012.05237.x
Subject(s) - raman spectroscopy , materials science , cubic zirconia , monoclinic crystal system , analytical chemistry (journal) , tetragonal crystal system , mineralogy , hydrothermal circulation , dental ceramics , autoclave , phase (matter) , ceramic , composite material , optics , chemistry , crystal structure , crystallography , metallurgy , geology , chromatography , physics , organic chemistry , seismology
The aims of this study were to calibrate the collection depth for RMS and, using the calibration, to evaluate the in‐depth phase transformation induced in a dental 3 Y ‐ TZP ceramic by hydrothermal aging, simulating LTD . Objectives 10x and 80x affording spatial resolutions of ~3 and ~1 μm, respectively, were used. Probe size was controlled by the confocal pinhole aperture. The collection depth of each probe (objective – pinhole combination) was calibrated on a wedge‐shaped pure tetragonal zirconia specimen. Pure tetragonal samples of a dental 3 Y ‐ TZP were aged in vitro in an autoclave, in Ringer solution, at 130°C, under 0.6 MPa, for 10, 15, 20, 25, and 90 h. Two specimens were used for each time interval and two unexposed specimens served as controls. Monoclinic volume fraction ( V fm ) was determined by X‐ray diffraction and by in‐depth probing with RCMS . Probes based on 10x objective penetrated up to 68 μm, whereas those based on the 80x were limited to 5 μm. Aging induced significant increase in V fm , ranging from 30% after 10 h to 80% after 90 h. After 90 h aging, the 80% V fm extended to at least 20 μm from the surface. A maximum V fm was identified at 2.5 μm subsurface depth in 10, 15, and 20 h aged specimens.