The effect of low temperature aging on the mechanical property & phase stability of Y-TZP ceramics

Abstract

Statement of problem: Recently Yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) has been introduced due to superior flexural strength and fracture toughness compared to other dental ceramic systems. Although zirconia has outstanding mechanical properties, the phenomenon of decrease in the life-time of zirconia resulted from degradation in flexural strength after low temperature aging has been reported.

Purpose: The objective of this study was to investigate degradation of flexural strength of Y-TZP ceramics after various low temperature aging treatments and to evaluate the phase stability and micro-structural change after aging by using X-ray diffraction analysis and a scanning electron microscope (SEM).

Material and methods: Y-TZP blocks of Vita In-Ceram YZ (Vita Zahnfabrik, Bad Säckingen, Germany) were prepared in 40 mm (length) × 4 mm (width) × 3 mm (height) samples. Specimens were artificially aged in distilled water by heat-treatment at a temperature of 75, 100, 125, 150, 175, 200, and 225℃ for 10 hours, in order to induce the phase transformation at the surface. To measure the mechanical property, the specimens were subjected to a four-point bending test using a universal testing machine (Instron model 3365; Instron, Canton, Mass, USA). In addition, X-ray diffraction analysis (DMAX 2500; Rigaku, Tokyo, Japan) and SEM (Hitachi s4700; Jeol Ltd, Tokyo, Japan) were performed to estimate the phase transformation. The statistical analysis was done using SAS 9.1.3 (SAS institute, USA). The flexural strength data of the experimental groups were analyzed by one-way analysis of variance and to detect statistically significant differences (α= .05).

Results: The mean flexural strength of sintered Vita In-Ceram YZ without autoclaving was 798 MPa. When applied aging temperature at below 125℃ for 10 hours, the flexural strength of Vita In-Ceram YZ increased up to 1,161 MPa. However, at above 150℃, the flexural strength started to decrease. Although low temperature aging caused the tetragonal-to-monoclinic phase transformation related to temperature, the minimum flexural strength was above 700 MPa.

Conclusion: The monoclinic phase started to appear after aging treatment above 100℃. With the higher aging temperature, the fraction of monoclinic phase increased. The ratio of monoclinic/tetragonal + monoclinic phase reached a plateau value, circa 75% above 175℃. The point of monoclinic concentration at which the flexural strength begins to decrease was between 12% and 54%.

Keywords: Low temperature aging; Mechanical property; Phase transformation; Y-TZP ceramic.

Fig. 1

The images taken by scanning electron microscope. (A) Vita In-Ceram YZ without autoclave aging, original magnification × 30.0 k (B) Vita In-Ceram YZ with autoclave aging at 150℃ for 10 hours, original magnification × 30.0 k (C) Vita In-Ceram YZ with autoclave aging at 225℃ for 10 hours, original magnification × 30.0 k

Fig. 2

X-ray diffraction pattern of Vita In-Ceram YZ after aging process at different temperatures.

Fig. 3

Graph of the flexural strength and monoclinic phase concentration of Vita In-Ceram YZ.