Effect of hydrothermal aging on the properties of zirconia with different levels of translucency.

OBJECTIVES: The aim of this study was to evaluate the effect of hydrothermal aging on the mechanical properties and translucency of dental zirconia with different levels of translucency. METHODS: Three different types of dental yttria-stabilized zirconia were used: 3Y-TZP (ZrO2 - 3 mol.% Y2O3) of medium opacity (designated Z3OP), 3Y-TZP of medium translucency (Z3MT), and 5Y-PSZ (ZrO2 - 5 mol.% Y2O3) of high translucency (Z5HT). A total of 120 specimens were sintered (n = 40 specimens/group). The control group (sintered→polished→heat-treated) and the aged group (sintered→polished→heat-treated→hydrothermally degraded at 134 °C, 2 bar, 5h) were characterized by relative density, quantitative phase analysis by X-ray diffraction using the Rietveld method, microstructural analysis by scanning electron microscopy, surface roughness and translucency. All groups were submitted to a biaxial flexural strength test. Data analysis using Kruskal-Wallis, Nemenyi (p-value = 0.05), and Weibull statistics were used. RESULTS: All sintered specimens presented full densification. After aging, an increase of the m-ZrO2 phase content was observed for the Z3OP group. On the other hand, Z3MT and Z5HT did not show any m-ZrO2 phase, indicating resistance to the hydrothermal degradation. Smaller grains were observed in the Z3MT group in relation to Z3OP group and the Z5HT group presented a bimodal grain distribution, where the largest grains were associated to cubic ZrO2. Z3OP exhibited a slight increase in roughness as a function of degradation, while the roughness remained statistically stable in the other groups. Translucency was little influenced by degradation, but considerably affected by increasing thickness. The Z5HT samples were the group with the highest translucency among the control groups. Z3OP exhibited the highest flexural strength, while being the most susceptible to hydrothermal degradation. The lowest values were presented by Z5HT in all groups, due to the high concentration of c-ZrO2 grains. CONCLUSION: Hydrothermal aging is less critical to the flexural strength of zirconia-based materials than the materials' composition and microstructure. Z5HT zirconia showed the highest translucency, however the measured difference is not visually perceptible. Z5HT was considered the most resistant to hydrothermal degradation.

Preparation of TiC/Ti3SiC2 Composite by Sintering Mechanical Alloyed Ti-Si-C Powder Mixtures.

The present work aims to evaluate the crystalline phases and microstructure of a TiC-Ti3SiC2 ceramic composite, obtained by mechanical alloying of Ti, C and Si powders and subsequent sintering. A mechanical alloying technique in a planetary ball mill for 1, 10, 50, 100 and 200 h using Ti, Si and C powders with molar ratios of 3:1:2 as feedstock in argon (Ar) gas was employed to prepare nano-sized Ti-Si-C powders. TiC crystallite size and lattice strain were evaluated by X-ray diffraction analysis (XRD) and the morphological characteristics and particle size distribution were examined using scanning electron microscope (SEM). After milling, a reduction of the average particle size and crystallinity is observed. Furthermore, after 10 h of milling time, TiC starts to crystallize. The powder mixture obtained after 200 h of milling was compacted and sintered at 1200 °C under controlled atmosphere, for 15 min, 2 h or 4 h with a heating rate of 5 °C/min. Almost full densification of samples sintered for 2 h and 4 h has been achieved, with relative densities close to 98.8±0.2% and TiC and Ti3SiC2 as crystalline phases with an average crystallite size of TiC near 0.7 µm. Rietveld refinement indicates that the majority TiC-cubic phase (>85 vol%) presents a unit cell volume of 8.03 nm³ after sintering at 1200 °C. Despite the maintenance of the volume of the hexagonal unit cell of Ti3SiC2, (15.05 nm³), the increase of the isothermal sintering time resulted in an increase of the lattice parameter "a", from 0.315 nm to 0.320 nm, and a reduction of the lattice parameter "c" from 1.750 nm to 1.705 nm. The control of the changes in the residual stresses within the TiC matrix and the Ti3SiC2 precipitates, which is associated with the deformation in the lattice parameters, must be controlled to achieve high fracture toughness in the composite.