Nanoscale physico-mechanical properties of an aging resistant ZTA composite.

OBJECTIVE: To characterize the effects of aging on the nanomechanical properties and 3D surface topographical parameters of an experimental Zirconia Toughened Alumina (ZTA) composite compared to its respective individual counterpart materials. METHODS: Disk-shaped specimens comprised of three material groups were processed: 1) ZTA 70/30 (70% alumina reinforced with 30% second-generation 3Y-TZP); 2) Zpex (Second-generation 3Y-TZP), and; 3) Al2O3 (High purity Alumina) (n = 10/material, 12 × 1 mm). After synthesis, ceramic powders were pressed, the green-body samples were sintered and polished. Nanoindentation testing was performed to record elastic modulus (E) and hardness (H). Interferometry was utilized to assess 3D surface roughness parameters (Sa, Sq), while X-ray diffraction (XRD) and scanning electron microscope (SEM) assessed the crystalline content and microstructure. All tests were performed before and after simulated aging (134°C, 2.2 bar, 20 h). Statistical analyses were performed using linear mixed-model and least square difference pos-hoc tests (α = 5%). RESULTS: XRD spectra indicated increase of monoclinic peaks for Zpex (~18%) relative to ZTA 70/30 (~2.5%) after aging. Additionally, aging did not affect the surface roughness parameters of ZTA 70/30 and Al2O3, although a significant increase in Sa was recorded for Zpex following aging (~90 nm) (p < 0.001). Al2O3 yielded the highest H and E values (H:21 GPa, E: 254 GPa), followed by ZTA 70/30 (H: 13 GPa, E: 214 GPa) and Zpex (H:11 GPa, E: 167 GPa), all significantly different (p < 0.03). CONCLUSION: ZTA 70/30 and Al2O3 presented high hydrothermal stability with respect to all evaluated variables, where artificial aging significantly increased the monoclinic content and surface roughness of Zpex.

Microstructural, mechanical, and optical characterization of an experimental aging-resistant zirconia-toughened alumina (ZTA) composite.

OBJECTIVE: To evaluate the effect of aging on the microstructural, mechanical, and optical properties of an experimental zirconia-toughened alumina composite with 80%Al2O3 and 20%ZrO2 (ZTA Zpex) compared to a translucent zirconia (Zpex) and Alumina. METHODS: Disc-shaped specimens were obtained by uniaxial and isostatic pressing the synthesized powders (n = 70/material). After sintering and polishing, half of the specimens underwent aging (20 h, 134 °C, 2.2 bar). Crystalline content and microstructure were evaluated using X-ray diffraction and scanning electron microscopy, respectively. Specimens underwent biaxial flexural strength testing to determine the characteristic stress, Weibull modulus, and reliability. Translucency parameter (TP) and Contrast ratio (CR) were calculated to characterize optical properties. RESULTS: ZTA Zpex demonstrated a compact surface with a uniform dispersion of zirconia particles within the alumina matrix, and typical alumina and zirconia crystalline content. ZTA Zpex and alumina exhibited higher CR and lower TP than Zpex. ZTA Zpex and Zpex showed significantly higher characteristic stress relative to alumina. While aging did not affect optical and mechanical properties of ZTA Zpex and alumina, Zpex demonstrated a significant increase in translucency, as well as a in characteristic stress. Alumina reliability was significantly lower than others at 300 MPa, ZTA Zpex and Zpex reliability decreased at 800 MPa, except for aged Zpex. SIGNIFICANCE: While aging did not affect the mechanical nor the optical properties of ZTA Zpex and alumina, it did alter both properties of Zpex. The results encourage further investigations to engineer ZTA as a framework material for long span fixed dental prostheses specially where darkened substrates, such as titanium implant abutments or endodontically treated teeth, demand masking.

Silica-Based Infiltrations for Enhanced Zirconia-Resin Interface Toughness.

Novel silica-based infiltrations on the surface of zirconia have the potential to improve their bondability, allowing for the etching/silane adhesive bonding technique. Nonetheless, adhesively bonded joints are subject to mixed tensile and shear stresses when the restoration is in occlusal service. Thus, we aimed to investigate the effect of 2 novel silica-based infiltrations on the interfacial toughness of adhesively bonded zirconia using the Brazil nut method, which allows for controlled types of stresses to be applied at the interfaces. In total, 150 3Y-TZP (In-Ceram YZ; Vita) Brazil nuts were machined and randomly assigned to 3 groups: C, control (air abraded); SG, sol-gel silica infiltration; and GI, glass infiltration. SG specimens were immersed twice in silicic acid for 20 min and dried (100°C, 1 h). GI specimens were presintered (1,400°C, 1 h) before a glass powder slurry was applied to the intaglio surface. All specimens were then sintered (1,530°C, 2 h). Following adhesive bonding (Panavia F 2.0, Kuraray) and water storage (37°C) for 10 d, the Brazil nuts were subdivided into groups baseline and aged (40,000 thermal cycles between 5°C and 55°C, with a dwell time of 30 s). The Brazil nuts were subjected to axial-loading tests using various inclinations (precrack angle with load direction): Θ = 0°, 5°, 10°, 15°, or 25°, which define the stress type at the interface, from pure tension (0°) to increasing levels of shear. Under pure tension (0°), GI yielded superior interfacial fracture energy, SG and C were similar, and aging had no effect. Under predominantly shear stresses (25°), aging significantly decreased interfacial fracture energy of C and SG, while GI remained stable and was superior. The glass infiltration of the zirconia intaglio surface increases its adhesive bonding interfacial toughness. The sol-gel silica infiltration method requires improvement to obtain a homogeneous surface infiltration and an enhanced bond strength.

A new silica-infiltrated Y-TZP obtained by the sol-gel method.

OBJECTIVE: The aim of this study was to evaluate silica infiltration into dental zirconia (VITA In-Ceram 2000 YZ, Vita Zahnfabrik) and its effects on zirconia's surface characteristics, structural homogeneity and bonding to a resin cement. METHODS: Infiltration was performed by immersion of the pre-sintered zirconia specimens in silica sols for five days (ZIn). Negative (pure zirconia specimens, ZCon-) and positive controls (specimens kept in water for 5 days, ZCon+) were also performed. After sintering, the groups were evaluated by X-ray diffraction (XRD), grazing angle X-ray diffraction (DRXR), scanning electron microscopy (SEM), contact angle measurements, optical profilometry, biaxial flexural test and shear bonding test. Weibull analysis was used to determine the Weibull modulus (m) and characteristic strength (σ0) of all groups. RESULTS: There were no major changes in strength for the infiltrated group, and homogeneity (m) was also increased. A layer of ZrSiO4 was formed on the surface. The bond strength to resin cement was improved after zirconia infiltration, acid conditioning and the use of an MDP primer. CONCLUSION: The sol-gel method is an efficient and simple method to increase the homogeneity of zirconia. Infiltration also improved bonding to resin cement. CLINICAL SIGNIFICANCE: The performance of a zirconia infiltrated by silica gel improved in at least two ways: structural homogeneity and bonding to resin cement. The infiltration is simple to perform and can be easily managed in a prosthesis laboratory.