RESUMEN
OBJECTIVE: To assess the influence of calcination process on the properties of minimally processed recycled 3Y-TZP, and to compare it with its commercial counterpart. METHODS: Non-milled 3Y-TZP waste was collected, fragmented and ball-milled to a granulometric < 5 µm. Half of the recycled powder was calcined at 900 °C. Recycled 3Y-TZP disks were uniaxially pressed and sintered to create two recycled groups: 1) Calcined and 2) Non-calcined to be compared with a commercial CAD/CAM milled 3Y-TZP. The microstructure of experimental groups was assessed through density (n = 6), scanning electron microscopy (n = 3) and energy-dispersive X-ray spectroscopy (n = 3); and the crystalline content was evaluated through X-ray diffraction (XRD) (n = 3). Optical and mechanical properties were investigated through reflectance tests (n = 10), and Vickers hardness, fracture toughness (n = 5), and biaxial flexural strength tests (n = 16), respectively. Fractographic analysis was performed to identify fracture origin and crack propagation. Statistical analyses were performed through ANOVA followed by Tukey´s test, and by Weibull statistics. RESULTS: Particle size distribution of recycled powder revealed an average diameter of â¼1.60 µm. The relative density of all experimental groups was > 98.15 % and XRD analysis exhibited a predominance of tetragonal-phase in both recycled groups, which were similar to the crystallographic pattern of the control group. Cross-section micrographs presented flaws on the non-calcined group, and a more homogeneous microstructure for the calcined and commercial groups. Commercial samples showed lower contrast-ratio and higher translucency-parameter than the recycled groups, where non-calcined presented higher translucency-parameter and lower contrast-ratio than its calcined counterpart. The commercial group presented higher fracture toughness and characteristic strength than the recycled groups. Moreover, the calcined group exhibited higher hardness, characteristic strength, and probability of survival at higher loads than the non-calcined group. Fractographic analysis depicted the presence of microstructural flaws in the non-calcined group, which may have acted as stress-raisers and led to failures at lower flexural strengths values. SIGNIFICANCE: The calcination process improved the microstructure, optical, and mechanical properties of the recycled 3Y-TZP.
RESUMEN
PURPOSE: To synthesize a zirconia-toughened alumina (ZTA) composite with 85% alumina matrix reinforced by 15% zirconia and to characterize its optical and mechanical properties before and after artificial aging, to be compared with a conventional dental zirconia (3Y-TZP). MATERIAL AND METHODS: After syntheses, ZTA and 3Y-TZP powders were uniaxially and isostatically pressed. Green-body samples were sintered and polished to obtain 80 disc-shaped specimens per group (12 × 1 mm, ISO 6872:2015). The crystalline content and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Optical properties were determined by the calculation of contrast ratio (CR) and translucency parameter (TP) using reflectance data. Mechanical properties were assessed by Vickers hardness, fracture toughness and biaxial flexural strength test (BFS). All analyses were conducted before and after artificial aging (20h, 134 °C, 0.22 MPa). Optical parameters and microhardness differences were evaluated through repeated-measures analysis of variance (p < 0.05). BFS data were analyzed using Weibull statistics (95% CI). RESULTS: The synthesis of the experimental ZTA composite was successful, with 98% of theoretical density, as shown in the SEM images. XRD patterns revealed typical zirconia and alumina crystalline phases. ZTA optical properties parameters showed no effect of aging, with a high CR and low TP values denoting a high masking-ability. 3Y-TZP presented lower masking-ability and aging significantly affected its optical properties. ZTA Vickers hardness, fracture toughness and Weibull parameters, including characteristic stress and Weibull modulus were not influenced by aging, while 3Y-TZP presented a significant decrease in characteristic stress and increase in fracture toughness after aging. The ZTA probability of survival for missions of 300 and 500 MPa was estimated at ~99% validating its use for 3-unit posterior fixed dental prostheses (FDP), and no different from conventional 3Y-TZP. At high-stress mission (800 MPa) a significant decrease in probability of survival was observed for aged 3Y-TZP (84%) and for immediate and aged ZTA (73 and 82% respectively). CONCLUSION: The ZTA composite presented a dense microstructure, with preservation of the crystalline content, optical and mechanical properties after artificial aging, which encourages future research to validate its potential use for large span FDP.
