Development of ZTA (80% Al2O3/20% ZrO2) pre-sintered blocks for milling in CAD/CAM systems.

The present work aims to develop a production method of pre-sintered zirconia-toughened-alumina (ZTA) composite blocks for machining in a computer-aided design and computer-aided manufacturing (CAD-CAM) system. The ZTA composite comprised of 80% Al2O3 and 20% ZrO2 was synthesized, uniaxially and isostatically pressed to generate machinable CAD-CAM blocks. Fourteen green-body blocks were prepared and pre-sintered at 1000 °C. After cooling and holder gluing, a stereolithography (STL) file was designed and uploaded to manufacture disk-shaped specimens projected to comply with ISO 6872:2015. Seventy specimens were produced through machining of the blocks, samples were sintered at 1600 °C and two-sided polished. Half of the samples were subjected to accelerated autoclave hydrothermal aging (20h at 134 °C and 2.2 bar). Immediate and aged samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Optical and mechanical properties were assessed by reflectance tests and by biaxial flexural strength test, Vickers indentation and fracture toughness, respectively. Samples produced by machining presented high density and smooth surfaces at SEM evaluation with few microstructural defects. XRD evaluation depicted characteristic peaks of alpha alumina and tetragonal zirconia and autoclave aging had no effect on the crystalline spectra of the composite. Optical and mechanical evaluations demonstrated a high masking ability for the composite and a characteristic strength of 464 MPa and Weibull modulus of 17, with no significant alterations after aging. The milled composite exhibited a hardness of 17.61 GPa and fracture toughness of 5.63 MPa m1/2, which remained unaltered after aging. The synthesis of ZTA blocks for CAD-CAM was successful and allowed for the milling of disk-shaped specimens using the grinding method of the CAD-CAM system. ZTA composite properties were unaffected by hydrothermal autoclave aging and present a promising alternative for the manufacture of infrastructures of fixed dental prostheses.

Stability of fatigued and aged ZTA compared to 3Y-TZP and Al2O3 ceramic systems.

To evaluate the effect of fatigue and aging on the crystalline content and reliability of a zirconia-toughened-alumina (ZTA) composite compared to its individual counterpart materials (3Y-TZP and Al2O3). Thirty-six disc-shaped specimens per group were obtained to comply with ISO 6872:2015. Crystalline content, microstructure and reliability of experimental groups were evaluated in four stages: 1) immediate; 2) aged; 3) fatigued; 4) aged + fatigue. Aging was performed in autoclave and Step-Stress-Accelerated-Life-Testing (SSALT) was performed using three stress profiles. Weibull statistics were used to determine Weibull parameters and life-expectancy. A significant increase in monoclinic phase in 3Y-TZP was observed after aging (19.31%), fatigue (17.88%) and aging + fatigue (55.81%), while ZTA evidenced minimal variation among all conditions (<5.69%). 3Y-TZP presented higher reliability than ZTA at 300 and 500 MPa, and ZTA outperformed Al2O3 at the same stress missions. None of the ceramics yielded acceptable reliability at 800 MPa. A higher characteristic strength was observed for 3Y-TZP, followed by ZTA and Al2O3. While after aging ZTA and Al2O3 remained stable, 3Y-TZP exhibited a significant increase in the characteristic stress. Aging did not affect the reliability of ZTA and Al2O3. 3Y-TZP demonstrated an increase in monoclinic content and characteristic strength after aging.

Alumina-toughened zirconia for dental applications: Physicochemical, mechanical, optical, and residual stress characterization after artificial aging.

To characterize the physicomechanical properties of an alumina-toughened zirconia (ATZ). ATZ synthesis consisted of the addition of alumina particles in an yttria-stabilized tetragonal zirconia polycrystals (3Y-TZP) matrix. Specimens were obtained by uniaxial and isostatic pressing ATZ and 3Y-TZP powders and sintering at 1600°C/1 h and 1550°C/1 h, respectively. Crystalline content and residual stress were evaluated using X-ray diffraction (XRD). Microstructure was characterized by scanning electron microscopy (SEM). Optical properties were determined by reflectance test. Mechanical properties were assessed by biaxial flexural strength test. All analyses were performed before and after aging (134°C, 20 h, 2 bar). XRD and SEM revealed a typical ATZ and 3Y-TZP crystalline content, chiefly tetragonal phase, with a dense polycrystalline matrix, though a smaller grain size for ATZ. Aging triggered a similar monoclinic transformation for both systems; however, ATZ exhibited higher residual compressive stresses than 3Y-TZP. While as-processed 3Y-TZP demonstrated significantly higher characteristic strength relative to ATZ, no significant difference was observed after aging (~215 MPa increase in the ATZ strength). ATZ presented significantly higher opacity relative to 3Y-TZP, although aging significantly increased the translucency of both systems (increase difference significantly higher in the 3Y-TZP compared to ATZ). ATZ physicomechanical properties support its applicability in the dental field, with a lower detrimental effect of aging relative to 3Y-TZP.

Aging resistant ZTA composite for dental applications: Microstructural, optical and mechanical characterization.

OBJECTIVE: To synthesize a zirconia toughened alumina (ZTA) composite with 70% alumina reinforced by 30% zirconia for dental applications and to characterize its microstructure and optical properties for comparison with the isolated counterpart materials and a first-generation 3Y-TZP. METHODS: Disc-shaped specimens were divided in four groups (n = 70/material): (1) 3YSB-E (first generation 3Y-TZP), (2) Zpex (second generation 3Y-TZP), (3) alumina, and (4) ZTA-Zpex 70/30. After synthesis, ceramic powders were pressed, and green-body samples sintered following a predetermined protocol. Specimens were polished to obtain a mirror surface finish. Apparent density was measured by Archimedes principle. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the crystalline content and microstructure. Reflectance tests were performed to determine the contrast-ratio (CR) and translucency-parameter (TP). Mechanical properties were assessed by biaxial flexural strength (BFS) test. All analyses were conducted before and after artificial aging (20 h, 134 °C, 2.2 bar). Optical parameters were evaluated through repeated-measures analysis of variance and Tukey tests (p < 0.05). BFS data were analyzed using Weibull statistics (95% CI). RESULTS: High density values (95-99%) were found for all ceramic materials and SEM images exhibited a dense microstructure. While XRD patterns revealed the preservation of crystalline content in the ZTA composite, an increase in the monoclinic peak was observed for pure zirconias after aging. Significantly higher CR and lower TP values were observed for the ZTA composite, followed by alumina, 3YSB-E, and Zpex. The highest characteristic stress was recorded for 3YSB-E, followed by intermediate values between ZTA and Zpex, and the lowest for alumina. Aging affected the optical and mechanical properties of both zirconias, while remained stable for ZTA composite and alumina. SIGNIFICANCE: The synthesis of experimental 70-30% ZTA composite was successful and its relevance for dental applications relies on its higher masking ability, aging resistance, and strength similar to zirconia.