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.