Effect of sintering process on microstructure, 4-point flexural strength, and grain size of yttria-stabilized tetragonal zirconia polycrystal for use in monolithic dental restorations.

Statement Of Problem: Modifications have been made in the microstructure and sintering parameters of monolithic zirconia to improve esthetics qualities and avoid chipping of 2-layer restorations. However, how these modifications affect the physical and mechanical properties of zirconia is unclear.

Purpose: The purpose of this in vitro study was to compare the influence of different sintering parameters on the microstructure, 4-point flexural strength, density, and grain size of 2 commercially available zirconia advocated for the fabrication of monolithic dental prostheses and 1 commercially available zirconia for use as a core material.

Material And Methods: Three presintered blocks (Ceramill Zolid, Prettau, and IPS e.max ZirCAD) were used. Specimens were cut and sintered as per the manufacturer's recommendation or as per a modified heating protocol. Ceramill Zolid (Z1450) was sintered at 1450 °C, Prettau (P1600) was sintered at 1600 °C, and IPS e.max ZirCAD (I1530) was sintered at 1530 °C by following the manufacturer's heating protocol. Groups Ceramill Zolid Z1530 and Z1600 were sintered at temperatures higher than the manufacturer's recommendation. Specimens from each group (n=13) were analyzed with X-ray diffraction (XRD), density calculus, average grain size measurement, and 4-point flexural tests. Data were compared by using ANOVA (α=.05).

Results: XRD analysis showed the presence of a tetragonal metastable phase in all groups before and after sintering. No significant differences were found in relative density values for the 3 Ceramill groups (5.98 g/cm). Groups I1530 (6.03 g/cm) and P1600 (6.03 g/cm) had similar density results greater than 6.00 g/cm. The average grain size of all groups remained lower than 1 μm. P1600 had the highest grain size (0.817 μm), and Z1450 presented the lowest grain size (0.465 μm). P1600 showed the most homogeneous flexural strength and the highest Weibull modulus (m=8.22). Z1530 presented the lowest Weibull modulus (m=4.58). IPS e.max ZirCAD (I1530) had the highest flexural strength (1057.41 ±150.54 MPa), and Ceramill Zolid Z1450 had the lowest (621.01 ±138.08 MPa).

Conclusions: The flexural strength, microstructure, crystal phase, and grain size of the analyzed zirconia varied as per the sintering processing. The IPS e.max ZirCAD had the highest flexural strength (1057.41 ±150.54 MPa), followed by Prettau zirconia (864.18 ±118.21), with a statistically significant difference (P<.05). The Ceramill Zolid zirconia presented the lowest flexural strength, as well as the lowest reliability for all sintering parameters used (Z1450: 621.01 ±138.08 MPa and m=5.42; Z1530: 713.10 ±175.44 MPa and m=4.58; Z1600: 630.15 ±112.08 MPa and m=6.87). At a lower heating rate (8 °C/min), the final density increased and excessive grain growth in group Z1530 was prevented.