Effect of sintering process on microstructure, 4-point flexural strength, and grain size of yttria-stabilized...

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.

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.

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).

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/cm³). Groups I1530 (6.03 g/cm³) and P1600 (6.03 g/cm³) had similar density results greater than 6.00 g/cm³. 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).

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.