Post-hot isostatic pressing: A healing treatment for process related defects and laboratory grinding damage of dental zirconia?

Abstract

ObjectiveProcessing parameters (powder granulation, compaction, debinding, greenbody shaping, sintering) and post-sinter rough, even fine grinding are influencing the final mechanical properties of 3Y-TZP. The hypothesis of this study was that post-sinter hot isostatic pressing (post-HIP) would be beneficial for improving reliability and strength of both sintered and coarse ground sintered zirconia by closing or reducing surface and/or small volume defects. Methods75 sintered bars of an experimental 3Y-TZP (3mm×4mm×45mm) with chamfered edges and 15μm diamond surface finish were provided by the manufacturer (Ivoclar Vivadent) and randomly distributed in five groups of N=15 each. G1 served as control (as received); G2 was post-HIPed at 1400°C and G3 at 1350°C, both using a pressure of 195MPa in Ar for 1h; G4 was coarse ground with 120μm diamond disk grain size; G5 was ground 120μm and post-HIPed at 1350°C at 195MPa, 1h in Ar. The specimens were fractured in air in 4 point-bending. Weibull characteristic strength (σ0) in MPa, m parameter (reliability) and confidence intervals (CI) at 90% confidence level are reported. Identification of the critical flaw was performed by SEM on the fractured surface of all specimens and XRD performed in all groups. ResultsG1: σ0=973 (932–1016), m=10.6 (7.45–15.1); G2: σ0=930 (871–995), m=6.9 (4.87–9.9); G3: σ0=898 (848–952), m=7.94 (5.6–11.4); G4: σ0=921 (857–991), m=6.35 (4.48–9.11); G5: σ0=881 (847–918), m=11.4 (8.03–16.3). G5 had a significantly lower σ0 than G1. No significant differences were seen in the reliability (m) among the groups. Fractography revealed critical intrinsic subsurface flaws of 10–60μm present in all groups resulting from the processing parameters. No “healing” (i.e. closing of defects by densification) resulted after post-HIP. Grinding sintered zirconia with 120μm diamond disks induced radial cracks of 10–20μm and an important pseudo-cubic phase transformation (56wt%) that was not completely removed after post-HIP. Post-HIP increased slightly the relative density by 0.1% but without improving the strength and reliability. SignificancePost-HIP was not efficient in closing large (10–60μm) subsurface (volume) processing defects.