Nanoindentation creep versus bulk compressive creep of dental resin-composites

ObjectivesTo evaluate nanoindentation as an experimental tool for characterizing the viscoelastic time-dependent creep of resin-composites and to compare the resulting parameters with those obtained by bulk compressive creep.MethodsTen dental resin-composites: five conventional, three bulk-fill and two flowable were investigated using both nanoindentation creep and bulk compressive creep methods. For nano creep, disc specimens (15 mm × 2 mm) were prepared from each material by first injecting the resin-composite paste into metallic molds. Specimens were irradiated from top and bottom surfaces in multiple overlapping points to ensure optimal polymerization using a visible light curing unit with output irradiance of 650 mW/cm2. Specimens then were mounted in 3 cm diameter phenolic ring forms and embedded in a self-curing polystyrene resin. Following grinding and polishing, specimens were stored in distilled water at 37 °C for 24 h. Using an Agilent Technologies XP nanoindenter equipped with a Berkovich diamond tip (100 nm radius), the nano creep was measured at a maximum load of 10 mN and the creep recovery was determined when each specimen was unloaded to 1 mN. For bulk compressive creep, stainless steel split molds (4 mm × 6 mm) were used to prepare cylindrical specimens which were thoroughly irradiated at 650 mW/cm2 from multiple directions and stored in distilled water at 37 °C for 24 h. Specimens were loaded (20 MPa) for 2 h and unloaded for 2 h. One-way ANOVA, Levene's test for homogeneity of variance and the Bonferroni post hoc test (all at p ≤ 0.05), plus regression plots, were used for statistical analysis.ResultsDependent on the type of resin-composite material and the loading/unloading parameters, nanoindentation creep ranged from 29.58 nm to 90.99 nm and permanent set ranged from 8.96 nm to 30.65 nm. Bulk compressive creep ranged from 0.47% to 1.24% and permanent set ranged from 0.09% to 0.38%. There was a significant (p = 0.001) strong positive non-linear correlation (r2 = 0.97) between bulk creep and nano creep that could also be expressed via a simple fractional-power function. A significant (p = 0.003) positive linear correlation (r2 = 0.69) existed between nano creep recovery and bulk creep recovery. With both methods of examination, except for Venus Bulk Fill™ (VB), the flowable and bulk-fill resin-composites exhibited creep within the range exhibited by the conventional resin-composites.SignificanceDespite the differences in loading and unloading conditions, in both methods of examination the correlation observed between the creep and recovery responses for a set of resin-composites was high. Both nano creep and recovery positively correlated with loading and unloading rates, respectively.