OBJECTIVES: To 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. METHODS: Ten 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 (15mm×2mm) 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 650mW/cm(2). Specimens then were mounted in 3cm 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 24h. Using an Agilent Technologies XP nanoindenter equipped with a Berkovich diamond tip (100nm radius), the nano creep was measured at a maximum load of 10mN and the creep recovery was determined when each specimen was unloaded to 1mN. For bulk compressive creep, stainless steel split molds (4mm×6mm) were used to prepare cylindrical specimens which were thoroughly irradiated at 650mW/cm(2) from multiple directions and stored in distilled water at 37°C for 24h. Specimens were loaded (20MPa) for 2h and unloaded for 2h. 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. RESULTS: Dependent on the type of resin-composite material and the loading/unloading parameters, nanoindentation creep ranged from 29.58nm to 90.99nm and permanent set ranged from 8.96nm to 30.65nm. 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 (r(2)=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 (r(2)=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. SIGNIFICANCE: Despite 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.
OBJECTIVES: To 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. METHODS: Ten 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 (15mm×2mm) 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 650mW/cm(2). Specimens then were mounted in 3cm 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 24h. Using an Agilent Technologies XP nanoindenter equipped with a Berkovich diamond tip (100nm radius), the nano creep was measured at a maximum load of 10mN and the creep recovery was determined when each specimen was unloaded to 1mN. For bulk compressive creep, stainless steel split molds (4mm×6mm) were used to prepare cylindrical specimens which were thoroughly irradiated at 650mW/cm(2) from multiple directions and stored in distilled water at 37°C for 24h. Specimens were loaded (20MPa) for 2h and unloaded for 2h. 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. RESULTS: Dependent on the type of resin-composite material and the loading/unloading parameters, nanoindentation creep ranged from 29.58nm to 90.99nm and permanent set ranged from 8.96nm to 30.65nm. 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 (r(2)=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 (r(2)=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. SIGNIFICANCE: Despite 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.