Objectives
This study seeks to correlate the interrelated properties of conversion, shrinkage, modulus and stress as dimethacrylate networks transition from rubbery to glassy states during photopolymerization.
Methods
An unfilled BisGMA/TEGDMA resin was photocured for various irradiation intervals (7–600 s) to provide controlled levels of immediate conversion, which was monitored continuously for 10 min. Fiber optic near-infrared spectroscopy permitted coupling of real-time conversion measurement with dynamic polymerization shrinkage (linometer), modulus (dynamic mechanical analyzer) and stress (tensometer) development profiles.
Results
The varied irradiation conditions produced final conversion ranging from 6 % to more than 60 %. Post-irradiation conversion (dark cure) was quite limited when photopolymerization was interrupted either at very low or very high levels of conversion while significant dark cure contributions were possible for photocuring reactions suspended within the post-gel, rubbery regime. Analysis of conversion-based property evolution during and subsequent to photocuring demonstrated that the shrinkage rate increased significantly at about 40 % conversion followed by late-stage suppression in the conversion-dependent shrinkage rate that begins at about 45–50 % conversion. The gradual vitrification process over this conversion range is evident based on the broad but well-defined inflection in the modulus versus conversion data. As limiting conversion is approached, modulus and, to a somewhat lesser extent, stress rise precipitously as a result of vitrification with the stress profile showing little if any late-stage suppression as seen with shrinkage.
Significance
Near the limiting conversion for this model resin, the volumetric polymerization shrinkage rate slows while an exponential rise in modulus promotes the vitrification process that appears to largely dictate stress development.
Objective
To determine if acid-etched, cross-linked dentin can be dehydrated without lowering bond strength below that of cross-linked wet-bonded dentin in vitro.
Methods
Using extracted human third molars, control acid-etched dentin was bonded with Single Bond Plus, using either the wet- or dry-bonding technique. Experimental acid-etched dentin was treated with 5 mass% grape seed extract (GSE) in different solvents for 1 min before undergoing wet vs. dry resin-dentin bonding with Single Bond Plus. Completely demineralized dentin beams were treated with 5% GSE for 0, 1 or 10 min, before measuring stiffness by 3-point flexure. Other completely demineralized beams were treated similarly and then incubated in buffer for 1 week to measure the collagen solubilization by endogenous dentin proteases.
Results
24 hr microtensile bond strengths (μTBS) in wet and dry controls were 53.5 ± 3.6 and 9.4 ± 1.8 MPa, respectively (p < 0.05). 5% GSE in water gave μTBS of 53.7 ± 3.4 and 39.1 ± 9.7 MPa (p < 0.05), respectively, while 5% GSE in ethanol gave μTBS of 51.2 ± 2.3 and 35.3 ± 2.0 MPa (p < 0.05). 5% GSE in 5% EtOH/95% water gave wet and dry μTBS of 53.0 ± 2.3 and 55.7 ± 5.1 MPa (p > 0.05). Cross-linking demineralized dentin with 5% GSE increased stiffness of dentin and decreased collagen degradation (p<0.05).
Significance
5% GSE pretreatment of acid-etched dentin for 1 min permits the dentin to be completely air-dried without lowering bond strength.
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