J.R. Condon

In vitro aging of dental composites in water—Effect of degree of conversion, filler volume, and filler/matrix coupling

The purpose of this study was to evaluate the long-term effect of aging in water on the physical properties of experimental composites having systematically controlled differences in degree of conversion (DC), filler volume fraction (Vf), and percentage of silane-treated fillers. Composites were made with a 50% Bis-GMA:50% TEGDMA light-cured resin and a 1-2 microm (average size) strontium glass filler (+ 5 wt% SiO2 microfiller). For composites A-E, the DC was varied from 56-66% by changing the curing time; for D and F-I, the Vf was varied from 28-62 vol%; and for D and J-M, the percent of fillers with a silane coupling agent (gamma-MPS) was varied from 20-100%. Fracture toughness (KIc), flexure strength (FS), elastic modulus (E), and hardness (KHN) were tested after soaking in water at 37 degrees C for 1 day, 6 months, 1 year, and 2 years. The KIc was reduced 20-30% for all composites after 6 months, with minimal changes thereafter. The FS was reduced for several composites at 6 months, but only those with poor cure (A and B) were lower at 2 years than they were initially. The E was not reduced for most composites. Hardness was reduced for most composites after 6 months, but many returned to their original levels at 2 years. Long-term aging in water caused a reduction in the KIc, independent of composition, but had little effect on other properties, suggesting limited degradation of composites in water.

Wear and Marginal Breakdown of Composites with Various Degrees of Cure

Loss of anatomical form due to wear has been cited as one factor limiting the clinical use of posterior composites. The physical properties and possibly the wear resistance of composite are influenced by the extent to which it is cured. The aim of this study was to vary degree of conversion (DC) in composites to test the hypothesis that resistance to wear and marginal breakdown could be improved by enhanced curing. A light-cured hybrid composite containing a 50% Bis-GMA/50% TEGDMA resin and 62 vol% of strontium glass (1 to 2 μm) with microfill silica was formulated (Bisco). Composite was placed into two 2.5-mm-diameter cylindrical holes in Co-Cr teeth replacing first and second molars in the mandibular dentures of 50 edentulous patients. The composites were light-cured for different time periods (9 s, 12 s, 25 s, 40 s, and 40 s + 10 min at 120°C) and then polished. The microfill Heliomolar was also tested. DC (%) was measured by FTIR and ranged between 55% for 9 s of light-curing and 67% for 40 s of light-curing followed by heat application. Impressions were evaluated at baseline, 6 mo, 1 yr, and 2 yrs. Stone casts were evaluated independently by three observers to determine the % of the total margin exhibiting breakdown. Epoxy replicas were measured with a profilometer for wear. Wear of the hybrid composite at 2 yrs ranged from a high of 144 μm with 9 s of light-curing to a low of 36 μm with 40 s of light-curing followed by heat. Heliomolar exhibited from 11 to 16 μm of wear at 2 yrs. There was a strong negative correlation (r2 = 0.91) between the degree of cure and the abrasive wear of the hybrid composites. Marginal breakdown was negligible for the hybrids, and was reduced for the microfill from 40% to 15% of the margin by heat treatment. This study showed that the resistance to abrasive wear of a dental composite could be improved by enhancement of its degree of conversion.

Rate of elution of leachable components from composite

The uptake of solvent and the elution of molecules from a dental composite and an unfilled resin were monitored with time during soaking in either water or an ethanol/water mixture. The results showed that approximately 50% of the leachable species were eluted from the composite within three hours of soaking in water, while 75% of the leachable molecules were eluted into the ethanol/water mixture. Elution of nearly all of the leachable components was complete within a 24-hour period in either solvent. The study lends support to the view that dental composites do not provide a chronic source of unreacted monomer to the pulp or other oral tissues, due to a rapid and complete elution of the molecules.

The Effects of Adhesive Thickness on Polymerization Contraction Stress of Composite

A layer of an unfilled adhesive resin placed between the tooth and composite restoration has been shown to absorb some of the stress generated in the composite during polymerization and to reduce interfacial leakage. The objectives of this study were to measure the change in polymerization contraction stress of bonded composite as the thickness of the resin adhesive was systematically varied, and to correlate the effects of the adhesive thickness and reduced stress on marginal leakage in class V cavities. The maximum contraction force of composite (Herculite XRV) was measured in a tensilometer as the thickness of the adhesive bonding agent (Scotchbond MP) was varied from 20 to 300 μm. Composite was placed in Class V cavities prepared on the labial surfaces of bovine teeth to which different thicknesses of adhesive had been applied by layering, and a marginal leakage test was performed by means of staining with silver nitrate. Contraction stress decreased significantly as the adhesive thickness was increased. This result was supported by a theoretical examination of the data. In class V cavities, additional adhesive layering in the marginal area reduced the overall degree of microleakage. The contraction stress generated during the placement of a composite restoration contributes significantly to early marginal leakage, and this stress was significantly absorbed and relieved by the application of an increasing thickness of low-stiffness adhesive.

Reduction of polymerization contraction stress for dental composites by two-step light-activation

OBJECTIVES The goal of this study was to assess the reduction of polymerization contraction stress of composites during a two-step light-activation process and to relate this reduction to the process of polymerization shrinkage and specimen thickness. METHODS Three test procedures were performed to compare two-step light-activation with delay with one-step continuous irradiation of composites: polymerization contraction stress using a closed-loop servohydraulic testing instrument, polymerization shrinkage by a mercury dilatometer, and degree of conversion by FTIR. For the one-step continuous curing method, the samples were light-activated for 60s at 330 mW/cm(2). For the two-step curing method, a 5s light exposure at 60 mW/cm(2) was followed by 2 min without light exposure, and then a second light exposure for 60s at 330 mW/cm(2). The same light parameters were used for measurements of stress, shrinkage, and degree of conversion. Three composites, Heliomolar, Herculite and Z100 were evaluated. The contraction stress experiments were repeated with varying thickness for Herculite using the one-step and two different two-step techniques. RESULTS Polymerization contraction stress 10 min after light-activation was significantly reduced (P<0.05) by the two-step method: 29.7% for Heliomolar, 26.5% for Herculite, and 19.0% for Z100. Total volumetric shrinkage and degree of conversion were not significantly different for composites cured by the two different techniques. Increasing the thickness of the composite sample reduced the measured contraction stress, especially for one of the two-step curing methods. SIGNIFICANCE A combination of low initial energy density followed by a lag period before a final high-intensity light irradiation provides a reduction of polymerization contraction stresses in dental composites. The stress reductions cannot be attributed to reductions in degree of conversion or unrestrained volumetric shrinkage.

In vitro Wear of Composite with Varied Cure, Filler Level, and Filler Treatment:

For the clinical wear of composite filling materials to be reduced, compositional factors such as degree of cure, filler level, and silanation level should be optimized. An oral-wear-simulating machine was used to explore the effects of these factors on abrasion and attrition wear as well as on opposing enamel wear. The composites were made from Sr glass (1-2 μm avg) and a 50/50 Bis-GMA/TEGDMA resin. Series I (A-D, E) were light-cured (Triad II) for 9, 12, 25, and 40 sec/side to produce degree of cure (DC) as measured by FTIR of 56, 60, 61, and 63%, respectively. E received an additional heat cure (120°C for 10 min) to reach a DC of 66%. Series II (D, F-I) were filled to 62, 53, 48, 37, and 28 vol%, respectively. In series III (D, J-M), the portion of fillers treated with a silane coupler (MPS) was 100, 80, 60, 40, and 20%, respectively. Samples were cycled 50,000 times against an enamel antagonist in a poppy seed/PMMA slurry in the oral wear simulator to produce abrasion (load = 20 N) and attrition (load = 70 N) simultaneously. Wear depth (μm; n = 5) was measured by profilometry. Results for each series were analyzed by ANOVA/Tukeys (p ≤0.05). The wear depths did reflect cure values, though only the abrasion difference for E < A was significant. Greater wear was correlated with lower filler levels (r2 = 0.88; p < 0.05), significantly increasing below 48 vol% (G). Wear increased linearly as the percent of silane-treated fillers was reduced (r2 = 0.99; p < 0.05). Abrasion and attrition did not differ significantly for any composite. Wear of the opposing enamel was largely unchanged by these factors. Compositional factors including degree of cure, filler level, and silanation directly affected the wear resistance of dental composites evaluated in an oral wear simulator.

Post-cure heat treatments for composites: properties and fractography

Two commercial and four experimental composites were subjected to post-cure heat treatments of 10 min and 3 h duration immediately after light-curing. Fracture toughness, flexural modulus, microhardness and degree of conversion (FTIR) were evaluated 24 h later. The results showed that post-cure heat treatments at 120 degrees C of short or long duration can be used to produce significant improvements in the degree of cure and the mechanical properties of dental composites used as inlays. A 10 min heat treatment was as effective as a 3 h treatment in enhancing properties and degree of cure. In addition, a 3 h heat treatment carried out 7 days after the initial light-curing was capable of improving properties and cure to almost the same extent as the immediate heat treatments. The improvement in properties, in conjunction with the fractography, indicate a toughening of the filled resin matrix and possibly an improved filler/matrix adhesion in the microfills. The changes appear to be predominantly the result of an increase in degree of cure.

Evaluation of composite wear with a new multi-mode oral wear simulator

OBJECTIVES The goals of this study were to develop a machine which simultaneously produces wear through the two main oral wear mechanisms of abrasion and attrition by the action of an enamel antagonist and to compare the results obtained for dental composites using this machine to those obtained from clinical studies and other in vitro studies. METHODS The accuracy of this new wear tester was determined by examining 11 commercial composite filling materials and 1 amalgam. Specimens were subjected to three-body abrasion and attrition wear for 50,000 cycles. Profilometry was used to quantitate wear of the composites. Linear regression analysis was used to correlate the results to those obtained from clinical studies, as well as from other in vitro wear testers. The area of enamel wear was also determined by image analysis. The SEM was used to evaluate the wear surfaces. RESULTS The lowest abrasion wear was recorded for the amalgam and for the microfill and smaller-particle composites. Attrition wear was enhanced for the microfill composites and one small-particle hybrid. There was a strong correlation between the results obtained with the new wear tester and those obtained in the clinical trials cited in the literature. Wear of the enamel antagonist was the greatest for the composites with the largest particle sizes. The wear tester showed a reasonable correlation with other wear-producing machines. SIGNIFICANCE A new wear tester developed to evaluate and discriminate abrasion and attrition wear provided results similar to those reported in the literature for a variety of commercial composites. The new machine is capable of characterizing the behavior of a material in multiple wear modes simultaneously with one simple, realistic test.

Effect of filler fraction and filler surface treatment on wear of microfilled composites

OBJECTIVES The aim of this study was to determine the effect of filler content and surface treatment on the wear of microfilled composites. METHODS Four microfilled composites with different filler contents (A=20, B=25, C=30, and D=35 vol.%) were made with a light-cured resin (Bis-GMA/UDMA/TEGDMA). The surface treatment of the colloidal silica in each varied: F=functional silane, NF=non-functional silane, U=untreated. Silux Plus served as a control. Specimens were made in steel molds and cured in a light curing unit Triad II (40s/side). Abrasion and attrition wear were evaluated in vitro in a wear tester (OHSU oral wear simulator) with an abrasive slurry (poppy seeds + PMMA) and a human enamel antagonist. The average of five specimens was computed and compared using a ANOVA/Tukeys test at P < or = 0.05. The surface of the wear patterns and the distribution of filler particles were examined using a scanning electron microscope and digital imaging. RESULTS As filler volume increased, wear was reduced regardless of filler treatment. Amounts of wear for specimens C and D were significantly lower than specimens A and B. Composites with functional silane treated microfiller (Group F) produced significantly less wear than those with non-functional microfiller (Group NF) at 30 and 35 vol.%, and less than the untreated microfiller (Group U) at 30 vol.%. Scanning electron microscopy of specimens of group NF showed large filler agglomerates (size > 1 microm) in the resin matrix, while specimens of group F and U showed fewer agglomerates. Digital imaging analysis revealed small filler clusters (size < or = 1 microm) in the resin matrix of all specimens. SIGNIFICANCE Wear resistance of microfilled composites is enhanced by higher filler volumes irrespective of surface treatment, but good filler/matrix adhesion is needed to minimize wear.

Reduced polymerization stress through non-bonded nanofiller particles

The stress that results from the placement of dental composite in a confined setting compromises the integrity of the marginal seal. Dental composites which include nanofiller particles that are not treated with a functional agent to couple them to the resin matrix can result in lower stress levels. Three types of nanofillers were evaluated having either a functional silane coating, a non-functional silane coating. or no coating. These were added at five different vol% levels to a photo-sensitized mixture of three dimethacrylate monomers alone or at three different vol% levels to the same resin filled with mini-filler particles to a clinically realistic level. The stress generated by these materials when cured in a confined setting was measured in a mechanical testing machine. The effect of monomer molecular weight on the stress levels was evaluated by preparing three resin formulations with varied co-monomer levels and filling them with bonded or non-bonded nanofillers. Reductions in polymerization stress of up to 31% were achieved among both the nanofilled resins and the mini-filled composite. The materials which contained a heightened level of diluent monomer produced significantly higher stress levels (ANOVA/Tukeys test, p < 0.05). Significant reductions in polymerization stress can be achieved through minor alterations in composite chemistry.