Robert L. Erickson

Energy dependent polymerization of resin-based composite

OBJECTIVE This study explores the relationship between the extent of polymerization and the radiant energy (dose) applied during the photopolymerization of resin-based composites. METHOD FTIR was used to measure the 5-min and 24-h conversion of four resin-based composites prepared in a thin film and polymerized under conditions of decreasing intensity and a constant exposure time (30s) using a tungsten halogen curing light. The measured conversion was obtained over a wide range of applied radiant energy. Additionally, samples for two of the materials were polymerized at various intensities and exposure times such that the dose remained constant. This process was performed at four dose levels representing approximately 75% of the conversion range. RESULTS The curing profiles (percent conversion versus applied radiant energy) depict a gradual decrease in conversion with decreasing energy followed by a rapid descent. Though there are differences in the maximum conversion attained between the materials, when conversion is represented as a fractional conversion relative to the maximum 24-h value, their 5-min and 24-h curing profiles appear quite similar. Additionally, very similar conversion was measured when the films were exposed using equivalent doses providing evidence for a reciprocal relationship between irradiance (power density) and exposure time. For the 24-h measurements, statistical equivalence (Fishers protected LSD at the 0.05 level) was noted for most of the combinations of exposure time and power density within a given dose. Generally, the exceptions occurred with the shortest exposure times. SIGNIFICANCE A reciprocal relationship between exposure time and power density adds significance to the study of conversion as a function of the total applied dose. This relationship establishes the curing profile as a universal correlation between exposure time and power density.

The effect of filler and silane content on conversion of resin based composite

OBJECTIVE This study examines the influence of filler loading and silane content on the conversion of photoactivated, resin-based composites as determined using Fourier transform infrared spectroscopy (FTIR). METHOD Zirconia/silica filler was processed with a silane coupling agent (gamma-methacryloxypropyltrimethoxysilane) to achieve a range of silane-to-filler compositions. Treated fillers were compounded with a photoactivated BisGMA/TEGDMA resin to yield a series of pastes all containing 72 wt% total solids. Diffuse reflectance FTIR was used to characterize methacrylate unsaturation of the silane on the filler particles while paste conversion was determined using transmission FTIR. A resin matrix conversion was determined by adjusting the paste conversion for silane unsaturation. Two additional series of pastes were compounded to achieve variable filler-to-resin ratios using non-treated filler and filler processed with 8 wt% silane. Paste conversion was determined using transmission FTIR. RESULTS Pastes compounded from fillers containing variable percent silane demonstrated linearly decreasing conversion (R(2)=0.986) with increasing silane content and ranged from 52.7 to 62.8%. Adjusting paste conversion for silane unsaturation yielded similar resin matrix conversion for all cured pastes (65.1+/-0.8%). Pastes compounded with increasing filler-to-resin ratios had progressively decreasing conversion. Correcting for silane unsaturation suggests this effect was independent of whether the filler was silane-treated or not. SIGNIFICANCE Composite resin matrix conversion as determined via FTIR can be underestimated by the presence of unreacted methacrylate from silane on the filler. A corrected resin matrix conversion can be estimated by adjusting for silane unsaturation. Additionally, increasing filler-to-resin ratio progressively decreases conversion independent of the presence of silane on the filler.

The role of etching in bonding to enamel: A comparison of self-etching and etch-and-rinse adhesive systems

OBJECTIVE Etch and resin infiltration morphologies were compared for three self-etch adhesive (SEA) systems and eleven model etch-and-rinse (ERA) systems using various phosphoric acid (PA) concentrations with Adper Single Bond Plus (SB) adhesive. Matches for the morphologies were made between each SEA system and one of the PA/SB systems and bond strength measurements were made for all the systems. The hypothesis was that similar morphology would result in similar bond strength assuming micro-mechanical bonding is the mechanism of adhesion. METHODS Three specimens were prepared on polished (4000 grit) human enamel for each adhesive system to examine etch and resin infiltration morphology by SEM. For the latter, the adhesive systems were bonded using recommended methods and the enamel was dissolved in acid to reveal the resin. The etch patterns for the SEA systems were determined by rinsing off the material with water and acetone. Polished (4000 grit) human enamel was used with each adhesive system to determine 24-h resin composite to enamel shear bond strengths (SBS). A minimum of 10 specimens were used for each group. Data were analyzed by a one factor ANOVA and Fishers PLSD post hoc test. RESULTS The SBS to polished enamel for two of the three SEA systems were statistically significantly greater (p<0.05) than the PA/SB matched systems, indicating that chemical bonding might be partly responsible for the measured bond strength. All three SEA systems provided statistically lower (p<0.05) SBS values than the PA/SB systems with PA concentrations between 2.5% and 40%. SIGNIFICANCE Although chemical bonding may be present for some SEA systems it does not provide enough increase in bond strength to compete with the bond produced by ERA systems using phosphoric acid etching of enamel.

Effect of surface treatments on the bond strength of glass ionomers to enamel.

OBJECTIVES The objective of this study was to evaluate the effect of various surface treatments on the bond strength of several glass ionomers to enamel, and to examine the resulting bond interface. METHODS Ground bovine enamel specimens were divided into groups which were pretreated with one of the following: (1) no pretreatment, (2) Vitremer primer, (3) 10% polyacrylic acid or (4) 35% phosphoric acid. A conventional glass ionomer and two resin-modified glass ionomers (RMGIs) were bonded to the pretreated enamel surfaces, stored in water for 24h and shear bond strengths measured. RMGIs were tested as light-cured and self-cured materials. Transverse sections of similarly prepared samples were etched with phosphoric acid for 60s to partially remove enamel and expose the enamel/glass-ionomer interface. The interface morphology was examined by SEM. RESULTS Polyacrylic acid and phosphoric acid conditioning resulted in significantly increased bond strength to enamel for all three glass ionomer materials, compared to no pretreatment (p<0.01). Light-cured bond strengths were in most cases, significantly greater than when self-cured (p<0.01). Examination of the bonded interfaces revealed the presence of polymer tags in the enamel conditioned with polyacrylic acid and phosphoric acid. SIGNIFICANCE Conditioners significantly improved the bond to enamel for the conventional glass ionomer and RMGIs that were examined in this study. Micromechanical bonding may play a role in the mechanism of bonding glass ionomer to enamel.

Bond strength of self-etch adhesives to pre-etched enamel

OBJECTIVE Bond strengths of composite resin to enamel using four self-etch adhesive (SEA) systems were compared with the bond strength of an etch-and-rinse adhesive (ERA) system, for both polished enamel and enamel pre-etched with phosphoric acid. The objective was to determine if the pre-etching would increase the bond strengths of the SEA systems to match the ERA system. METHODS Ten specimens were used for each adhesive to determine 24-h resin composite to enamel shear bond strengths (SBS) to polished (4000 grit) human enamel and this was repeated for the SEA systems for enamel that was pre-etched with phosphoric acid for 15s. SEM analysis was made to assess the degree of etching and resin penetration into enamel for each of the adhesive systems. Data were analyzed by a two factor ANOVA with a Tukey HSD post hoc test. RESULTS The SBS to polished enamel for all four SEA systems were statistically significantly lower (p<0.05) than the ERA control, but with pre-etched enamel there were no statistically significant differences (p>0.05) between any of the adhesive systems. All four of the SEA systems demonstrated statistically significant increases in bond strength between bonding to polished and pre-etched enamel, ranging from 27% to 86%. The results of SEM analysis showed no differences in the resin penetration patterns of any of the adhesives for enamel that was etched with phosphoric acid. SIGNIFICANCE Pre-etching enamel may enhance the bond strength of SEA systems to values comparable with those found with ERA adhesive systems, which may improve their overall performance in clinical use.

The Influence of Admixing Microfiller to Small-particle Composite Resin on Wear, Tensile Strength, Hardness, and Surface Roughness

A series of photo-initiated composite resins, with a Bis-GMA-TEGDMA resin matrix, was investigated in vitro for occlusal wear, surface roughness, diametral tensile strength, and hardness. The materials contained mixtures of ground quartz (macro filler, 3 μm) and colloidal silica (micro filler, 0. 04μm), with total filler being constant at 68.5% by volume. The study was conducted to determine the influence of an increasing ratio of micro to macrofiller in the mixtures. When the macrofiller was gradually replaced by 3, 5, 7.5, 10, 15, and 20 vol% of microfiller, wear resistance increased substantially, ultimately to a constant level. Any influence on surface roughness or tensile strength and hardness could not be demonstrated.

A fluoride-releasing composite for dental applications.

OBJECTIVES The aim of this work was to attempt formulation of a dental composite, for investigational purposes, which will release fluoride at a rate comparable to glass ionomer materials, while retaining physical properties adequate for potential use in a number of dental applications. METHODS An organic fluoride material, tetrabutylammonium tetrafluoroborate (TBATFB), was incorporated into a hydrophilic monomer system made of 2,2-bis[4-(2-hydroxy-3-methacroyloxypropoxy)phenyl]-propane (BisGMA) and 2-hydroxyethyl methacrylate (HEMA). This fluoride-containing monomer system was filled with silane treated quartz to 81 wt%. The resultant material was tested for fluoride release, physical strength properties and bond strength to enamel, each in comparison to control materials. RESULTS Cumulative fluoride release from the experimental composite was approximately linear over time and comparable to glass ionomer materials. The long term rate of release exceeded several of the glass ionomer materials tested. Diametral tensile strength was comparable to resin-modified glass ionomer (RMGI) materials. Bond strength to etched enamel was statistically equivalent to a commercially available hybrid composite control. SIGNIFICANCE The experimental resin-based composite material could potentially be used as an alternative to glass ionomer materials in non-stress bearing restorative applications and for orthodontic bracket bonding, where high fluoride release is desirable.

Fatigue of enamel bonds with self-etch adhesives

OBJECTIVE Fatigue testing of adhesive bonds to tooth structures in conjunction with bond strength testing can provide more useful information for examining the effectiveness of dental adhesives. The purpose of this study was to determine the shear bond strength (SBS) and shear fatigue limit (SFL) of composite to enamel bonds using modern adhesive systems. METHODS Twelve specimens each were used to determine 24-h resin composite (Z100-3M ESPE) to enamel shear bond strengths with an etch-and-rinse system (ERA), Adper Single Bond Plus (SB), and four self-etch adhesives (SEA)--Adper Prompt-L-Pop (PLP), Clearfil SE (CSE), Clearfil S(3) (CS3) and Xeno IV (X4). A staircase method of fatigue testing was used in a four-station fatigue cycler to determine the SFL of composite to enamel bonds with the adhesives (16-20 specimens for each adhesive) at 0.25 Hz for 40,000 cycles. ANOVA and Tukeys post hoc test were used for the SBS data and a modified t-test with Bonferroni correction was used for comparisons of the SFL. RESULTS The SBS and SFL of the etch-and-rinse system were significantly greater (p<0.05) than those of the four self-etch adhesives. The SBS and SFL of CSE were also significantly greater than for the other three self-etch systems. The ratio of SFL to SBS was highest with the etch-and-rinse system and the ratio became increasing smaller in the same order that the values for SBS decreased with the self-etch systems. SIGNIFICANCE The lower fatigue limits for composite to enamel bonds obtained with the self-etch adhesive systems may indicate that greater enamel margin breakdown will occur with restorations where these systems are used for bonding.

Influence of different etching modes on bond strength and fatigue strength to dentin using universal adhesive systems

OBJECTIVES The purpose of this study was to determine the dentin bonding ability of three new universal adhesive systems under different etching modes using fatigue testing. METHOD Prime & Bond elect [PE] (DENTSPLY Caulk), Scotchbond Universal [SU] (3M ESPE), and All Bond Universal [AU] (Bisco) were used in this study. A conventional single-step self-etch adhesive, Clearfil Bond SE ONE [CS] (Kuraray Noritake Dental) was also included as a control. Shear bond strengths (SBS) and shear fatigue strength (SFS) to human dentin were obtained in the total-etch mode and self-etch modes. For each test condition, 15 specimens were prepared for the SBS and 30 specimens for SFS. SEM was used to examine representative de-bonded specimens, treated dentin surfaces and the resin/dentin interface for each test condition. RESULTS Among the universal adhesives, PE in total-etch mode showed significantly higher SBS and SFS values than in self-etch mode. SU and AU did not show any significant difference in SBS and SFS between the total-etch mode and self-etch mode. However, the single-step self-etch adhesive CS showed significantly lower SBS and SFS values in the etch-and-rinse mode when compared to the self-etch mode. Examining the ratio of SFS/SBS, for PE and AU, the etch-and-rinse mode groups showed higher ratios than the self-etch mode groups. SIGNIFICANCE The influence of different etching modes on dentin bond quality of universal adhesives was dependent on the adhesive material. However, for the universal adhesives, using the total-etch mode did not have a negative impact on dentin bond quality.

Adhesive Bond Strengths to Enamel and Dentin Using Recommended and Extended Treatment Times

This study examined the effect of different enamel and dentin conditioning times on the shear bond strength of a resin composite using etch-and-rinse and self-etch adhesive systems. Shear bond strengths were determined following treatment of flat ground human enamel and dentin surfaces (4000 grit) with 11 adhesive systems: 1) AdheSE One Viva Pen-(ASE), 2) Adper Prompt L-Pop-(PLP), 3) Adper Single Bond Plus-(SBP), 4) Clearfil SE Bond-(CSE), 5) Clearfil S3 Bond-(CS3), 6) OptiBond All-In-One-(OBA), 7) OptiBond Solo Plus-(OBS), 8) Peak SE-(PSE), 9) Xeno IV-(X4), 10) Xeno V-(X5) and 11) XP Bond-(XPB) using recommended treatment times and an extended treatment time of 60 seconds (n = 10/group). Composite (Z100) to enamel and dentin bond strengths (24 hours) were determined using Ultradent fixtures and debonded with a crosshead speed of 1 mm/minute. The data were analyzed with a three-way Analysis of Variance (ANOVA) and Fishers LSD post hoc test. The highest shear bond strengths (MPa) to enamel were achieved by the three etch-and-rinse systems at both the recommended treatment time (SBP-40.5 +/- 6.1; XPB-38.7 +/- 3.7; OBS- 35.2 +/- 6.2) and the extended treatment time (SBP-44.5 +/- 8.1; XPB-40.9 +/- 5.7; OBS-35.0 +/- 4.5). Extending the enamel treatment time did not produce a significant change (p > 0.05) in bond strength for the 11 adhesive systems tested. OBS generated the highest (46.2 +/- 7.9) bond strengths to dentin at the recommended treatment time. At the extended treatment time X4 (42.2 +/- 11.7), PSE (42.1 +/- 9.7) and OBS (41.4 +/- 8.0) produced the highest bond strengths to dentin. The bond strength change between recommend and extended treatment times was significant (p < 0.05) for PSE, but the other 10 systems did not exhibit any significant change.