Mark A. Latta

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 Enamel Etching Time on Roughness and Bond Strength

The current study examined the effect of different enamel conditioning times on surface roughness and bond strength using an etch-and-rinse system and four self-etch adhesives. Surface roughness (Ra) and composite to enamel shear bond strengths (SBS) were determined following the treatment of flat ground human enamel (4000 grit) with five adhesive systems: (1) Adper Single Bond Plus (SBP), (2) Adper Prompt L-Pop (PLP), (3) Clearfil SE Bond (CSE), (4) Clearfil S3 Bond (CS3) and (5) Xeno IV (X4), using recommended treatment times and an extended treatment time of 60 seconds (n = 10/group). Control groups were also included for Ra (4000 grit surface) and SBS (no enamel treatment and Adper Scotchbond Multi-Purpose Adhesive). For surface roughness measurements, the phosphoric acid conditioner of the SBP etch-and-rinse system was rinsed from the surface with an air-water spray, and the other four self-etch adhesive agents were removed with alternating rinses of water and acetone. A Proscan 2000 non-contact profilometer was used to determine Ra values. Composite (Z100) to enamel bond strengths (24 hours) were determined using Ultradent fixtures and they were debonded with a crosshead speed of 1 mm/minute. The data were analyzed with ANOVA and Fishers LSD post-hoc test. The etch-and- rinse system (SBP) produced the highest Ra (microm) and SBS (MPa) using both the recommended treatment time (0.352 +/- 0.028 microm and 40.5 +/- 6.1 MPa) and the extended treatment time (0.733 +/- 0.122 microm and 44.2 +/- 8.2 MPa). The Ra and SBS of the etch-and-rinse system were significantly greater (p < 0.05) than all the self-etch systems and controls. Increasing the treatment time with phosphoric acid (SBP) and PLP produced greater surface roughness (p < 0.05) but did not result in significantly higher bond strengths (p > 0.05).

Round robin test: Wear of nine dental restorative materials in six different wear simulators - Supplement to the round robin test of 2005

OBJECTIVE The purpose of the present study was to submit the same materials that were tested in the round robin wear test of 2002/2003 to the Alabama wear method. METHODS Nine restorative materials, seven composites (belleGlass, Chromasit, Estenia, Heliomolar, SureFil, Targis, Tetric Ceram) an amalgam (Amalcap) and a ceramic (IPS Empress) have been submitted to the Alabama wear method for localized and generalized wear. The test centre did not know which brand they were testing. Both volumetric and vertical loss had been determined with an optical sensor. After completion of the wear test, the raw data were sent to IVOCLAR for further analysis. The statistical analysis of the data included logarithmic transformation of the data, the calculation of relative ranks of each material within each test centre, measures of agreement between methods, the discrimination power and coefficient of variation of each method as well as measures of the consistency and global performance for each material. RESULTS Relative ranks of the materials varied tremendously between the test centres. When all materials were taken into account and the test methods compared with each other, only ACTA agreed reasonably well with two other methods, i.e. OHSU and ZURICH. On the other hand, MUNICH did not agree with the other methods at all. The ZURICH method showed the lowest discrimination power, ACTA, IVOCLAR and ALABAMA localized the highest. Material-wise, the best global performance was achieved by the leucite reinforced ceramic material Empress, which was clearly ahead of belleGlass, SureFil and Estenia. In contrast, Heliomolar, Tetric Ceram and especially Chromasit demonstrated a poor global performance. The best consistency was achieved by SureFil, Tetric Ceram and Chromasit, whereas the consistency of Amalcap and Heliomolar was poor. When comparing the laboratory data with clinical data, a significant agreement was found for the IVOCLAR and ALABAMA generalized wear method. SIGNIFICANCE As the different wear simulator settings measure different wear mechanisms, it seems reasonable to combine at least two different wear settings to assess the wear resistance of a new material.

Comparison of the wear and flexural characteristics of flowable resin composites for posterior lesions

Abstract Objectives. To determine the localized wear and flexural properties of flowable resin composites for posterior lesions compared with universal resin composites produced by the same manufacturers. Methods. Ten specimens of each of three flowable resins, G-ænial Universal Flo, G-ænial Flo and Clearfil Majesty Flow, and the corresponding resin composite materials, Kalore and Clearfil Majesty Esthetics, were prepared in custom fixtures and subjected to 400,000 wear machine cycles to simulate localized wear. The total maximum depth and volume loss of the wear facets was calculated for each specimen using a profilometer. A three-point bending test was performed to determine the flexural strength, modulus of elasticity and resilience. Values were statistically compared using one-way analysis of variance (ANOVA) followed by Tukeys Honestly Significant Difference (HSD) test. Results. The wear depth ranged from 58.3–126.9 m and the volumetric loss ranged from 0.019–0.049 mm3, with significant differences observed between restorative materials. The wear depth of G-ænial Universal Flo was significantly smaller than those of the other resin composites tested. The flexural strengths and elastic modulus ranged from 90.5–135.1 MPa and from 4.7–7.6 GPa, respectively. A significantly greater flexural strength and higher elastic modulus was found for G-ænial Universal Flo than the other composites. Conclusions. The wear and mechanical properties of the flowable resin composites tested suggested improved performance compared with universal resin composites.

Bond strength of a resin cement to a composite inlay material

Abstract Although resin cements have been effectively bonded to mineralized tooth structures, bonding to a cured composite material has remained a challenge. This study evaluated the shear bond strength of a resin cement bonded to a cured composite inlay material by use of a variety of composite surface treatments: (1) hydrofluoric acid/60 seconds, (2) ammonium bifluoride/60 seconds, (3) resin adhesive, (4) microabrasion with 50 μm aluminum oxide, and (5) microabrasion with 50 μm aluminum oxide and application of a resin adhesive. The resin cement was also bonded to human enamel that was etched with phosphoric acid. Scanning electron microscopy examinations were completed to evaluate the effects of the composite surface treatments. The results indicated that microabrasion of a cured composite enhances bonding of a resin cement. The bond strength of a resin cement to a composite surface that was air abraded with aluminum oxide, with or without the application of a resin adhesive, was higher than surface treatments with hydrofluoric acid or ammonium bifluoride. Scanning electron microscopy indicated that an irregular surface on the composite was created with aluminum oxide air abrasion.

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.

Influence of water storage on fatigue strength of self-etch adhesives

OBJECTIVES The purpose of this study was to determine enamel and dentin bond durability after long-term water storage using self-etch adhesives. METHODS Two single step self-etch adhesives (SU, Scotchbond Universal and GB, G-ӕnial Bond) and a two-step self-etch adhesive (OX, OptiBond XTR) were used. The shear bond strength (SBS) and shear fatigue strength (FS) of the enamel and dentin were obtained with and without phosphoric acid pre-etching prior to application of the adhesives. The specimens were stored in distilled water at 37 °C for 24 h, 6 months, and one year. A staircase method was used to determine the FS using a frequency of 10 Hz for 50,000 cycles or until failure occurred. RESULTS The SBS and FS of enamel bonds were significantly higher with pre-etching, when compared to no pre-etching for the same water storage period. The FS of dentin bonds with pre-etching tended to decrease relative to no pre-etching at the same storage period. For the one year storage period, SU and GB with pre-etching showed significantly lower FS values than the groups without pre-etching. CONCLUSIONS The influence of water storage on FS of the self-etch adhesives was dependent on the adhesive material, storage period and phosphoric acid pre-etching of the bonding site. CLINICAL SIGNIFICANCE Phosphoric acid pre-etching of enamel improves the effectiveness of self-etch adhesive systems. Inadvertent contact of phosphoric acid on dentin appears to reduce the ability of self-etch adhesives to effectively bond resin composite materials.

Fatigue limits of enamel bonds with moist and dry techniques

OBJECTIVE Shear fatigue limit (SFL) testing, coupled with shear bond strength (SBS) measurements can provide valuable information regarding the ability of adhesive systems to bond to mineralized tooth structures. The clinical technique for enamel bonding with adhesive resins has shifted from bonding to a thoroughly dried acid conditioned surface to a moist surface to facilitate dentin bonding. The purpose of this study was to compare the performance of ethanol-containing etch-and-rinse adhesive (ERA) systems on moist and dry enamel by determining the resin composite to enamel SBS and SFL, and examining the relationship of SBS and SFL. METHODS Twelve specimens each were used to determine 24-h resin composite (Z100 - 3M ESPE) to enamel SBS to moist and dry surfaces with two ERA systems, Adper Single Bond Plus (SBP) and OptiBond Solo Plus (OBP). A staircase method of fatigue testing was used in a four-station fatigue cycler to determine the SFL of resin composite to enamel bonds (moist and dry) with the two ERA systems (20 specimens for each test condition) at 0.25Hz 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 SFL. RESULTS The two ERA systems each generated statistically similar SBS (p>0.05) to moist and dry enamel and the SBS of SBP was significantly higher than OBP on dry enamel (p<0.05). The SFL of SBP was significantly greater to dry enamel when compared to moist enamel and there was not a significant difference in the SFL of OBP on dry and moist enamel. There were no significant differences in SFL values between SBP on either moist or dry enamel and OBP on both moist and dry enamel. SIGNIFICANCE Fatigue testing may provide more useful information than SBS tests regarding the performance of dental adhesive systems. The chemical composition, solvents and filler components of ERA systems may influence their ability to develop long-term durable bonds to both moist and dry enamel surfaces.

Effect of Phosphoric Acid Pre-etching on Fatigue Limits of Self-etching Adhesives

The purpose of this study was to use shear bond strength (SBS) and shear fatigue limit (SFL) testing to determine the effect of phosphoric acid pre-etching of enamel and dentin prior to application of self-etch adhesives for bonding resin composite to these substrates. Three self-etch adhesives--1) G- ænial Bond (GC Corporation, Tokyo, Japan); 2) OptiBond XTR (Kerr Corp, Orange, CA, USA); and 3) Scotchbond Universal (3M ESPE Dental Products, St Paul, MN, USA)--were used to bond Z100 Restorative resin composite to enamel and dentin surfaces. A stainless-steel metal ring with an inner diameter of 2.4 mm was used to bond the resin composite to flat-ground (4000 grit) tooth surfaces for determination of both SBS and SFL. Fifteen specimens each were used to determine initial SBS to human enamel/dentin, with and without pre-etching with a 35% phosphoric acid (Ultra-Etch, Ultradent Products Inc, South Jordan, UT, USA) for 15 seconds prior to the application of the adhesives. A staircase method of fatigue testing (25 specimens for each test) was then used to determine the SFL of resin composite bonded to enamel/dentin using a frequency of 10 Hz for 50,000 cycles or until failure occurred. A two-way analysis of variance and Tukey post hoc test were used for analysis of SBS data, and a modified t-test with Bonferroni correction was used for the SFL data. Scanning electron microscopy was used to examine the area of the bonded restorative/tooth interface. For all three adhesive systems, phosphoric acid pre-etching of enamel demonstrated significantly higher (p<0.05) SBS and SFL with pre-etching than it did without pre-etching. The SBS and SFL of dentin bonds decreased with phosphoric acid pre-etching. The SBS and SFL of bonds using phosphoric acid prior to application of self-etching adhesives clearly demonstrated different tendencies between enamel and dentin. The effect of using phosphoric acid, prior to the application of the self-etching adhesives, on SBS and SFL was dependent on the adhesive material and tooth substrate and should be carefully considered in clinical situations.