Toshiki Takamizawa

Enamel bonding of single-step self-etch adhesives: Influence of surface energy characteristics

OBJECTIVES This study examined the surface free energy of enamel treated with the single-step self-etching adhesives Bond Force, Clearfil tri-S Bond and G-Bond. METHODS The labial enamel surfaces of bovine mandibular incisors were wet ground with #180-grit, #600-grit and #2000-grit silicon carbide paper. The adhesives were applied to the ground enamel, and then rinsed with acetone and distilled water. The surface free energies were determined by measuring the contact angles of three test liquids placed on the adhesive-treated enamel. The data for each adhesive system were analyzed using analysis of variance and Tukeys honestly significant difference test. RESULTS The surface free energies of the samples treated with the G-Bond and tri-S Bond adhesives increased as the surface roughness decreased. No significant differences in the surface free energy were found for the samples treated with the Bond Force adhesive regardless of the surface roughness. CONCLUSION The results indicated that the surface free energies and their components of the treated enamel surfaces were different among the adhesive systems used.

Effect of Prior Acid Etching on Bonding Durability of Single-Step Adhesives

This study investigated the effect of prior phosphoric acid etching on the enamel bond strength of five single-step self-etch adhesive systems: Absolute, Clearfil tri-S Bond, Fluoro Bond Shake One, G-Bond and One-Up Bond F Plus. Bovine mandibular incisors were mounted in self-curing resin, and the facial surfaces were wet ground with #600 silicon carbide paper. Adhesives were applied to the enamel surfaces with or without prior phosphoric-acid etching and light irradiated. The resin composites were condensed into a mold and light irradiated. In total, 40 specimens were tested per adhesive system with and without prior acid etching and were further divided into two groups: those stored in water at 37 degrees C for 24 hours without cycling and those stored in water at 37 degrees C for 24 hours followed by thermal cycling between 5 degrees C and 55 degrees C with 10,000 repeats. After storage under each set of conditions, the specimens were tested in shear mode at a crosshead speed of 1.0 mm/minute. Two-way analysis of variance, the Students t-test and the Tukey HSD test were used to analyze the data at a significance level of 0.05. For the specimens without prior acid etching, the mean bond strengths to enamel ranged from 11.0 to 14.6 MPa after 24-hour storage in water, while the corresponding values for specimens with prior acid etching ranged from 15.2 to 19.3 MPa. When these specimens were subjected to thermal cycling, the mean bond strengths ranged from 11.3 to 17.0 MPa without prior acid etching and from 12.3 to 23.2 MPa with prior acid etching. The changes in enamel bond strengths differed among the adhesive systems tested. After 24-hour storage in water, the most common failure modes were adhesive failure and mixed failure for specimens with and without prior acid etching, respectively. Thus, through a careful choice of adhesive system, prior acid etching can increase the bond strengths of single-step self-etch adhesive systems.

Effect of Air-drying Time of Single-application Self-etch Adhesives on Dentin Bond Strength

This study examined the effect of air-drying time of adhesives on the dentin bond strength of several single-application self-etch adhesive systems. The adhesive/resin composite combinations used were: Adper Prompt L-Pop/Filtek Z250 (AP), Clearfil Tri-S Bond/Clearfil AP-X (CT), Fluoro Bond Shake One/Beautifil (FB), G-Bond/Gradia Direct (GB) and One-Up Bond F Plus/Palfique Estelite (OF). Bovine mandibular incisors were mounted in self-curing resin and wet ground with #600 SiC to expose labial dentin. Adhesives were applied according to each manufacturers instructions followed by air-drying time for 0 (without air-drying), 5 and 10 seconds. After light irradiation of the adhesives, the resin composites were condensed into a mold (phi4x2 mm) and polymerized. Ten samples per test group were stored in 37 degrees C distilled water for 24 hours; they were then shear tested at a crosshead speed of 1.0 mm/minute. One-way ANOVA followed by Tukeys HSD tests (alpha = 0.05) were done. FE-SEM observations of the resin/dentin interface were also conducted. Dentin bond strength varied with the different air drying times and ranged from 5.8 +/- 2.4 to 13.9 +/- 2.8 MPa for AP, 4.9 +/- 1.5 to 17.1 +/- 2.3 MPa for CT, 7.9 +/- 2.8 to 13.8 +/- 2.4 MPa for FB, 3.7 +/- 1.4 to 13.4 +/- 1.2 MPa for GB and 4.6 +/- 2.1 to 13.7 +/- 2.6 MPa for OF. With longer air drying of adhesives, no significant changes in bond strengths were found for the systems used except for OF. Significantly lower bond strengths were obtained for the 10-second air-drying group for OF. From FE-SEM observations, gaps between the cured adhesive and resin composites were observed for the specimens without the air drying of adhesives except for OF. The data suggests that, with four of the single-application self-etch adhesive systems, air drying is essential to obtain adequate dentin bond strengths, but increased drying time does not significantly influence bond strength. For the other system studied, the bond strength of the non-air dried group was not significantly different from the five second drying time, but prolonged drying was very detrimental to bond strength. For all five of the systems studied, a five-second air-drying time appeared to be appropriate.

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.

Ultrasonic Determination of the Effect of Casein Phosphopeptide-Amorphous Calcium Phosphate Paste on the Demineralization of Bovine Dentin

The purpose of this study was to investigate the demineralization of dentin by measuring changes in the velocity of the sonic longitudinal waves transmitted through this substrate. One group of samples was immersed in demineralization solution for 10 min twice a day and then stored in artificial saliva. Two additional groups of samples were treated with a solution of casein phosphopeptide-amorphous calcium phosphate (CPP-ACP) paste or a placebo paste without CPP-ACP before demineralization and a control group was stored in artificial saliva. The sonic velocity of the demineralized specimens was found to decrease significantly over time. No significant increase in sonic velocity was observed in specimens treated with CPP-ACP, suggesting that CPP-ACP acted to prevent demineralization.

pH changes of self-etching primers mixed with powdered dentine

OBJECTIVES The purpose of this study was to examine the pH changes of self-etching primers mixed with dentine powder. METHODS Four self-etching primer adhesive systems were used: Clearfil SE Bond, Imperva Fluoro Bond, Mac Bond II, and Unifil Bond. Dentine discs obtained from extracted bovine incisors were milled and pulverized into a fine powder. The dentine powder was then mixed with solutions of self-etching primers diluted with distilled water. The pH changes of the primer-dentine powder mixtures were measured by a solid-state pH sensor connected to a pH meter at time points 10, 20, 30, 60, 120, 180, 300, and 600 s after the start of mixing. Data were analyzed by the Tukey HSD test and the Dunnett test at a significance level of 0.05. RESULTS The baseline pH values of the self-etching primers ranged from 1.83 to 2.34, with Mac Bond II exhibiting a significantly lower value than the other three products. After mixing with the dentine powder, the pH values significantly increased, ranging from 6.95 to 7.37 at 600 s after mixing; there were no significant differences in these values among the self-etching primers used. An insoluble precipitate was formed in the case of Clearfil SE Bond, indicating a chemical reaction between the functional monomer and the dentine powder. CONCLUSIONS The dentine has a strong buffering capacity against the acidity of self-etching primers.

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.

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.

Influence of temporary cement contamination on the surface free energy and dentine bond strength of self-adhesive cements

OBJECTIVES The surface free energy and dentine bond strength of self-adhesive cements were examined after the removal of temporary cements. METHODS The labial dentine surfaces of bovine mandibular incisors were wet ground with #600-grit SiC paper. Acrylic resin blocks were luted to the prepared dentine surfaces using HY Bond Temporary Cement Hard (HY), IP Temp Cement (IP), Fuji TEMP (FT) or Freegenol Temporary Cement (TC), and stored for 1 week. After removal of the temporary cements with an ultrasonic tip, the contact angle values of five specimens per test group were determined for the three test liquids, and the surface-energy parameters of the dentine surfaces were calculated. The dentine bond strengths of the self-adhesive cements were measured after removal of the temporary cements in a shear mode at a crosshead speed of 1.0mm/min. The data were subjected to one-way analysis of variance (ANOVA) followed by Tukeys HSD test. RESULTS For all surfaces, the value of the estimated surface tension component γ(S)(d) (dispersion) was relatively constant at 41.7-43.3 mJm(-2). After removal of the temporary cements, the value of the γ(S)(h) (hydrogen-bonding) component decreased, particularly with FT and TC. The dentine bond strength of the self-adhesive cements was significantly higher for those without temporary cement contamination (8.2-10.6 MPa) than for those with temporary cement contamination (4.3-7.1 MPa). CONCLUSIONS The γ(S) values decreased due to the decrease of γ(S)(h) values for the temporary cement-contaminated dentine. Contamination with temporary cements led to lower dentine bond strength. CLINICAL SIGNIFICANCE The presence of temporary cement interferes with the bonding performance of self-adhesive cements to dentine. Care should be taken in the methods of removal of temporary cement when using self-adhesive cements.

Influence of surface treatment of contaminated zirconia on surface free energy and resin cement bonding

Influences of contamination and cleaning methods on the bonding of resin cement to zirconia ceramics were examined. Airborne particle-abraded zirconia (IPS e.max ZirCAD) specimens were contaminated with saliva and cleaned with tap water (SC) or by application of 37% phosphoric acid (PA), Ivoclean (IC), or additional airborne particle abrasion (AB). Specimens without contamination served as controls. After application of Monobond Plus to the surface of the specimens, resin cement was mixed and inserted into a mold. Surface free energies of the specimens were determined by measuring contact angles. Surface treatment and storage conditions significantly influenced bond strength, while there was no significant interaction between the two factors. Surface free energies of the SC and IC groups were significantly lower than those of the other groups. Additional AB of saliva-contaminated zirconia increased the strength of bonding with the resin cement as well as increased surface free energy.