Keishi Tsubota

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.

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 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.

Bonding Durability of Single-Step Adhesives to Previously Acid-Etched Dentin

This study investigated the effect of phosphoric acid etching on the dentin 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 SiC paper. Adhesives were applied on the prepared dentin surfaces with and without prior phosphoric acid etching and light irradiated. Resin composite was condensed into a mold (ø4x2 mm), light irradiated and stored in water at 37 degrees C. Four groups (n=10) were made per adhesive system: with and without prior acid etching and with and without thermal cycling between 5 degrees C and 55 degrees C for 10,000 cycles. The specimens were tested in a shear mode at a crosshead speed of 1.0 mm/minute. Two-way ANOVA, Student t-test and Tukey HSD test at a level of 0.05 were done. For specimens without prior acid etching, the mean bond strengths to bovine dentin ranged from 12.8 to 17.1 MPa and ranged from 6.7 to 13.3 MPa for specimens with prior acid etching after 24 hours storage in water. When the specimens were subjected to thermal cycling, the mean bond strengths ranged from 10.7 to 24.8 MPa for the specimens without prior acid etching and 4.6 to 13.9 MPa for the specimens with prior acid etching. The changes in dentin bond strength were different among the adhesive systems tested. Failure modes were commonly adhesive failure associated with mixed failure for specimens with prior acid etching. For specimens without prior acid etching, failures in composite and dentin were increased. From the results of this in vitro study, prior acid etching might be not acceptable for increasing the dentin bond strengths of single-step self-etch adhesive systems.

Influence of oxygen inhibition on the surface free‐energy and dentin bond strength of self‐etch adhesives

We compared the surface free-energies and dentin bond strengths of single-step self-etch adhesives with and without an oxygen-inhibited layer. The labial dentin surfaces of bovine mandibular incisors were wet ground with #600-grit silicon carbide paper. The adhesives were applied to the ground dentin, light-irradiated, and the oxygen-inhibited layer was either retained or removed with ethanol. The surface free-energies were determined by measuring the contact angles of three test liquids placed on the cured adhesives. The dentin bond strengths of specimens with and without the oxygen-inhibited layer were measured. For all surfaces, the value of the estimated surface tension component was relatively constant at 35.5-39.8 mJ m(-2) . The value of the , Lewis acid component increased slightly when the oxygen-inhibited layer was removed, whereas that of the , Lewis base component decreased significantly. The bond strengths of the self-etch adhesives were significantly lower in specimens without an oxygen-inhibited layer (13.2-13.6 MPa) than in those with an oxygen-inhibited layer (17.5-18.4 MPa). These results indicate that the presence of an oxygen-inhibited layer in single-step self-etch adhesives with advanced photoinitiators promotes higher dentin bond strength.

Effect of thermal cycling on enamel bond strength of single-step self-etch systems

This study investigated the influence of thermal cycling on the enamel bond strength of single-step self-etch adhesive systems. The systems used were Absolute, Clearfil tri-S Bond, 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 SiC paper. Adhesives were applied on the prepared enamel surfaces and light irradiated according to each manufacturers instructions. Resin composites were condensed into a mold (ø4x2 mm) and light irradiated for 30 seconds. Thirty specimens per adhesive systems were divided into 1 of 3 test groups (n=10) following storage in water at 37 degrees C for 24 hours. The specimens were then stored in 37 degrees C water for 24 hours, followed by thermal cycling 10,000 and 20,000 times between 5 degrees C and 60 degrees C. After each storage condition, the specimens were tested in shear mode at a crosshead speed of 1.0-mm/minute. One-way ANOVAs and Tukey HSD test at a level of 0.05 were conducted. After 24 hours of water storage, the mean enamel bond strengths ranged from 11.3 to 16.9 MPa, and Clearfil tri-S Bond showed significantly higher bond strength. After thermal cycling, the mean bond strengths ranged from 8.3 to 20.7 MPa. The changes in enamel bond strengths were different among the adhesive systems tested. Failure modes after the test were commonly adhesive failure associated with partial cohesive failure adhesive in resin. With a careful choice of adhesive systems, the benefit to using single-step self-etch systems in terms of simplifying the clinical procedure might be acceptable, even after thermal stresses.

pH changes upon mixing of single-step self-etching adhesives with powdered dentin.

PURPOSE Single-step self-etching adhesives have been developed as a bonding material that adheres to the tooth surface. The adhesives contain acidic resin monomers that penetrate the dentin but can be neutralized to stop the reaction. This study aimed to improve understanding of the pH changes that occur when self-etching adhesives are mixed with dentin powder. MATERIALS AND METHODS Dentin disks obtained from extracted bovine incisors were milled and pulverized into a fine powder. The powder was mixed with diluted self-etching adhesives, and pH changes were measured by a solid-state pH sensor connected to a pH meter at various time points after the start of mixing. Data were analyzed by Tukeys Honestly Significant Difference (HSD) test and Dunnetts test at a significance level of 0.05. Precipitates from the adhesive/ dentin powder mixture were observed by scanning electron microscopy (SEM). RESULTS The baseline pH values of the self-etching adhesives ranged from 0.97 to 2.83. After mixing with the dentin powder, the pH values significantly increased, ranging from 6.30 to 7.11 at 180 s after mixing. SEM observation revealed products of the reaction between dentin powder and self-etching adhesive which indicate a chemical reaction between the functional monomer and dentin. CONCLUSION Dentin has a strong modulation effect against the acidity of self-etching adhesives.

Influence of Delayed Placement of Composites Over Cured Adhesives on Dentin Bond Strength of Single-application Self-etch Systems

This study examined the relationship between delay in composite placement over cured adhesives and the dentin bond strength of several single-application self-etch adhesive systems. The adhesive system/resin composite combinations used were: Adper Prompt L-Pop/Filtek Z250 (AP), AQ Bond Plus/Metafil C (AQ), Fluoro Bond Shake One/Beautifil (FB), G-Bond/Solare (GB), One-Up Bond F Plus/Palfique Estelite (OF), Xeno IICF Bond/Xeno CF (XE). Bovine mandibular incisors were mounted in self-curing resin and wet ground with #600 SiC to expose labial dentin. The adhesives were applied according to each manufacturers instructions, and resin pastes were condensed into a mold (ø4x2 mm) immediately, and 1, 2, 5 and 10 minutes after light irradiation of the adhesives. Ten samples per test group were stored in 37 degrees C water for 24 hours, then shear tested at a crosshead speed of 1.0 mm/minute. One-way ANOVA followed by Tukeys HSD test (alpha = 0.05) was done. SEM observations of the dentin surface after the tests were also conducted. Dentin bond strength ranged from 9.5 +/- 2.2 to 14.0 +/- 2.4 MPa for AP, 7.3 +/- 2.2 to 12.2 +/- 3.1 MPa for AQ, 10.0 +/- 3.5 to 16.3 +/- 2.4 MPa for FB, 11.4 +/- 1.5 to 16.3 +/- 1.2 MPa for GB, 14.2 +/- 3.4 to 15.1 +/- 3.0 MPa for OF and 11.5 +/- 2.4 to 15.9 +/- 2.2 MPa for XE. Except for OF, no significant differences were found among the 2 to 10 minute delayed placement groups for the systems used. Significant lower bond strengths were obtained for the immediate placement groups except for OF. From SEM observations, cohesive failure of the dentin surface was more pronounced with the longer delay in placement. The data suggest that delayed composite placement over the cured adhesives are suggested for optimum dentin bond strength of single-application self-etch adhesive systems.