Influence of Methods of Application of Self-etching Adhesive Systems on Adhesive Bond Strength to Enamel

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of surface conditioning methods on the microtensile bond strength of resin composite to composite after aging conditions

Objectives. This study evaluated the effect of two different surface conditioning methods on the repair bond strength of a bis-GMA-adduct/bis-EMA/TEGDMA based resin composite after three aging conditions.Methods. Thirty-six composite resin blocks (Esthet X, Dentsply) were prepared (5 mm x 6 mm x 6 mm) and randomly assigned into three groups for aging process: (a) immersion in citric acid (pH 3.0 at 37 degrees C, 1 week) (CA); (b) boiling in water for 8h (BW) and (c) thermocycling (x5000, 5-55 degrees C, dwell time: 30s) (TC). After aging, the blocks were assigned to one of the following surface conditioning methods: (1) silica coating (30 mu m SiOx) (CoJet, 3M ESPE) + silane (ESPE-Sil) (CJ), (2) phosphoric acid + adhesive resin (Single Bond, 3M ESPE) (PA). Resin composite (Esthet.X (R)) was bonded to the conditioned substrates incrementally and light polymerized. The experimental groups formed were as follows: Gr1:CA + PA; Gr2:CA + CJ Gr3:BW + PA; Gr4: BW + CJ; Gr5:TC + PA; Gr6: TC + CJ. The specimens were sectioned in two axes (x and y) with a diamond disc under coolant irrigation in order to obtain non-trimmed bar specimens (sticks, 10 mm x 1 mm x 1 mm) with 1 mm(2) of bonding area. The microtensile test was accomplished in a universal testing machine (crosshead speed: 0.5 mm min(-1)).Results. The means and standard deviations of bond strength (MPa +/- S.D.) per group were as follows: Gr1: 25.5 +/- 10.3; Gr2: 46.3 +/- 10.1; Gr3: 21.7 +/- 7.1; Gr4: 52.3 +/- 15.1; GrS: 16.1 +/- 5.1; Gr6, 49.6 +/- 13.5. The silica coated groups showed significantly higher mean bond values after all three aging conditions (p < 0.0001) (two-way ANOVA and Tukey tests, alpha = 0.05). The interaction effect revealed significant influence of TC aging on both silica coated and acid etched groups compared to the other aging methods (p < 0.032). Citric acid was the least aggressive aging medium.Significance. Chairside silica coating and silanization provided higher resin-resin bond strength values compared to acid etching with phosphoric acid followed by adhesive resin applications. Thermocycling the composite substrates resulted in the lowest repair bond strength compared to citric acid challenge or boiling in water. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Microtensile bond strength of a resin cement to feldpathic ceramic after different etching and silanization regimens in dry and aged conditions

Objectives. This study evaluated the durability of bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens with and without silane coupling agent application.Methods. Thirty-two blocks (6.4 mm x 6.4 mm x 4.8 mm) were fabricated using a microparticulate feldspathic ceramic (Vita VM7), ultrasonically cleaned with water for 5 min and randomly divided into four groups, according to the type of etching agent and silanization method: method 1, etching with 10% hydrofluoric (HF) acid gel for I min + silanization; method 2, HF only; method 3, etching with 1.23% acidulated phosphate fluoride (APF) for 5 min + silanization; method 4, APF only. Conditioned blocks were positioned in their individual silicone molds and resin cement (Panavia F) was applied on the treated surfaces. Specimens were stored in distilled water (37 degrees C) for 24 h prior to sectioning. After sectioning the ceramic-cement blocks in x- and Y-axis with a bonded area of approximately 0.6 mm(2), the microsticks of each block were randomly divided into two storage conditions: Dry, immediate testing; TC, thermal cycling (12,000 times) + water storage for 150 d, yielding to eight experimental groups. Microtensile bond strength tests were performed in universal testing machine (cross-head speed: 1 mm/min) and failure types were noted. Data obtained (MPa) were analyzed with three-way ANOVA and Tukey's test (alpha = 0.05).Results. Significant influence of the use of silane (p < 0.0001), storage conditions (p = 0.0013) and surface treatment were observed (p = 0.0014). The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 +/- 5.8 and 17.4 +/- 4.8 MPa, respectively). Silanization after HF acid gel and APT treatment increased the results dramatically (14.5 +/- 4.2-17.4 +/- 4.8 MPa) compared to non-silanized groups (2.6 +/- 0.8-8.9 +/- 3.1 MPa) where the failure type was exclusively (100%) adhesive between the cement and the ceramic.Significance. Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results significantly, with the latter providing higher results. Long-term thermocycling and water storage did not decrease the results in silanized groups. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Estudo da penetração de agentes ácidos para o condicionamento do esmalte dental em cimentos à base de hidróxido de cálcio.

It was verified the penetration of phosphoric acid into 3 commercial calcium hydroxide-based cements (Life, Renew and Prisma VLC Dycal). The colorimetric method employed permitted the identidication of phosphorus amount in representative samples of 6 successive layers 0.1 mm thick of each material. The acid etching used were the commercial products Scotchbond Etching Gel--3M at 36.114% by weight and Solução Condicionadora--Johnson & Johnson at 36.054% by weight. The contact time was 60 seconds. The result showed that layers 0.1 mm tick for Life and Prisma VLC Dycal and 0.2 mm thick for Renew were able to block the penetration of phosphoric acid solution whereas layers 0.1 mm thick for the 3 cements were able to block the penetration of phosphoric acid gel.

Use of one-bottle adhesive as an intermediate bonding layer to reduce sealant microleakage on saliva-contaminated enamel

Purpose: To evaluate the influence of three different adhesives, each used as an intermediary layer, on microleakage of sealants applied under condition of salivary contamination. Materials and Methods: Six different experimental conditions were compared, 3 with adhesives and 3 without. After prophylaxis and acid etching of enamel, salivary contamination was placed for 10 s. In Group SC the sealant was applied after saliva without bonding agent and then light-cured. In Group SCA, after saliva, the surface was air dried, and then the sealant was applied and cured. In Groups ScB, SB and PB, a bonding agent (Scotchbond Dual Cure/3M, Single Bond/3M and Prime & Bond 2.1/Dentsply, respectively) was applied after the saliva and prior to the sealant application and curing. After storage in distilled water at 37°C for 24 hrs, the teeth were submitted to 500 thermal cycles (5°C and 55°C), and silver nitrate was used as a leakage tracer. Leakage data were collected on cross sections as percentage of total enamel-sealant interface length. Representative samples were evaluated under SEM. Results: Sealants placed on contaminated enamel with no bonding agent showed extensive microleakage (94.27% in SC; 42.65% in SCA). The SEM revealed gaps as wide as 20 μm in areas where silver nitrate leakage could be visualized. In contrast, all bonding agent groups showed leakage less than 6.9%. Placement of sealant with a dentin-bonding agent on contaminated enamel significantly reduced microleakage (P< 0.0001). The use of a bonding agent as an intermediary layer between enamel and sealant significantly reduced saliva's effect on sealant microleakage.

Resistance to maxillary premolar fractures after restoration of class II preparations with resin composite or ceromer.

OBJECTIVE: The aim of this study was to evaluate the resistance to fracture of intact and restored human maxillary premolars. METHOD AND MATERIALS: Thirty noncarious human maxillary premolars, divided into three groups of 10, were submitted to mechanical tests to evaluate their resistance to fracture. Group 1 consisted of intact teeth. Teeth in group 2 received mesio-occlusodistal cavity preparations and were restored with direct resin composite restorations. Teeth in group 3 received mesio-occlusodistal cavity preparations and were restored with ceromer inlays placed with the indirect technique. After restoration, teeth were stored at 37 degrees C for 24 hours and then thermocycled for 500 cycles at temperatures of 5 degrees C and 55 degrees C. RESULTS: Statistical analysis revealed that group 3 (178.765 kgf) had a significantly greater maximum rupture load than did group 1 (120.040 kgf). There was no statistically significant difference between groups 1 and 2 or between groups 2 and 3. CONCLUSION: Class II cavity preparations restored with indirect ceromer inlays offered greater resistance to fracture than did intact teeth. The fracture resistance of teeth restored with resin composite was not significantly different from that of either the ceromer or intact teeth.

Effect of 2% chlorhexidine on microtensile bond strength of composite to dentin

Purpose: To evaluate the effect of 2% chlorhexidine on the microtensile bond strength of composite resin to dentin treated with three dentin bonding systems. Materials and Methods: Flat dentinal surfaces were prepared in 24 extracted human third molars. Teeth were randomly divided into 8 distinct experimental groups according to the adhesive applied (Prime & Bond NT, Single Bond and Clearfil SE Bond), the application (yes/no) of chlorhexidine, and the time point at which it was applied (before or after acid etching the dentin). Composite resin blocks were built up over treated surfaces, and teeth were then stored in water at 37°C for 24 h. Samples were thermocycled, stored under the same conditions, and then vertically sectioned, thus obtaining specimens with 1.0 ± 0.1 mm2 cross-sectional area. Specimens were stressed in tension at 0.5 mm/min crosshead speed. Bond strength results were evaluated using a one-way ANOVA (p < 0.05). The modes of failures were verified using optical microscopy. Dentin disks were obtained from 3 additional teeth treated in the same manner for observation under SEM. The most representative samples of fractured specimens were also observed under SEM. Results: No statistically significant differences of bond strength values were found between any groups. Failures occurred mainly within the bond; exclusively adhesive fractures (adhesive-dentin) were not observed. Conclusion: The 2% chlorhexidine solution, applied before or after acid etching of the dentin, did not interfere with the microtensile bond strength of composite resin to the dentin treated with Prime & Bond NT, Single Bond, or Clearfil SE Bond bonding systems.

Effects of dentin collagen removal on microleakage of bonded restorations

Purpose: To evaluate the effects of removing dentin collagen exposed by acid etching on the microleakage of bonded restorations with and without flowable composite application and submitted to thermocycling and long-term water storage. Materials and Methods: Standardized Class V cavities were prepared in 180 bovine incisors. They were randomly assigned to three groups according to the adhesive technique used. Conventional group (C): Single Bond was applied according to the manufacturer's instructions and Z250 composite was placed. Hypochlorite group (H): After acid etching a 10% NaOCl aqueous solution was applied for 1 min, then Single Bond and Z250 were applied. Hypochlorite and Flowable group (HF): Similar to group H, but following adhesive application, a thin layer of Natural Flow flowable composite was applied before the Z250. Each group was divided into three subgroups (0, 6, 12), which remained immersed in distilled water for 24 h or 6 or 12 months and underwent 500, 1500 or 2500 thermal cycles, respectively. At the end of each storage time, the specimes were stained with silver nitrate, decalcified, immersed in methyl salicylate for clearing and observed under a stereomicroscope to determine microleakage (scores 0 to 4). The data were analyzed using the Kruskal-Wallis and the Multiple Comparison Tests (α = 0.05). Results: After 12 months, every group showed significant increases in microleakage. There was no significant difference between Groups H and HF for the three different periods of time, but they showed statistically less microleakage than Group C. Conclusion: The removal of dentinal collagen reduced the marginal microleakage when compared to the conventional technique. The use of the flowable composite did not produce significant effects. No technique was completely effective in preventing microleakage.

Experimental peri-implant tissue breakdown around different dental implant surfaces: Clinical and radiographic evaluation in dogs

Purpose: Tissue reactions to 4 different implant surfaces were evaluated in regard to the development and progression of ligature-induced peri-implantitis. Materials and Methods: In 6 male mongrel dogs, a total of 36 dental implants with different surfaces (9 titanium plasma-sprayed, 9 hydroxyapatite-coated, 9 acid-etched, and 9 commercially pure titanium) were placed 3 months after mandibular premolar extraction. After 3 months with optimal plaque control, abutment connection was performed. Forty-five days later, cotton ligatures were placed around the implants to induce peri-implantitis. At baseline and 20, 40, and 60 days after placement, the presence of plaque, peri-implant mucosal redness, bleeding on probing, probing depth, clinical attachment loss, mobility, vertical bone loss, and horizontal bone loss were assessed. Results: The results did not show significant differences among the surfaces for any parameter during the study (P > .05). All surfaces were equally susceptible to ligature-induced peri-implantitis over time (P < .001). Correlation analysis revealed a statistically significant relationship between width of keratinized tissue and vertical bone loss (r 2 = 0.81; P = .014) and between mobility and vertical bone loss (r 2 = 0.66; P = .04), both for the titanium plasma-sprayed surface. Discussion and Conclusions: The present data suggest that all surfaces were equally susceptible to experimental peri-implantitis after a 60-day period.

The effect of adhesive and flowable composite on postoperative sensitivity: 2-Week results

Objective: To measure 2-week postoperative sensitivity in Class II composite restorations placed with a self-etching adhesive (Clearfil SE Bond) or a total-etch adhesive (Prime&Bond NT) with or without a flowable composite as cervical increment. Method and materials: Upon approval by the University of Guarulhos Committee on Human Subjects, 100 restorations were inserted in 46 patients who required Class II restorations in their molars and premolars. Enamel and dentin walls were conditioned with a self-etching primer (for Clearfil SE Bond) or etched with 34% phosphoric acid (for Prime&Bond NT). A 1- to 2-mm-thick increment of a flowable composite (Filtek Flow) was used in the proximal box in 50% of the restorations of each adhesive. Preparations were restored with a packable composite (Surefil). The restorations were evaluated preoperatively and 2 weeks postoperatively for sensitivity to cold, air, and masticatory forces using a visual analog scale. Marginal integrity of the accessible margins was also evaluated. Statistical analysis used a mixed linear model with subject as a random effect. Results: Ninety-eight teeth from 44 subjects were observed at 2 weeks. The type of adhesive and use of flowable composite had no significant effects or interaction for any of the four outcomes of interest, ie, change from baseline to 2 weeks in sensitivity and response time for the cold or air stimulus. For the air stimulus, the overall average change from baseline was not significant for either sensitivity or response time. For the cold stimulus, the overall average change from baseline was significant for both sensitivity and response time. No case of sensitivity to masticatory forces was observed. Conclusion: No differences in postoperative sensitivity were observed between a self-etch adhesive and a total-etch adhesive at 2 weeks. The use of flowable composite did not decrease postoperative sensitivity.

Efficacy of EDTA-T gel for smear layer removal at root surfaces

Objective: The purpose of this in vitro study was to investigate the efficacy of EDTA gel preparation, associated with texapon detergent (EDTA-T), for removing the smear layer at human root surfaces. Method and materials: An experimental smear layer was produced by scaling using periodontal curettes, and the root surfaces were etched with the following concentrations of EDTA-T: 5%, 10%, 15%, 20%, 24%, and negative control (saline solution) for 1, 2, or 3 minutes using both passive and active methods. The surfaces were evaluated by scanning electron microscopy, and photomicrographs were evaluated in relation to smear removal. Results: All EDTA-T groups were more effective than the control group (P < .0001). EDTA-T at 15% was more effective when applied by the passive method, although this difference was not observed for the active method. The active method was statistically better than the passive method (P < .0001). Conclusion: The etching of the root surface with EDTA-T gel by active application, independently of the other factors evaluated, was effective for smear layer removal.

Histomorphometric evaluation of a threaded, sandblasted, acid-etched implant retrieved from a human lower jaw: A case report

The purpose of this study was to histomorphometrically evaluate the bone-to-implant contact and bone area around a titanium implant retrieved from a human lower jaw. A screw-shaped titanium implant (sandblasted and acid-etched surface) was removed from a 68-year-old male after having been in function for 40 months because of a fracture of the abutment screw. Following the implant removal, an undecalcified section was obtained. The histomorphometric analysis showed a rate of 75.40% of bone-to-implant contact and 89.30% of bone area filling within the limits of the implant threads. The surrounding bone healed in a well-organized pattern and could not be differentiated from the anginal alveolus. The histologic evidence showed a high degree of osseointegration in a threaded, sandblasted, and acid-etched implant retrieved from a human lower jaw after functional loading for 40 months. Copyright © 2005 by Lippincott Williams & Wilkins.

Effect of dentinal surface preparation on bond strength of self-etching adhesive systems

The aim of this study was to evaluate the effects of dentin surface treatments on the tensile bond strength (TBS) of the self-etching primer Clearfil SE Bond (CSE) and the one-step self-etching One-Up Bond F (OUB). The exposed flat dentin surfaces of twenty-four sound third molars were prepared with diamond bur at high-speed, carbide bur at low-speed or wet ground with #600 grit SiC paper. The adhesive systems were applied to the dentin surfaces and light-cured according to the manufacturers' instructions. A 6-mm high composite crown was incrementally built-up and each increment was light-cured for 40 seconds. After being stored in water (37°C/24 h), the samples were serially sectioned parallel to the long axis, forming beams (n = 20) with a cross-sectional area of approximately 0.8 mm 2. The specimens were tested in a Universal Testing Machine at 0.5 mm/min. The cross-sectional area was measured and the results (MPa) were analyzed by two-way ANOVA and Tukey Test (p < 0.05). Overall, the groups treated with CSE exhibited the highest TBS for all surface treatments. Dentin surfaces prepared with carbide bur at low speed reduced TBS in the CSE group; however, OUB was not affected by surface treatments. The effect of surface abrasive methods on TBS was material-dependent.

The effect of temperature on self-etching adhesive penetration.

The purpose of this study was to investigate the penetration of an aggressive self-etching adhesive system at refrigerated and room temperatures into ground and unground enamel surfaces. Thirty extracted human teeth were used to measure adhesive penetration into enamel by light microscopy analysis (x400). The unground enamel surfaces were cleaned with pumice and water using a rotary dental brush. For each specimen, part of the unground enamel was manually ground and part was kept intact. A self-etch adhesive was evaluated for its ability to penetrate ground and unground enamel surfaces at room temperature (25 degrees C), at 30 minutes after removal from the refrigerator, and immediately after removal from the refrigerator (6 degrees C). Data were analyzed using variance and the Tukey test, which revealed significant differences in length of penetration of this material when applied on ground and unground enamel surfaces and between the different temperatures used (P > .05). The self-etching system used in this study had significantly lower penetration into unground enamel and at 6 degrees C (P < .05). No statistical difference was found between the interactions of these factors. It was concluded that the self-etching system produced the best penetration into ground enamel surface at room temperature (25 degrees C) and at 30 minutes after removing the specimens from the refrigerator.

Tensile bond strength of self-etching versus total-etching adhesive systems under different dentinal substrate conditions

The use of acid etchants to produce surface demineralization and collagen network exposure, allowing adhesive monomers interdiffusion and consequently the formation of a hybrid layer, has been considered the most efficient mechanism of dentin bonding. The aim of this study was to compare the tensile bond strength to dentin of three adhesive systems, two self-etching ones (Clearfil SE Bond - CSEB and One Up Bond F - OUBF) and one total-etching one (Single Bond - SB), under three dentinal substrate conditions (wet, dry and re-wet). Ninety human, freshly extracted third molars were sectioned at the occlusal surface to remove enamel and to form a flat dentin wall. The specimens were restored with composite resin (Filtek Z250) and submitted to tensile bond strength testing (TBS) in an MTS 810. The data were submitted to two-way ANOVA and Tukey's test (p = 0.05). Wet dentin presented the highest TBS values for SB and CSEB. Dry dentin and re-wet produced significantly lower TBS values when using SB. OUBF was not affected by the different conditions of the dentin substrate, producing similar TBS values regardless of the surface pretreatments.