The Journal of Adhesive Dentistry, 04/2012

Purpose: To test the hypothesis that stress distribution is more complex than generally assumed during microtensile testing by determining the stress level in the adhesive region of a virtual dentin-adhesive-composite stick using FEA (finite element analysis). Materials and Methods: A 3D FEA model simulating a dentin-adhesive-composite stick was analyzed. The length of the composite and the dentin was 5.0 mm each and the thickness of the adhesive layer was 0.02 mm. For the stress analysis, either only one lateral side of the stick or both end surfaces were attached. A 20-N load was then exerted on the stick with its 1.0 mm2 cross-sectional area, and von Mises stresses were calculated. Results: Large variations in stress levels existed. The highest stresses were located in the dentin and composite sections, near the adhesive interface. The stress level in these regions in the stick attached to one lateral side was more than 5 times higher than the 20 MPa stress calculated by dividing the force with the crosssectional area. For the specimen glued to the ends of the sticks, the stress level differences at the bonded interfaces were around 22 MPa, which decreased to 12 to 14 MPa in the center of the adhesive. Thus, this load condition yielded von Mises stress levels at the interface that were closer to the expected stress level than were the lateral-side attached specimens. Conclusion: The calculated stress levels were higher and more complex than the strength values obtained by dividing the load at failure by the cross-sectional area. Reported strength values from microtensile tests therefore do not represent the true bond strength values at either the dentin/adhesive or adhesive/composite interface. However, the high stress levels in dentin and composite may explain the cohesive failures reported in the literature. Keywords: FEA, von Mises, modulus of elasticity, Poisson's ratio, loading condition

Purpose: Bonding to non-carious cervical lesion (NCCL) sclerotic dentin that involves acid etching continues to be a challenging problem due to its altered chemical structure. In the present study, the objective was to investigate the chemical response of NCCL sclerotic dentin to the different acid etching times. Materials and Methods: Extracted human premolars affected with NCCLs were selected, and a cavity matching the natural lesion with respect to size and location was prepared on the lingual surface of each tooth to serve as the control. The dentin surfaces were treated for 15 s and 30 s using 37% phosphoric acid and then analyzed by Raman microspectroscopic mapping/imaging. Results: NCCL dentin substrates had dramatic effects on the chemical profile of dentin demineralization. The spectral comparison showed that the demineralized layer generated by the acid treatment was highly irregular in terms of depth and mineral component retained, especially when NCCL sclerotic dentin was etched for 15 s. When the etching time was increased to 30 s, the demineralization of NCCL sclerotic dentin was more effective and comparable to the nonsclerotic control that was treated for 15 s. Different etching times affected the depth, degree, and profile of the dentin demineralization. Conclusion: The shorter etching time (ie, 15 s) might not be adequate for NCCL sclerotic dentin. However, the longer etching time (ie, 30 s) would induce much deeper demineralized dentin for nonsclerotic substrates. Thus, although extended etching times can be used to remove the hypermineralized layer, further studies are required to analyze the impact this might have on the dentin bonding. Keywords: Raman spectroscopy, noncarious cervical lesions, sclerotic dentin, acid etching, demineralization

Purpose: To evaluate the influence of fusion sputtering on zirconia-resin microtensile bond strength after 6 months of water storage. Materials and Methods: Zirconia disks received one of the following surface treatments: particle abrasion with 50-µm aluminum oxide particles or fusion sputtering, while as-sintered specimens served as a control. The prepared zirconia disks (Lava Zirconia) were bonded to pre-aged composite disks (Filtek Z250) using a phosphatemonomer- containing resin cement (RelyX Unicem), and the bonded specimens were sectioned into micro-bars (1 x 1 x 6 mm) which were either immediately tested or after 6 months of water storage (n = 25). Scanning electron microscopy (SEM) and surface roughness were performed for the prepared specimens. Data were analyzed using two-way ANOVA (α = 0.05). Results: Particle abrasion (33.1 MPa) and fusion sputtering (42.5 MPa) produced significantly higher MTBS values and resisted degradation after 6 months of water storage, while as-sintered specimens (12.4 MPa) demonstrated a significant reduction in bond strength after water storage (2.9 MPa). SEM examination indicated that fusion sputtering resulted in the creation of retentive zirconia beads on the treated surface, which enhanced micromechanical retention with adhesive resin and prevented interfacial failure. Conclusions: Fusion sputtering is a new and a simple method suitable for enhancing the bond strength of adhesive resins to zirconia-based frameworks. Keywords: fusion sputtering, MTBS, zirconia, SEM

Purpose: To follow the chemical composition of bovine enamel during phosphoric acid-induced demineralization. Materials and Methods: Enamel samples were ground into a fine powder, selecting the 150- and 200-µm fractions in order to obtain a more homogeneous study material. They were immersed in diluted phosphoric acid (0.1%) for increasing durations ranging from 1 to 1440 min. The chemical composition of the solution and enamel powder was determined after each sequential treatment by means of atomic absorption (AA) and Fourier transform infrared (FTIR) spectroscopy. Results: AA data revealed that the amount of calcium mobilized to the solution by the acid treatment was higher at shorter exposure times. However, FTIR data showed that the degree of mineralization of the enamel remained constant during the treatment, indicating that the mineral and organic components were lost at the same rate. Interestingly, poorly crystalline phosphate and carbonate-rich mineral components were preferentially removed and were presumably the main source of calcium released by the acid exposure. FTIR results also demonstrated that organic components rich in hydrophobic groups were preferentially removed during acid treatment. Conclusion: Etching with phosphoric acid produces a nonhomogeneous demineralization of bovine enamel, with the selective removal of poorly crystalline mineral and hydrophobic organic components. Keywords: calcium, demineralization, FTIR, hydroxyapatite, phosphoric acid

Purpose: To evaluate the accuracy of Image Tool Software 3.0 (ITS 3.0) to detect marginal microleakage using the stereomicroscope as the validation criterion and ITS 3.0 as the tool under study. Materials and Methods: Class V cavities were prepared at the cementoenamel junction of 61 bovine incisors, and 53 halves of them were used. Using the stereomicroscope, microleakage was classified dichotomously: presence or absence. Next, ITS 3.0 was used to obtain measurements of the microleakage, so that 0.75 was taken as the cut-off point, and values equal to or greater than 0.75 indicated its presence, while values between 0.00 and 0.75 indicated its absence. Sensitivity and specificity were calculated by point and given as 95% confidence interval (95% CI). Results: The accuracy of the ITS 3.0 was verified with a sensitivity of 0.95 (95% CI: 0.89 to 1.00) and a specificity of 0.92 (95% CI: 0.84 to 0.99). Conclusion: Digital diagnosis of marginal microleakage using ITS 3.0 was sensitive and specific. Keywords: marginal microleakage, diagnosis, validity of tests

Purpose: To evaluate the tensile bond durability and ability of four MMA-based adhesive resins to prevent demineralization along the hybrid layer when exposed to a demineralizing solution. Materials and Methods: A PMMA rod was bonded to human dentin using one of four MMA-based adhesive systems: Super-Bond C&B (SB), SBP-40TX (SBP, experimental), M-Bond (MB), and M-Bond II (MB II). Bonded specimens were sectioned into 0.9 mm x 0.9 mm beams and subjected to microtensile bond strength (µTBS) testing after water storage at 37°C for 24 h or 10,000 thermal cycles. Data were analyzed with two-way ANOVA and Bonferroni's t-test. Fracture mode analysis of the bonding interface was performed using a scanning electron microscope (SEM) and statistically analysed using the chi-square test. To disclose the demineralization inhibition potential through formation of an acid-base resistant zone (ABRZ), the bonded interface was exposed to a demineralizing solution (pH 4.5) for 90 min, and then 5% NaOCl for 20 min. After argon-ion etching, the interfacial ultrastructure was observed using an SEM. Results: µTBS values without thermocycling were not significantly different (p > 0.05) among 4 adhesive resins. After thermocycling, a significant decrease in µTBS was found in MB and MB II (p 0.001), whereas SB and SBP showed no significant change (p > 0.05). Failure modes were significantly different (p 0.05). An ABRZ was seen in SBP, MB, and MB II, while this protective zone was absent in SB. Conclusion: Dentin bonding performance after thermocycling was material dependent in MMA-based adhesive resins. The ABRZ formation was only observed in the self-etching systems. Keywords: MMA-based adhesive resin, microtensile bond strength, acid-base resistant zone

Purpose: To introduce a mapping method to characterize large dentin surfaces using digital microscopy and to discuss the advantages and possible applications of the method. Materials and Methods: Twenty unerupted third molars were sectioned transversally exposing coronal dentin surfaces. The microscopic mosaic method was used to generate a large field image with the resolution necessary to measure characteristics of dentin tubules. The AxioVision 4.7 software was used to control a motorized optical microscope and the process of acquiring approximately 400 small images to generate each dentin mosaic. An image analysis routine measured the number of tubules (NT) and the ratio between the total area of tubules and the area of the mosaic - the area fraction (AF) - of each mosaic. An automatic procedure transformed the mosaic image into a color map, providing a direct visual representation of tubule density through colors. The dentin maps were used for a comparative qualitative analysis of tubule density distribution of each sample. Results: The results for NT (92450 to 196029 tubules/sample) and AF (4.12% to 11.10%) demonstrated a wide variation among dentin samples. The maps confirmed the microstructure variety, also revealing strong local variations in tubule density within each sample. Conclusion: The mapping method was able to perform dentin morphology characterization and is a valuable tool for producing a baseline for dentin adhesion studies. The method could be also useful in determining the real contribution of dentin structures to the final adhesion quality. Keywords: adhesion, digital microscopy, image analysis, dentin map

Purpose: This study evaluated the effect of chlorhexidine (CHX) incorporation into experimental dentin adhesives with different hydrophilicities on the microtensile bond strength (µTBS) to dentin. Materials and Methods: Flat, deep dentin surfaces were prepared from 60 extracted human third molars. Three ethanol-solvated (50 wt% ethanol/50 wt% comonomers) experimental adhesives with varying degrees of hydrophilicity were prepared for the CHX-free groups. For the CHX-containing groups, chlorhexidine diacetate was further added to the ethanol-solvated adhesives to form a concentration of 2.0 wt% CHX. Dentin surfaces were etched with 37% phosphoric acid for 15 s, rinsed and blot dried before bonding. The adhesives were generously applied to dentin with a microbrush for 15 s. A second application of fresh adhesive was made and light cured for 20 s (600 mW/cm2) after solvent evaporation. Composite buildups were made using Filtek Z250 (3M ESPE). The bonded teeth were sectioned into 0.9 mm x 0.9 mm beams and stressed to failure at a crosshead speed of 1 mm/min. Testing was performed 24 h after specimen preparation and 12 months after storage in artificial saliva. The µTBS data were analyzed using three-way ANOVA and Tukey's multiple comparison tests. Fractographic analysis was performed by SEM. Results: Significant differences were observed for the three factors "adhesive hydrophilicity" (p 0.001), "CHX incorporation" (p = 0.001), and "storage time" (p 0.001). Interaction among these three factors was also significant (p 0.001). Incorporation of CHX had no effect on the immediate bond strength of the three experimental adhesives (p > 0.05). After storage in artificial saliva, significant reduction in bond strength was observed in all adhesive groups, except for CHX-containing adhesive I (p 0.001). The µTBS of the CHX-containing experimental adhesive III was significantly higher than the corresponding CHX-free adhesive (p 0.001) after aging. Conclusion: When incorporated into hydrophilic dental adhesives, chlorhexidine can partially reduce the degradation of the resin-dentin bonds. Keywords: chlorhexidine, resin, dentin, longevity, degradation

Purpose: To assess the influence of ozone gas and ozonated water application to prepared cavity and bonded interfaces on the resin/dentin bond strength of two-step etch-and-rinse adhesive systems (Adper Single Bond 2 [SB2] and XP-Bond [XP]). Materials and Methods: Sixty extracted human third molars were sectioned perpendicularly to their long axes to expose flat occlusal dentin surfaces. In experiment 1, dentin was treated with ozone before the bonding procedure, while in experiment 2, ozone was applied to resin/dentin bonded interfaces. In experiment 1, dentin surfaces were treated either with ozone gas (2100 ppm), ozonated water (3.5 ppm), or distilled water for 120 s, and then bonded with SB2 or XP according to manufacturers' instructions. Hybrid composite buildups were incrementally constructed and the teeth were sectioned into resin-dentin sticks (0.8 mm2). In experiment 2, dentin surfaces were first bonded with SB2 or XP, composite buildups were constructed, and bonded sticks obtained. The sticks were treated with ozone as previously described. Bonded sticks were tested under tensile stress at 1 mm/min. Silver nitrate impregnation along the resin/dentin interfaces was also evaluated under SEM. Results: Two-way ANOVA (adhesive and ozone treatment) detected no significant effect for the cross-product interaction and the main factors in the two experiments (p > 0.05), which was confirmed by the photomicrographs. Conclusion: Ozone gas and ozonated water used before the bonding procedure or on resin/dentin bonded interfaces have no deleterious effects on the bond strengths and interfaces. Keywords: ozone, dentin bonding agents, microtensile bond strength, interface integrity, scanning electron microscopy

Purpose: To evaluate the ability of the provisional filling material Cavit-W alone or in combination with different restorative materials to prevent bacterial leakage through simulated access cavities in a resin buildup material. Materials and Methods: LuxaCore resin cylinders were subdivided into 4 experimental groups (n = 30), plus a positive (n = 5) and a negative (n = 30) control group. One bore hole was drilled through each cylinder, except those in the negative control group (G1). The holes were filled with Cavit-W (G2), Cavit-W and Ketac-Molar (glassionomer cement, G3), Cavit-W and LuxaCore bonded with LuxaBond (G4), Cavit-W and LuxaCore (G5), or left empty (G6). Specimens were mounted in a two-chamber leakage setup. The upper chamber was inoculated with E. faecalis. An enterococci-selective broth was used in the lower chamber. Leakage was assessed for 60 days and compared using Fisher's exact test (α 0.05) corrected for multiple testing. Results: Bacteria penetrated specimens in the positive control group within 24 h. All specimens in the negative control group resisted bacterial leakage for 60 days. Twenty-seven specimens in G2, 26 in G3, and 16 specimens in G5 showed bacterial leakage by the end of the experiment. G4 prevented bacterial penetration completely. The statistical comparison revealed significant differences between G4 and all other experimental groups. Conclusion: Under the current conditions, Cavit-W alone or combined with a glass-ionomer cement did not prevent bacterial leakage through a resin buildup material for two months. In contrast, covering Cavit-W with a bonded resin material resulted in a bacteria-tight seal for two months. Keywords: core buildup composite, temporary restoration, bacteria, leakage

Purpose: To assess the microhardness of three resin composites employed in the adhesive luting of indirect composite restorations and examine the influence of the overlay material and thickness as well as the curing time on polymerization rate. Materials and Methods: Three commercially available resin composites were selected: Enamel Plus HRI (Micerium) (ENA), Saremco ELS (Saremco Dental) (SAR), Esthet-X HD (Dentsply/DeTrey) (EST-X). Post-polymerized cylinders of 6 different thicknesses were produced and used as overlays: 2 mm, 3 mm, 3.5 mm, 4 mm, 5 mm, and 6 mm. Two-mm-thick disks were produced and employed as underlays. A standardized amount of composite paste was placed between the underlay and the overlay surfaces which were maintained at a fixed distance of 0.5 mm. Light curing of the luting composite layer was performed through the overlays for 40, 80, or 120 s. For each specimen, the composite to be cured, the cured overlay, and the underlay were made out of the same batch of resin composite. All specimens were assigned to three experimental groups on the basis of the resin composite used, and to subgroups on the basis of the overlay thickness and the curing time, resulting in 54 experimental subgroups (n = 5). Forty-five additional specimens, 15 for each material under investigation, were produced and subjected to 40, 80, or 120 s of light curing using a microscope glass as an overlay; they were assigned to 9 control subgroups (n = 5). Three Vicker's hardness (VH) indentations were performed on each specimen. Means and standard deviations were calculated. Data were statistically analyzed using 3-way ANOVA. Within the same material, VH values lower than 55% of control were not considered acceptable. Results: The used material, the overlay thickness, and the curing time significantly influenced VH values. In the ENA group, acceptable hardness values were achieved with 3.5-mm or thinner overlays after 120 or 80 s curing time (VH 41.75 and 39.32, respectively), and with 2-mm overlays after 40 s (VH 54.13). In the SAR group, acceptable hardness values were only achieved with 2-mm-thick overlays after 120 or 80 s curing time (VH 39.81 and 29.78, respectively). In the EST-X group, acceptable hardness values were only achieved with 3-mm or thinner overlays, after 120 or 80 s curing time (VH 36.20 and 36.03, respectively). Conclusion: Curing time, restoration thickness, and overlay material significantly influenced the microhardness of the tested resin composites employed as luting agents. The clinician should carefully keep these factors under control. Keywords: indirect composite restoration, luting, Vickers hardness

Purpose: This study evaluated and compared bonding characteristics of resin-based luting agents and special ceramic primers to zirconia. Materials and Methods: Disk specimens (n = 242) were fabricated from zirconium dioxide ceramics (Katana) and bonded with four resin-based luting agents without priming. In addition, zirconia was bonded with 7 bondingsystem combinations of three priming agents and three resin-based luting agents. Two of the resin-based luting agents and two ceramic priming agents contain an identical adhesive monomer, 10-methacryloyloxydecyl dihydrogen phosphate (MDP), either in the material itself or in the priming agent. Shear bond strength was determined after 20,000 cycles of thermocycling. The Kruskal-Wallis test was performed for both pre- and post-thermocycling groups to evaluate the difference among primer and luting agent variations. On the basis of the Kruskal-Wallis test, Steel-Dwass multiple comparisons were further performed to compare the difference among four luting agents and seven conbinations of three primers and three luting agents for both pre- and post-thermocycling conditions. Results: Within the four unprimed groups, Clearfil SA Cement (5.8 MPa) and Panavia F 2.0 (6.7 MPa) showed statistically higher post-thermocycling bond strength than the other materials (0.1 MPa) (p 0.05). Among the seven primer/cement combinations, Clearfil Ceramic Primer combined with Clearfil Esthetic Cement exhibited the highest post-thermocycling bond strength (7.5 MPa), followed by two groups primed with Monobond Plus (4.0-4.6 MPa) (p 0.05). Conclusion: Application of resin-based luting and priming agents containing the adhesive monomer MDP provide better bond strength to zirconia than do other systems. Keywords: bonding, phosphate, primer, zirconia