The Journal of Adhesive Dentistry, 04/2016

Purpose: To evaluate the bond strength between composite resin and feldspathic ceramic following repair protocols with and without hydrofluoric acid and aging by thermocycling. Materials and Methods: Forty-eight glass feldspathic ceramic blocks (8 x 8 x 6 mm) were divided into three groups on the basis of their surface repair treatment: 1. 10% hydrofluoric acid + Signum Ceramic Primer I + Signum Ceramic Primer II (control group); 2. abrasive rubber tips + Signum Ceramic Primer I + Signum Ceramic Primer II (test group); 3. Signum Ceramic Primer I + Signum Ceramic Primer II (negative control group). The treated surface of each block was built up with composite and then sectioned to produce nontrimmed bars (adhesive area = 1 mm²). Half of the bars from each group were aged by 6000 cycles of 30-s immersions in water baths at 5°C and 55°C, with a transfer time of 2 s. The other bars were immediately subjected to microtensile bond strength testing. The mean bond strength for each block was then recorded and submitted to two-way ANOVA and Tukey's test (α = 0.05). Results: The aging protocol influenced the bond strength values of all groups (p = 0.000). The non-aged groups submitted to surface treatment protocols 1 (13.1 ± 2.5 MPa) and 2 (11.5 ± 5.1 MPa) presented the highest bond strength values. Conclusions: The interface bond strength of all groups was susceptible to aging. Surface treatment protocol 2, with abrasive rubber tips and no hydrofluoric acid, appeared to be the most promising option, as the resulting bond strength values were similar to those of the control group. Keywords: feldspathic repair, glass ceramic, ceramic surface treatment

Purpose: To evaluate the influence of different surface treatments of six novel CAD/CAM materials on the bonding effectiveness of two luting composites. Materials and Methods: Six different CAD/CAM materials were tested: four ceramics - Vita Mark II; IPS Empress CAD and IPS e.max CAD; Celtra Duo - one hybrid ceramic, Vita Enamic, and one composite CAD/CAM block, Lava Ultimate. A total of 60 blocks (10 per material) received various mechanical surface treatments: 1. 600-grit SiC paper; 2. sandblasting with 30-μm Al2O3; 3. tribochemical silica coating (CoJet). Subsequent chemical surface treatments involved either no further treatment (control), HF acid etching (HF), silanization (S, or HF acid etching followed by silanization (HF+S). Two specimens with the same surface treatment were bonded together using two dual-curing luting composites: Clearfil Esthetic Cement (self-etching) or Panavia SA Cement (self-adhesive). After 1 week of water storage, the microtensile bond strength of the sectioned microspecimens was measured and the failure mode was evaluated. Results: The bonding performance of the six CAD/CAM materials was significantly influenced by surface treatment (linear mixed models, p < 0.05). The luting cement had a significant influence on bond strength for Celtra Duo and Lava Ultimate (linear mixed models, p < 0.05). Mechanical surface treatment significantly influenced the bond strength for Celtra Duo (p = 0.0117), IPS e.max CAD (p = 0.0115), and Lava Ultimate (p < 0.0001). Different chemical surface treatments resulted in the highest bond strengths for the six CAD/CAM materials: Vita Mark II and IPS Empress CAD: S, HF+S; Celtra Duo: HF, HF+S; IPS e.max CAD: HF+S; Vita Enamic: HF+S, S. For Lava Ultimate, the highest bond strengths were obtained with HF, S, HF+S. Failure analysis showed a relation between bond strength and failure type: more mixed failures were observed with higher bond strengths. Mainly adhesive failures were noticed if no further surface treatment was done. The percentage of adhesive failures was higher for CAD/CAM materials with higher flexural strength (Celtra Duo, IPS e.max CAD, and Lava Ultimate). Conclusion: The bond strength of luting composites to novel CAD/CAM materials is influenced by surface treatment. For each luting composite, an adhesive cementation protocol can be specified in order to obtain the highest bond to the individual CAD/CAM materials. Keywords: CAD/CAM block, composite cement, microtensile bond strength, surface treatment

Purpose: To determine the influence of aging in artificial saliva compared to distilled water on the dentin microtensile bond strength (μTBS) of different adhesive systems. Materials and Methods: Occlusal enamel and superficial dentin of 42 teeth were removed and roots were sectioned to expose the pulp chamber for connecting the tooth segments to an intrapulpal pressure assembly. According to the tested adhesives, tooth segments were allocated to three groups (n = 14): an etch-and-rinse adhesive (Adper Scotchbond Multi-Purpose, SBMP), a two-step self-etching adhesive (Clearfil SE Bond, CSE), and a singlestep self-etching adhesive (Clearfil S3 Bond, S3). Each adhesive system was applied to the dentin surface according to its manufacturer's instructions, while intrapulpal pressure was simulated. Resin composite (3M ESPE) was built up in two increments of 2 mm each. Each bonded specimen was sectioned to obtain eight sticks (0.8 ± 0.01 mm2). Sticks of each group were divided equally (n = 56) according to the storage solution, either distilled water or artificial saliva. For each storage solution, half of the sticks of each subgroup (n = 28) was stored for 24 h at 37°C and the other half was thermocycled for 10,000 cycles between 5°C and 55°C. Sticks were then subjected to μTBS testing. Data were statistically analyzed using multifactor ANOVA with repeated measures and Bonferroni's post-hoc test (p < 0.05). Student's t-test was used for pairwise comparison. Failure modes were determined for all tested sticks using scanning electron microscopy. Results: The decrease in bond strength of the three adhesives was significantly higher in distilled water than in artificial saliva. The predominant failure modes were adhesive and mixed. Conclusion: The decrease in bond strength was more pronounced for specimens stored in distilled water than in artificial saliva. Keywords: distilled water, artificial saliva, adhesives, dentin bonding, bond strength, storage, microtensile bond strength

Purpose: To evaluate the influence of enamel condition and etching strategy on bond strength of a universal adhesive in primary teeth. Materials and Methods: Thirty-six primary molars were randomly assigned to six groups (n = 6) according to the enamel condition (sound [S] and demineralized [DEM]/cariogenic challenge by pH cycling prior to restorative procedures) and adhesive system (Scotchbond Universal Adhesive [SBU]) used in either etch-and-rinse (ER) or selfetching (SE) mode, with Clearfil SE Bond as the self-etching control. The adhesives were applied to flat enamel surfaces and composite cylinders (0.72 mm2) were built up. After 24-h storage in water, specimens were subjected to the microshear test. Bond strength (MPa) data were analyzed using two-way ANOVA and Tukey's post-hoc tests (α = 0.05). Results: Significant differences were found considering the factors adhesive system (p = 0.003) and enamel condition (p = 0.001). Demineralized enamel negatively affected the bond strength, with μSBS values approximately 50% lower than those obtained for sound enamel. SBU performed better in etch-and-rinse mode, and the bond strength found for SBU applied in self-etching mode was similar to that of CSE. Conclusions: Enamel etching with phosphoric acid improves the bond strength of a universal adhesive system to primary enamel. Demineralized primary enamel results in lower bond strength. Keywords: multimode adhesive, microshear bond strength, enamel, etching strategy

Purpose: This study evaluated the effect of application technique and preparation size on the fracture strength (FS), microtensile bond strength (μTBS) and marginal integrity (MI) of direct resin composite restorations. Materials and Methods: Conservative (5 × 2 × 2 mm) or extended (5 × 4 × 2 mm) preparations below the cementoenamel junction were performed in 140 human maxillary premolars (n = 70 per group). After adhesive application (XP Bond), half of each group was restored with the bulk technique (one 4-mm increment of Surefill SDR Flow plus one 1-mm horizontal capping layer of TPH3 [Spectrum TPH3 resin composite]) and half incrementally (TPH3 in three horizontal incremental layers, 1.5 to 2 mm each), all using a metal matrix band. After storage (24 h at 37°C), the proximal surfaces of each tooth were polished with Sof-Lex disks. For FS measurement, 60 restorations were mounted in a universal testing machine and subjected to a compressive axial load applied parallel to the long axis of the tooth, running at a crosshead speed of 0.5 mm/min. For μTBS testing, 40 teeth were longitudinally sectioned to obtain resin-dentin bonded sticks from the cavity floor (bonded area: 0.8 mm2). Specimens were tested in tension at 0.5 mm/min. The external marginal integrity of both proximal surfaces was analyzed using SEM of epoxy resin replicas. The μTBS, marginal integrity, and fracture resistance data were subjected to two-way ANOVA, and Tukey's post-hoc test was used for pair-wise comparisons (a = 0.05). Results: Fracture resistance, microtensile bond strength, and marginal integrity values were not statistically significantly affected by application technique or preparation size (p = 0.71, p = 0.82, and p = 0.77, respectively). Conclusions: The use of a bulk-fill flowable composite associated with a conventional resin composite as a final capping layer did not jeopardize the fracture strength, bond strength to dentin, or marginal integrity of posterior restorations. Keywords: filling technique, preparation, microtensile bond strength, marginal integrity, fracture strength, direct resin composite restorations

Purpose: To examine whether a difference exists between the in vivo biocompatibility of glass-ionomer cements (GICs) containing chlorhexidine (CHX) in different concentrations. Materials and Methods: Eighty-four male Wistar rats were distributed into 7 groups (n = 12) and received subcutaneous implants of small tubes containing different materials, as follows: Ketac control (K), Ketac-CHX 10% (K10), Ketac-CHX 18% (K18), Resilience control (R), Resilience-CHX 10% (R10), Resilience-CHX 18% (R18), Control (polyethylene). The animals were then sacrificed on post-insertion days 7, 15 and 30, and tissues were examined under an optical microscope for inflammatory infiltrate, edema, necrosis, granulation tissue, multinucleated giant cells, and collagen fibers. The results were statistically analyzed using Kruskal-Wallis and Dunn's tests (p < 0.05). Results: Groups K18 and R18 showed larger areas of intense inflammatory infiltrate, with significant differences between group C and groups K18 and R18 (p = 0.007) at 7 days, and between groups C and K18 (p = 0.017) at 15 days. In terms of tissue repair, groups K18 and R18 demonstrated a lower quantity of collagen fibers with significant differences from group C (p = 0.019) at 7 days, and between group K18 and group C (p = 0.021) at 15 days. Conclusion: The 18% concentration of CHX was shown to have a toxic effect. The 10% concentration of CHX was shown to be suitable for tissue contact. The addition of CHX to the glass-ionomer cements is a highly promising method for obtaining of an antibacterial GIC for use in clinical practice. Keywords: glass-ionomer cements, biocompatible materials, dentistry

Purpose: To evaluate the microshear bond strength (μSBS) of several universal adhesive systems applied on five different indirect restorative materials. Materials and Methods: Five CAD/CAM materials were selected: 1) indirect resin composite (LAV); 2) feldspathic glass ceramic (VTR); 3) leucite-reinforced glass-ceramic (EMP); 4) lithium disilicate ceramic (EMX); 5) yttrium-stabilized zirconium dioxide (CZI). For each material, 15 blocks were cut into 4 rectangular sections (6 × 6 × 6 mm) (n = 60 per group), and processed as recommended by the respective manufacturer. For each indirect material, the following adhesive systems were applied according to the respective manufacturer's instructions: 1) AdheSE Universal [ADU]; 2) All-Bond Universal (ABU); 3) Ambar Universal (AMB); 4) Clearfil Universal (CFU); 5) Futurabond U (FBU); 6) One Coat 7 Universal (OCU); 7) Peak Universal Bond (PUB); 8) Prime&Bond Elect (PBE); 9) Scotchbond Universal Adhesive (SBU); 10) Xeno Select (XEN, negative control). After the application of the adhesive system, cylinder-shaped transparent matrices were filled with a dual-curing resin cement (NX3) and light cured. Specimens were stored in water (37°C for 24 h) and tested in shear mode at 1.0 mm/min (mSBS). The failure pattern and μSBS were statistically evaluated (a = 0.05). Results: LAV, VTR, and EMP showed a greater number of cohesive fractures than EMX and CZI (p < 0.0001). PUB was the only adhesive for which the mean μSBS reached the highest ranking of statistical significance for all five substrates. When each adhesive was compared across the five substrates, 8 out of 10 (ADU, ABU, AMB, CFU, OCU, PUB, PBE, and SBU) reached the statistically highest mean μSBS when applied on CZI. Conclusion: The specific chemical composition of universal adhesives was not the decisive factor in the bond strength values measured for different CAD/CAM indirect materials. There was a wide variability in mean μSBS when different universal adhesives were applied to the several CAD/CAM indirect materials. Most universal adhesives bonded well to air-abraded zirconia. Keywords: resin cement, universal dentin adhesive, CAD/CAM restorative materials, bond strength

Purpose: To evaluate the accelerated fatigue resistance of thick CAD/CAM composite resin overlays luted with three different bonding methods. Materials and Methods: Forty-five sound human second mandibular molars were organized and distributed into three experimental groups. All teeth were restored with a 5-mm-thick CAD/CAM composite resin overlay. Group A: immediate dentin sealing (IDS) with Optibond FL and luted with light-polymerizing composite (Herculite XRV). Group B: IDS with Optibond FL and luted with dual-polymerizing composite (Nexus 3). Group C: direct luting with Optibond FL and dual-polymerizing composite (Nexus 3). Masticatory forces at a frequency of 5 Hz were simulated using closed-loop servo-hydraulics and forces starting with a load of 200 N for 5000 cycles, followed by steps of 400, 600, 800, 1000, 1200 and 1400 N for a maximum of 30,000 cycles. Each step was applied through a flat steel cylinder at a 45-degree angle under submerged conditions. Results: The fatigue test generated one failure in group A, three failures in group B, and no failures in group C. The survival table analysis for the fatigue test did not demonstrate any significant difference between the groups (p = 0.154). The specimens that survived the fatigue test were set up for the load-to-failure test with a limit of 4600 N. The survival table analysis for the load-to-failure test demonstrates an average failure load of 3495.20 N with survival of four specimens in group A, an average failure load of 4103.60 N with survival of six specimens in group B, and an average failure load of 4075.33 N with survival of nine specimens in group C. Pairwise comparisons revealed no significant differences (p < 0.016 after Bonferroni correction). Conclusion: Within the limitations of this in vitro study, it can be concluded that although the dual-polymerizing luting material seems to provide better results under extreme conditions, light-polymerizing luting composites in combination with IDS are not contraindicated with thick restorations. Keywords: CAD/CAM, composite resin, dual-polymerizing, fatigue resistance, immediate dentin sealing, light-polymerizing, overlays

Purpose: To evaluate the effect of chlorhexidine or glutaraldehyde pretreatment on the bonding stability of selfetching and etch-and-rinse adhesives to bleached dentin. Materials and Methods: The occlusal surface of 80 third molars was abraded to expose a flat mid-dentin surface, which was then subjected to a bleaching procedure using 20% hydrogen peroxide and sodium perborate for 14 days. Afterwards, the specimens were kept in distilled water, followed by application of either a three-step etchand- rinse (Adper Scotchbond Multi-Purpose Plus, SBMP) or a two-step self-etching (Clearfil SE Bond, CSE) adhesive system. For each approach, the bleached dentin was treated with chlorhexidine or glutaraldehyde, or left untreated, prior to the adhesive procedure. Unbleached dentin was used as a control. Composite cylinders were built up over the adhesive-covered dentin followed by parallel sectioning of specimens to obtain 1-mm slices. The slices were trimmed to obtain hourglass-shaped specimens with approximately 1.0 mm2 of bonding interface. Half of the specimens were subjected to microtensile bond strength (μTBS) testing after 24 h, while the other half were stored in distilled water for 3 months prior to the μTBS test. The mode of failure was analyzed using optical microscopy. Results: For the SBMP protocol, the highest μTBS was achieved with glutaraldehyde-treated dentin, and the same μTBS values were maintained after 3 months of storage. For the CSE protocol, the highest μTBS was obtained with chlorhexidine-treated dentin. Conclusion: Glutaraldehyde and chlorhexidine pretreatment should be considered to improve the μTBS of adhesives to bleached dentin, while the pretreatment effect was adhesive dependent.

Purpose: To evaluate the effect of cervical margin relocation (CMR) for crowns designed using CAD/CAM technology, and made of pre-cured resin or lithium disilicate, before and after thermomechanical loading. The test hypothesis was that the marginal quality of the crowns would not be influenced by the CMR with composite resins before or after thermomechanical loading. Materials and Methods: Standard crown preparations were created in 40 human molars. The margins were located in enamel, except for the mesial proximal box, where the cervical margin was 2.0 mm below the cementoenamel junction, with 4.0 mm in the buccolingual and 2.0 mm in the mesiodistal dimension. For the CMR technique, a 2-mm layer of conventional or flowable composite resin was applied to the mesial box. Using the Cerec CAD/CAM system, 40 standard crowns were prepared, and restorations were luted using a dual-curing adhesive cement. SEM analysis was performed using epoxy resin replicas before and after loading to assess the marginal quality of interfaces of the mesial proximal box with CMR/crown and the distal face of the tooth without CMR. Statistical differences between groups were analyzed using the Kruskal-Wallis test and Bonferroni's post-hoc test. Results: The null hypothesis was accepted, since no statistically significant differences were found in marginal quality before and after thermomechanical cycling (p > 0.05). Conclusion: The implementation of CMR before and after thermomechanical cycling had no effect on the quality of cervical margins. To establish whether CMR is a suitable procedure for the adhesive luting of composite resin crowns in deep proximal boxes, additional studies are required. Keywords: marginal adaptation, relocation, resin composite, CAD/CAM crown, resin cements, lithium disilicate