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.

Surface conditioning of a composite used for inlay/onlay restorations: Effect on mu TBS to resin cement

Purpose: To assess the effect of the composite surface conditioning on the microtensile bond strength of a resin cement to a composite used for inlay/onlay restorations.Materials and Methods: Forty-two blocks (6 x 6 x 4 mm) of a microfilled composite (Vita VMLC) were produced and divided into 3 groups (N = 14) by composite surface conditioning methods: Gr1 - etching with 37% phosphoric acid, washing, drying, silanization; Gr2 - air abrasion with 50-Im Al203 particles, silanization; Gr3 - chairside tribochemiCal silica coating (CoJet System), silanization. Single-Bond (one-step adhesive) was applied on the conditioned surfaces and the two resin blocks treated with the same method were cemented using RelyX ARC (dual-curing resin cement). The specimens were stored for 7 days in water at 37 degrees C and then sectioned to produce nontrimmed beam samples, which were submitted to microtensile bond strength testing (mu TBS). For statistical analysis (one-way ANOVA and Tukey's test, = 0.05), the means of the beam samples from each luted specimen were calculated (n = 7).Results: mu TBS values (MPa) of Gr2 (62.0 +/- 3.9a) and Gr3 (60.5 +/- 7.9a) were statistically similar to each other and higher than Gr1 (38.2 +/- 8.9b). The analysis of the fractured surfaces revealed that all failures occurred at the adhesive zone.Conclusion: Conditioning methods with 50-Im Al203 or tribochemical silica coating allowed bonding between resin and composite that was statistically similar and stronger than conditioning with acid etching.

In vitro biocompatibility of poly(vinylidene fluoride-trifluoroethylene)/barium titanate composite using cultures of human periodontal ligament fibroblasts and keratinocytes

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

Structural study of composites of aerosil fumed silica and tetraethoxysilane-derived sonogels

Composites of aerosil fumed silica and tetraethoxysilane-derived sonogel were prepared by changing the aerosil content between 0 and 30wt% with respect to the silica content in the original tetraethoxysilane (TEOS). The structural characteristics were studied by density and Vickers microhardness measurements and analyzed by means of small-angle X-ray scattering (SAXS). The structure of the composite aerosil/TEOS-derived sonogel can be described as inclusions of the aerosil particles embedded in the matrix of the TEOS-derived sonogel, forming an aerosil/matrix interfacial surface inside the composite. The weakening of the bonding of aerosil/matrix interface, as suggested by the reported decrease in microhardness, increases the fracture toughness of the composite. The additive effect of the aerosil particles on the structure of the sonogel accounts for the increase of the bulk density and reduction of the specific surface of the composite. Some internal structure associated with the microclusters making up the sonogels is apparent from systematic deviations from Porod's law found in the system with small aerosil contents. (c) 2005 Elsevier B.V. All rights reserved.

Composite Resin to Yttria Stabilized Tetragonal Zirconia Polycrystal Bonding: Comparison of Repair Methods

Purpose: The purpose of the current study was to evaluate different approaches for bonding composite to the surface of yttria stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics.Methods: One hundred Y-TZP blocks were embedded in acrylic resin, had the free surface polished, and were randomly divided into 10 groups (n=10). The tested repair approaches included four surface treatments: tribochemical silica coating (TBS), methacryloxydecyldihidrogenphosphate (MDP)-containing primer/silane, sandblasting, and metal/zirconia primer. Alcohol cleaning was used as a "no treatment" control. Surface treatment was followed by the application (or lack thereof) of an MDP-containing resin cement liner. Subsequently, a composite resin was applied to the ceramic surface using a cylindrical mold (4-mm diameter). After aging for 60 days in water storage, including 6000 thermal cycles, the specimens were submitted to a shear test. Analysis of variance and the Tukey test were used for statistical analyses (alpha=0.05).Results: Surface treatment was a statistically significant factor (F=85.42; p<0.0001). The application of the MDP-containing liner had no effect on bond strength (p=0.1017). TBS was the only treatment that had a significantly positive effect on bond strength after aging.Conclusion: Considering the evaluated approaches, TBS seems to be the best surface treatment for Y-TZP composite repairs. The use of an MDP-containing liner between the composite and Y-TZP surfaces is not effective.

On the specific filtration mechanism of a mesoporous silica membrane, prepared with non-connecting parallel pores

We report the singular filtration properties of an ultrafiltration membrane made with mesoporous silica that exhibits cylindrical pores aligned mostly normal to the support. This membrane supported on tubular commercial macroporous alumina supports was prepared by the interfacial growth mechanism between stable silica-surfactant hybrid micelles made of the association of silica oligomers with polyethyleneoxide-based (PEO) surfactants and sodium fluoride, a well-known silica condensation catalyst [Boissière et al., An ultrafiltration membrane made with mesoporous MSU-X silica, Chem. Mater. 15 (2003) 460-463]. It appears that the combined effect of the silica nature of the membrane, whose surface charge can be easily adjusted by changing the pH and the non-connected cylindrical shape of the pores provides a new behavior in the retention properties, as proved by the filtration of polyoxyethylene polymers (PEO) with different molecular weights. Depending on the filtration conditions, a rejection rate of 80% and a steep cut-off at 2000 Da can be obtained or, on the reverse, polymers three times bigger than the pore diameter can diffuse through the membrane. This new filtration mechanism, which opens up new modes of separation modes, is explained in the light of both topology of the porous network and pH-dependent interactions between PEO polymers and silica porous media. © 2004 Elsevier B.V. All rights reserved.

Effect of silica coating on flexural strength of fiber posts

Purpose: Fiber-reinforced composite (FRC) posts can be air-abraded to obtain good attachment to the resin cement. This study tested the effect of silica coating on the flexural strength of carbon, opaque, and translucent quartz FRC posts. Materials and Methods: Six experimental groups of FRC posts (n = 10 per group) were tested, either as received from the manufacturer or after chairside silica coating (30-μm CoJet-Sand). Results: There was no significant difference in the flexural strength of nonconditioned (504 to 525 MPa) and silica-coated (514 to 565 MPa) specimens (P > .05) (analysis of variance). The type of post did have a significant effect on flexural strength (P < .05). Conclusion: Chairside silica coating did not affect the flexural strength of both carbon and quartz FRC posts.

Resin microtensile bond strength to feldspathic ceramic: Hydrofluoric acid etching vs tribochemical silica coating

This study aimed to compare the microtensile bond strength of resin cement to alumina-reinforced feldspathic ceramic submitted to acid etching or chairside tribochemical silica coating. Ten blocks of Vitadur-α were randomly divided into 2 groups according to conditioning method: (1) etching with 9.6% hydrofluoric acid or (2) chairside tribochemical silica coating. Each ceramic block was luted to the corresponding resin composite block with the resin cement (Panavia F). Next, bar specimens were produced for microtensile testing. No significant difference was observed between the 2 experimental groups (Student t test, P> .05). Both surface treatments showed similar microtensile bond strength values.

Bond strength durability of direct and indirect composite systems following surface conditioning for repair

Purpose: This study evaluated the effect of surface conditioning methods and thermocycling on the bond strength between a resin composite and an indirect composite system in order to test the repair bond strength. Materials and Methods: Eighteen blocks (5 x 5 x 4 mm) of indirect resin composite (Sinfony) were fabricated according to the manufacturer's instructions. The specimens were randomly assigned to one of the following two treatment conditions (9 blocks per treatment): (1) 10% hydrofluoric acid (HF) for 90 s (Dentsply) + silanization, (2) silica coating with 30-Ìm SiOx particles (CoJet) + silanization. After surface conditioning, the bonding agent was applied (Adper Single Bond) and light polymerized. The composite resin (W3D Master) was condensed and polymerized incrementally to form a block. Following storage in distilled water at 37°C for 24 h, the indirect composite/resin blocks were sectioned in two axes (x and y) with a diamond disk under coolant irrigation to obtain nontrimmed specimens (sticks) with approximately 0.6 mm2 of bonding area. Twelve specimens were obtained per block (N = 216, n = 108 sticks). The specimens from each repaired block were again randomly divided into 2 groups and tested either after storage in water for 24 h or thermocycling (6000 cycles, 5°C to 55°C). The microtensile bond strength test was performed in a universal testing machine (crosshead speed: 1 mm/min). The mean bond strengths of the specimens of each block were statistically analyzed using two-way ANOVA (α = 0.05). Results: Both surface conditioning (p = 0.0001) and storage conditions (p = 0.0001) had a significant effect on the results. After 24 h water storage, silica coating and silanization (method 2) showed significantly higher bond strength results (46.4 ± 13.8 MPa) than that of hydrofluoric acid etching and silanization (method 1) (35.8 ± 9.7 MPa) (p < 0.001). After thermocycling, no significant difference was found between the mean bond strengths obtained with method 1 (34.1 ± 8.9 MPa) and method 2 (31.9 ± 7.9 MPa) (p > 0.05). Conclusion: Although after 24 h of testing, silica coating and silanization performed significantly better in resin-resin repair bond strength, both HF acid gel and silica coating followed by silanization revealed comparable bond strength results after thermocycling for 6000 times.

Microtensile bond strength of a repair composite to leucite-reinforced feldspathic ceramic

The purpose of this study was to evaluate the microtensile bond strength of a repair composite resin to a leucite-reinforced feldspathic ceramic (Omega 900, VITA) submitted to two surface conditionings methods: 1) etching with hydrofluoric acid + silane application or 2) tribochemical silica coating. The null hypothesis is that both surface treatments can generate similar bond strengths. Ten ceramic blocks (6x6x6 mm) were fabricated and randomly assigned to 2 groups (n=5), according to the conditioning method: G1- 10% hydrofluoric acid application for 2 min plus rinsing and drying, followed by silane application for 30 s; G2- airborne particle abrasion with 30 μm silica oxide particles (CoJet-Sand) for 20 s using a chairside air-abrasion device (CoJet System), followed by silane application for 5 min. Single Bond adhesive system was applied to the surfaces and light cured (40 s). Z-250 composite resin was placed incrementally on the treated ceramic surface to build a 6x6x6 mm block. Bar specimens with an adhesive area of approximately 1 ± 0.1 mm2 were obtained from the composite-ceramic blocks (6 per block and 30 per group) for microtensile testing. No statistically significant difference was observed between G1 (10.19 ± 3.1 MPa) and G2 (10.17 ± 3.1 MPa) (p=0.982) (Student's t test; á = 0.05). The null hypothesis was, therefore, accepted. In conclusion, both surface conditioning methods provided similar microtensile bond strengths between the repair composite resin and the ceramic. Further studies using long-term aging procedures should be conducted.

Surface conditioning of a composite used for inlay/onlay restorations: Effect on μTBS to resin cement

Purpose: To assess the effect of the composite surface conditioning on the microtensile bond strength of a resin cement to a composite used for inlay/onlay restorations. Materials and Methods: Forty-two blocks (6 × 6 × 4 mm) of a microfilled composite (Vita VMLC) were produced and divided into 3 groups (N = 14) by composite surface conditioning methods: Gr1 - etching with 37% phosphoric acid, washing, drying, silanization; Gr2 - air abrasion with 50-l̀m Al2O3 particles, silanization; Gr3 - chairside tribochemical silica coating (CoJet System), silanization. Single-Bond (one-step adhesive) was applied on the conditioned surfaces and the two resin blocks treated with the same method were cemented using RelyX ARC (dual-curing resin cement). The specimens were stored for 7 days in water at 37°C and then sectioned to produce nontrimmed beam samples, which were submitted to microtensile bond strength testing (μTBS). For statistical analysis (one-way ANOVA and Tukey's test, · = 0.05), the means of the beam samples from each luted specimen were calculated (n = 7). Results: μTBS values (MPa) of Gr2 (62.0 ± 3.9a) and Gr3 (60.5 ± 7.9a) were statistically similar to each other and higher than Gr1 (38.2 ± 8.9b). The analysis of the fractured surfaces revealed that all failures occurred at the adhesive zone. Conclusion: Conditioning methods with 50-l̀m Al2O3 or tribochemical silica coating allowed bonding between resin and composite that was statistically similar and stronger than conditioning with acid etching.

Preparo e caracterização de novos compósitos de celulose bacteriana

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Comparison of Physicochemical Surface Conditioning Methods for Adhesion of bis-GMA Resin Cement to Particulate Filler Composite and Surface Characterization

This study compared the effect of physicochemical surface conditioning methods on the adhesion of bis-GMA-based resin cement to particulate filler composite (PFC) used for indirect dental restorations. PFC blocks (N (block)=54, n (block)=9 per group) were polymerized and randomly subjected to one of the following surface conditioning methods: a) No conditioning (Control-C), b) Hydrofluoric acid (HF)etching for 60s (AE60), c) HF for 90s (AE90), d) HF for 120s (AE120), e) HF for 180s (AE180), and f) air-abrasion with 30 mu m silica-coated alumina particles (AB). The conditioned surfaces were silanized with an MPS silane, and an adhesive resin was applied. Resin composite blocks were bonded to PFC using resin cement and photo-polymerized. PFC-cement-resin composite blocks were cut under coolant water to obtain bar specimens (1mmx0.8mm). Microtensile bond strength test (mu TBS)was performed in a universal testing machine (1mm/min). After debonding, failure modes were classified using stereomicroscopy. Surface characterization was performed on a set of separate specimen surfaces using Scanning Electron Microscopy (SEM), X-Ray Dispersive Spectroscopy (XDS), X-Ray Photoelectron Spectroscopy (XPS), and Fourier Transform-Raman Spectroscopy (FT-RS). Mean mu TBS (MPa) of C (35.6 +/- 4.9) was significantly lower than those of other groups (40.2 +/- 5.6-47.4 +/- 6.1) (p<0.05). The highest mu TBS was obtained in Group AB (47.4 +/- 6.1). Prolonged duration of HF etching increased the results (AE180: 41.9 +/- 7), but was not significantly different than that of AB (p>0.05). Failure types were predominantly cohesive in PFC (34 out of 54) followed by cohesive failure in the cement (16 out of 54). Degree of conversion (DC) of the PFC was 63 +/- 10%. SEM analysis showed increased irregularities on PFC surfaces with the increased etching time. Chemical surface analyses with XPS and FT-RS indicated 11-70% silane on the PFC surfaces that contributed to improved bond strength compared to Group C that presented 5% silane, which seemed to be a threshold. Group AB displayed 83% SiO2 and 17% silane on the surfaces.

Effect of Surface Conditioning Modalities on the Repair Bond Strength of Resin Composite to the Zirconia Core / Veneering Ceramic Complex

Purpose: This study evaluated the effect of different surface conditioning protocols on the repair strength of resin composite to the zirconia core / veneering ceramic complex, simulating the clinical chipping phenomenon.Materials and Methods: Forty disk-shaped zirconia core (Lava Zirconia, 3M ESPE) (diameter: 3 mm) specimens were veneered circumferentially with a feldspathic veneering ceramic (VM7, Vita Zahnfabrik) (thickness: 2 mm) using a split metal mold. They were then embedded in autopolymerizing acrylic with the bonding surfaces exposed. Specimens were randomly assigned to one of the following surface conditioning protocols (n = 10 per group): group 1, veneer: 4% hydrofluoric acid (HF) (Porcelain Etch) + core: aluminum trioxide (50-mu m Al2O3) + core + veneer: silane (ESPE-Sil); group 2: core: Al2O3 (50 mu m) + veneer: HF + core + veneer: silane; group 3: veneer: HF + core: 30 mu m aluminum trioxide particles coated with silica (30 mu m SiO2) + core + veneer: silane; group 4: core: 30 mu m SiO2 + veneer: HF + core + veneer: silane. Core and veneer ceramic were conditioned individually but no attempt was made to avoid cross contamination of conditioning, simulating the clinical intraoral repair situation. Adhesive resin (VisioBond) was applied to both the core and the veneer ceramic, and resin composite (Quadrant Posterior) was bonded onto both substrates using polyethylene molds and photopolymerized. After thermocycling (6000 cycles, 5 degrees C-55 degrees C), the specimens were subjected to shear bond testing using a universal testing machine (1 mm/min). Failure modes were identified using an optical microscope, and scanning electron microscope images were obtained. Bond strength data (MPa) were analyzed statistically using the non-parametric Kruskal-Wallis test followed by the Wilcoxon rank-sum test and the Bonferroni Holm correction (alpha = 0.05).Results: Group 3 demonstrated significantly higher values (MPa) (8.6 +/- 2.7) than those of the other groups (3.2 +/- 3.1, 3.2 +/- 3, and 3.1 +/- 3.5 for groups 1, 2, and 4, respectively) (p < 0.001). All groups showed exclusively adhesive failure between the repair resin and the core zirconia. The incidence of cohesive failure in the ceramic was highest in group 3 (8 out of 10) compared to the other groups (0/10, 2/10, and 2/10, in groups 1, 2, and 4, respectively). SEM images showed that air abrasion on the zirconia core only also impinged on the veneering ceramic where the etching pattern was affected.Conclusion: Etching the veneer ceramic with HF gel and silica coating of the zirconia core followed by silanization of both substrates could be advised for the repair of the zirconia core / veneering ceramic complex.

Microtensile Bond Strenh Between Indirect Composite Resin Inlays and Dentin: Effect of Cementation Strategy and Mechanical Aging

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)