INFLUENCE of DIFFERENT SURFACE CONDITIONING PROTOCOLS on MICROTENSILE BOND STRENGTH of SELF-ADHESIVE RESIN CEMENTS TO DENTIN

Statement of problem. According to manufacturers, bonding with self-adhesive resin cements can be achieved without any pretreatment steps such as etching, priming, or bonding. However, the benefit of saving time with these simplified luting systems may be realized at the expense of compromising the bonding capacity.Purpose. The purpose of this study was to assess whether different dentin conditioning protocols influence the bond performance of self-adhesive resin cements to dentin.Material and methods. Flat dentin surfaces from 48 human molars were divided into 4 groups (n=12): 1) control, no conditioning; 2) H(3)PO(4), etching with 37% H(3)PO(4) for 15 seconds; 3) SEBond, bonding with self-etching primer adhesive (Clearfil SE Bond); and 4) EDTA, etching with 0.1M EDTA for 60 seconds. The specimens from each dentin pre-treatment were bonded using the self-adhesive cements RelyX Unicem, Maxcem or Multilink Sprint (n=4). The resin-cement-dentin specimens were stored in water at 37 degrees C for 7 days, and serially sectioned to produce beam specimens of 1.0 mm(2) cross-sectional area. Microtensile bond strength (mu TBS) testing was performed at 1.0 mm/min. Data (MPa) were analyzed by 2-way ANOVA and Tukey multiple comparisons test (alpha=.05). Fractured specimens were examined with a stereomicroscope (x40) and classified as adhesive, mixed, or cohesive. Additional bonded interfaces were evaluated under a scanning electron microscope (SEM).Results. Cement-dentin mu TBS was affected by the dentin conditioning approach (P <.001). RelyX Unicem attained statistically similar bond strengths to all pre-treated dentin surfaces. H(3)PO(4)-etching prior to the application of Maxcem resulted in bond strength values that were significantly higher than the other groups. The lowest mu TBS were attained when luting Multilink Sprint per manufacturers' recommendations, while H(3)PO(4)-etching produced the highest values followed by Clearfil SE bonding and EDTA. SEM observations disclosed an enhanced potential of the self-adhesive cements to form a hybrid layer when applied following manufacturer's instructions.Conclusions. When evaluated self-adhesive resin cements are used, selectively etching dentin with H(3)PO(4) prior to luting results in the most effective bonding. (J Prosthet Dent 2011;105:227-235)

Resin Bonding to a Feldspar Ceramic After Different Ceramic Surface Conditioning Methods: Evaluation of Contact Angle, Surface pH, and Microtensile Bond Strength Durability

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

Effect of Acid Neutralization and Mechanical Cycling on the Microtensile Bond Strength of Glass-ceramic Inlays

Objectives: To evaluate the hypothesis that a process of hydrofluoric acid precipitate neutralization and fatigue load cycling performed on human premolars restored with ceramic inlays had an influence on microtensile bond strength results (MTBS). Methods: MOD inlay preparations were performed in 40 premolars (with their roots embedded in acrylic resin). Forty ceramic restorations were prepared using glass-ceramic (IPS Empress). The inner surfaces of all the restorations were etched with 10% hydrofluoric acid for 60 seconds, rinsed with water and dried. The specimens were divided into two groups (N=20): 1-without neutralization; 2-with neutralization. All the restorations were silanized and adhesively cemented (self-curing and self-etching luting composite system, Multilink). Ten premolars from each group were submitted to mechanical cycling (1,400,000 cycles, 50N, 37 degrees C). After cycling, the samples were sectioned to produce non-trimmed beam specimens (vestibular dentin-restoration-lingual dentin set), which were submitted to microtensile testing. Results: Bond strength was significantly affected by the surface treatment (p<0.0001) (no neutralization > neutralization) and mechanical cycling (p<0.0001) (control > cycling) (2-way ANOVA and Tukey test, alpha=.05). Conclusion: Hydrofluoric acid precipitate neutralization appears to significantly damage the resin bond to glass-ceramic and should not be recommended. The clinical simulation of the specimens, by using mechanical cycling, is important when evaluating the ceramic-dentin bond.

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.

Effect of ceramic surface treatment on the microtensile bond strength between a resin cement and an alumina-based ceramic

Purpose: The objective of this study was to test the following hypothesis: the silica coating on ceramic surface increases the bond strength of resin cement to a ceramic. Materials and Methods: In-Ceram Alumina blocks were made and the ceramic surface was treated: G1 - sandblasting with 110-μm aluminum oxide particles; G2 - Rocatec System: tribochemicai silica coating (Rocatec-Pre powder + Rocatec-Plus powder + Rocatec-Sil); G3 - CoJet System: silica coating (CoJet-Sand) + ESPE-Sil. The ceramic blocks were cemented to composite blocks with Panavia F resin cement (under a load of 750 g/1 min). The cemented blocks were stored in distilled water at 37°C for 7 days and sectioned along the x and y axes with a diamond disk. Samples with an adhesive area of ca 0.8 mm 2 (n = 45) were obtained. The samples were attached to an adapted device for the microtensile test, which was performed in a universal testing machine (EMIC) at a crosshead speed of 1 mm/min. Results: The obtained results were submitted to ANOVA and Tukey's test. Mean values of tensile strength (MPa) and standard deviation values were: (G1) 16.8 ± 3.2; (G2) 30.6 ± 4.5; (G3) 33.0 ± 5.0. G2 and 63 presented greater tensile strength than G1. There was no significant difference between G2 and G3. All the failures took place at the ceramic/resin cement interface. Conclusion: The silica coating (Rocatec or CoJet systems) of the ceramic surface increased the bond strength between the Panavia F resin cement and alumina-based ceramic.

Microtensile bond strength of a resin cement to glass infiltrated zirconia-reinforced ceramic: The effect of surface conditioning

This study evaluated the effect of three surface conditioning methods on the microtensile bond strength of resin cement to a glass-infiltrated zirconia-reinforced alumina-based core ceramic. Thirty blocks (5×5×4 mm) of In-Ceram Zirconia ceramics (In-Ceram Zirconia-INC-ZR, VITA) were fabricated according to the manufacturer's instructions and duplicated in resin composite. The specimens were polished and assigned to one of the following three treatment conditions (n=10): (1) Airborne particle abrasion with 110 μm Al2O3 particles + silanization, (2) Silica coating with 110 μm SiOx particles (Rocatec Pre and Plus, 3M ESPE) + silanization, (3) Silica coating with 30 μm SiOx particles (CoJet, 3M ESPE) + silanization. The ceramic-composite blocks were cemented with the resin cement (Panavia F) and stored at 37 °C in distilled water for 7 days prior to bond tests. The blocks were cut under coolant water to produce bar specimens with a bonding area of approximately 0.6 mm2. The bond strength tests were performed in a universal testing machine (cross-head speed: 1 mm/min). The mean bond strengths of the specimens of each block were statistically analyzed using ANOVA and Tukey's test (α≤0.05). Silica coating with silanization either using 110 μm SiOx or 30 μm SiOx particles increased the bond strength of the resin cement (24.6±2.7 MPa and 26.7±2.4 MPa, respectively) to the zirconia-based ceramic significantly compared to that of airborne particle abrasion with 110-μm Al2O3 (20.5±3.8 MPa) (ANOVA, P<0.05). Conditioning the INC-ZR ceramic surfaces with silica coating and silanization using either chairside or laboratory devices provided higher bond strengths of the resin cement than with airborne particle abrasion using 110 μm Al2O3. © 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Microtensile bond strength between a quartz fiber post and a resin cement: Effect of post surface conditioning

Purpose: To test the bond strength between a quartz-fiber-reinforced composite post (FRC) and a resin cement. The null hypothesis was that the bond strength can be increased by using a chairside tribochemical silica-coating system. Materials and Methods: Thirty quartz-FRCs (Light-Post) were divided into 3 groups according to the post surface treatment: G1) Conditioning with 32% phosphoric acid (1 min), applying a silane coupling agent; G2) etching with 10% hydrofluoric acid (1 min), silane application; G3) chairside tribochemical silica coating method (CoJet System): air abrasion with 30-μ SiO x-modified Al2O3 particles, silane application. Thereafter, the posts were cemented into a cylinder (5 mm diameter, 15 mm height) with a resin cement (Duo-Link). After cementation, the specimens were stored in distilled water (37°C/24 h) and sectioned along the x and y axes with a diamond wheel under cooling (Lab-cut 1010) to create nontrimmed bar specimens. Each specimen was attached with cyanoacrylate to an apparatus adapted for the microtensile test. Microtensile testing was conducted on a universal testing machine (1 mm/min). The data obtained were submitted to the one-way ANOVA and Tukey test (α = 0.05). Results: A significant influence of the conditioning methods was observed (p < 0.0001). The bond strength of G3 (15.14 ± 3.3) was significantly higher than the bond strengths of G1 (6.9 ± 2.3) and G2 (12.60 ± 2.8) (p = 0.000106 and p = 0.002631, respectively). Notwithstanding the groups, all the tested specimens showed adhesive failure between the resin cement and FRC. Conclusion: The chairside tribochemical system yielded the highest bond strength between resin cement and quartz-fiber post. The null hypothesis was accepted (p < 0.0001).

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.

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.

Analysis of hybrid layer thickness, resin tag length and their correlation with microtensile bond strength using a total etch adhesive to intact dentin.

The objective of this study was to evaluate the use of a two-step total etch and rinse adhesive, the correlation between the hyybrid layer thickness (HL) and bond strength (BS), and between resin tag length (RT) and bond strength in the same teeth, and also to evaluate the fracture patterns of the tested specimens. Ten human molars were used for the restorative procedure and then sectioned in two halves (mesio-distally). The materials used were Adper Single Bond 2, 3M ESPE, Ultra etch gel, Ultradent and Filtek Z250, 3M ESPE. One half were utilized to measure the HL thickness and RT length through light microscopy analysis (400x), and the other half was subject to a microtensile test to measure the BS. The fractured surfaces were analyzed by scanning electron microscopy and fracture patterns classified. The Pearson correlation test was applied (p = 0.05). The results of the analyses of each specimen then were correlated: mean HL thickness = 4.39 (0.48) microm, mean length of RT = 9.94 (1.69) microm, mean BS = 23.98 (10.24) MPa. A statistically significant correlation between HL thickness and bond strength was found (r = 0.93). The two step etch and rinse adhesive system, showed a strong correlation between HL thickness and bond strength. The most common fractures were adhesive, followed by cohesive in resin.

Correlation between hybrid layer thickness, resin tag length and microtensile bond strength of a self-etching adhesive system

The purpose of this study was to evaluate the correlation between the hybrid layer thickness, resin tag length and resin bond strength of a self-etching adhesive system to sound dentin tissue in vivo. After performing restorative procedures and tooth extractions, ten specimens were sectioned in a mesiodistal direction. One dental section was used for light microscope analysis, in which both the resin tag length and hybrid layer thickness were measured, while the other section was analyzed using a microtensile test (0.5 mm/min). The fractured surface of the latter section was characterized using a stereoscopic magnifying glass (40x magnifcation). The results were subject to statistical analysis using the Pearson Correlation Test (a = 0.05). The hybrid layer thickness, resin tag length and resin bond strength mean values were 2.19 microm (0.34), 4.34 microm (0.28) and 9.73 MPa (5,55), respectively. In addition, correlation tests between the resin tag length and the resin bond strength (r=0.014) and also between the hybrid layer thickness and bond strength (r=0.43), showed no statistically significant correlation. The microtensile bond strength of Adper Prompt L Pop self-etching adhesive system does not depend on hybrid layer thickness or resin tag length.

Microtensile bond strength of resin cements to caries-affected dentin

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

Effect of the Etching Duration and Ultrasonic Cleaning on Microtensile Bond Strength Between Feldspathic Ceramic and Resin Cement

This study assessed the effect of different etching durations of feldspathic ceramic with hydrofluoric acid (HF) and ultrasonic cleaning of the etched ceramic surface on the microtensile bond strength stability of resin to a feldspathic ceramic. The research hypotheses investigated were: (1) different etching times would not affect the adhesion resistance and (2) ultrasonic cleaning would improve the adhesion. Ceramic blocks (6 x 6 x 5 mm) (N = 48) were obtained. The cementations surfaces were duplicated in resin composite. The six study groups (n = 8) were: G1Etching with 10% aqueous HF (30 s) + silane; G 210% HF (1 min) + silane; G3-10% HF (2 min) + silane; G4-10% HF (30 s) + ultrasonic cleaning (4 min) in distilled water + silane; G5-10% HF (1 min) + ultrasonic cleaning + silane; G6-10% HF (2 min) ultrasonic cleaning + silane. The cemented blocks were sectioned into microbars for the microtensile test. The etching duration did not create significant difference among the groups (p = .156) but significant influence of ultrasonic cleaning was observed (p = .001) (Two-way ANOVA and Tukey's test, p > 0.05). All the groups after ultrasonic cleaning presented higher bond strength (19.38-20.08 MPa) when compared with the groups without ultrasonic cleaning (16.2117.75 MPa). The bond strength between feldspathic ceramic and resin cement was not affected by different etching durations using HF. Ultrasonic cleaning increased the bond strength between ceramic surface and resin cement, regardless of the etching duration.

Zirconia-Porcelain Bonding: Effect of Multiple Firings on Microtensile Bond Strength

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