Microtensile bond strengths and scanning electron microscopic evaluation of self-adhesive and self-etch resin cements to intact and etched enamel

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

Effect of delayed start of light-curing on microtensile bond strengths of two adhesives bonded to dentin

The aim of the present study was to evaluate the microtensile bond strength to dentin (ATBS) of two total-etching adhesives applied with delays of 1-30 s for curing. Fifty extracted molar teeth were used. Occlusal enamel was sectioned to expose flat dentin surface, which was further polished with 600-grit paper for smear layer standardization. The specimens were divided into two groups, G1: Single Bond total-etching adhesive (SB), and G2: Prime & Bond NT total-etching adhesive (PB). Each group was further divided into 5 subgroups according to the delayed light-cure initiation after the adhesive systems application (n=5): Subgroup 1s - 1 s; Subgroup 5s -5 s; Subgroup 10s - 10 s; Subgroup 20s - 20 s; Subgroup 30s - 30 s. Composite resin cones 5 mm height and 10 mm in diameter were fabricated. Specimens were stored in distilled water at 37 degrees C for 24 h and sectioned to obtain 1 x 1 mm(2) transversal specimens. Specimens were thermocycled and mu TBS was measured. Data were submitted to two-way ANOVA (AdhesiveXDelay time) and Tukey's test. The level of significance was set at 5%. The results in mean MPa(+/- SD) for interaction between adhesive and delay time were: PB/1s - 23.82 +/- 2.54a; SB/5s - 19.52 +/- 2.67b; PB/5s - 18.56 +/- 3.06bc; SB/1s - 15.49 +/- 2.69cd; SB/20s - 16.33 +/- 2.55d; SB/10s - 13.88 +/- 1.67d; PB/10s - 11.04 +/- 1.28e; PB/30s - 10.89 +/- 1.31e; PB/20s - 10.24 +/- 2.33e; SB/30s - 9.19 +/- 1.91e. It was concluded that light-cure initiation timing of total-etching adhesives interferes negatively with mu TBS to dentin. (C) 2014 Elsevier Ltd. All rights reserved.

Influence of different dentin etching times and concentrations and air-abrasion technique on dentin microtensile bond strength

Purpose: To determine the influence of different dentin treatments on the microtensile bond strengths of adhesive resins to dentin. Methods: Fifteen human molars were ground to 600-grit to obtain flat root-dentin surfaces. Five different dentin treatments were evaluated: Group 1 - 10% phosphoric acid for 30 seconds; Group 2 - 37% phosphoric acid for 15 seconds; Group 3 - air-abrasion for 10 seconds followed by 10% phosphoric acid for 30 seconds; Group 4 - air-abasion for 10 seconds followed by 37% phosphoric acid for 15 seconds. The dental adhesive (OptiBond Solo Plus) was applied according to manufacturer's instructions and followed by composite (Z100) application to provide sufficient bulk for microtensile bond testing. All samples were placed in distilled water for 24 hours at 37degreesC, thermocycled for 500 cycles in distilled water at 10degreesC and 50degreesC, and serially sliced perpendicular to the adhesive surface and subjected to tensile forces (0.5 mm/minute). Additional samples were prepared for SEM to observe the adhesive interface. Results: Group 2 exhibited significantly (P< 0.05) lower bond strength values than all other treatments. The bond strengths of the different conditions were (in MPa): Group 1: 43.0 +/- 16.1; Group 2: 29.2 +/- 8.3; Group 3: 48.1 +/- 14.2; Group 4: 41.0 +/- 9.3. The dentin treated with phosphoric acid 37% for 15 seconds showed the lowest values of microtensile bond strength. The results obtained with Groups 1, 3 and 4 were statistically similar.

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.

THE EFFECT of IMMEDIATE DENTIN SEALING on THE MARGINAL ADAPTATION and BOND STRENGTHS of TOTAL-ETCH and SELF-ETCH ADHESIVES

Statement of problem. Sealing ability and bond strengths of total-etch and self-etch dentin adhesives used for immediate dentin sealing have not been assessed and established.Purpose. The purpose of this study was to determine the effectiveness of immediate dentin sealing (IDS) using total-etch or self-etch dentin adhesives on microleakage and microtensile bond strength.Material and methods. Twenty recently extracted molars were selected, and standard MOD inlay preparations were made with the gingival margins located below the cemento-enamel unction. The teeth were assigned to 4 experimental groups (n=5) according to the indirect composite restoration cementation technique used: (1) immediate dentin sealing with Adper Single Bond (TEBI); (2) conventional adhesive cementation technique using Adper Single Bond (TEAI); (3) immediate dentin sealing using Adper Prompt L-Pop (SEBI); or (4) conventional adhesive cementation technique using Adper Prompt L-Pop (SEAI). The restored teeth were thermal cycled 1,000 times between 5 degrees and 55 degrees C and then immersed in 50% ammoniacal silver nitrate. Three specimens per restoration were evaluated for microleakage, according to predefined scores, and submitted to Friedman's test (alpha-.05). The specimens were then sectioned to obtain 0.8 +/- 0.2-mm-thick sticks (with n ranging from 32 to 57 specimens) and submitted to microtensile bond strength (mu TBS) testing. The obtained data were submitted to 2-way ANOVA test (alpha=.05).Results. None of the experimental groups demonstrated complete elimination of marginal microleakage. There were significant differences in microleakage of the tested adhesives (P>.001). IDS microleakage scores were similar to those obtained using the conventional cementation technique (CCT) for both adhesives. The highest mean bond strengths were obtained with TEBI (51.1 MPa), whereas SEAI showed the lowest mean bond strengths (1.7 MPa). IDS resulted in significantly higher bond strengths than CCT (P<.001).Conclusions. Total-etch and self-etch adhesives have a significant effect on IDS. IDS resulted in high bond strengths for both adhesives; however, the microleakage was similar to that obtained with CCT (J Prosthet Dent 2009;102:1-9)

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)

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.

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).

Effect of seating forces on cement-ceramic adhesion in microtensile bond tests

Objectives: The aim of this study was to evaluate the effect of different seating forces during cementation in cement-ceramic microtensile bond strength (μTBS). Materials and methods: Forty-five blocks (5 × 5 × 4 mm3) of a glass-infiltrated alumina-based ceramic (In-Ceram Alumina) were fabricated according to the manufacturer's instructions and duplicated in resin composite. Ceramic surfaces were polished, cleaned for 10 min in an ultrasonic bath, silica coated using a laboratory type of air abrasion device, and silanized. Each treated ceramic block was then randomly assigned to five groups (n = 9) and cemented to a composite block under five seating forces (10 g, 50 g, 100 g, 500 g, and 750 g) using a dual-cured resin cement (Panavia F). The ceramic-cement-composite assemblies were cut under coolant water to obtain bar specimens (1 mm × 0. 8 mm2). The μTBS tests were performed in a universal testing machine (1 mm/min). The mean bond strengths values were statistically analyzed using one-way ANOVA (α ≤ 0. 05). Results: Different seating forces resulted in no significant difference in the μTBS results ranging between 13. 1 ± 4. 7 and 18. 8 ± 2. 1 MPa (p = 0. 13) and no significant differences among cement thickness. Conclusions: Excessive seating forces during cementation seem not to affect the μTBS results. Clinical relevance: Excessive forces during the seating of single all-ceramic restorations cementation seem to display the same tensile bond strength to the resin cement. © 2012 Springer-Verlag.

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

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

Inlays Made From a Hybrid Material: Adaptation and Bond Strengths

The aim of this study was to evaluate the internal fit, marginal adaptation, and bond strengths of inlays made of computer-aided design/computer-aided manufacturing feldspathic ceramic and polymer-infiltrated ceramic. Twenty molars were randomly selected and prepared to receive inlays that were milled from both materials. Before cementation, internal fit was achieved using the replica technique by molding the internal surface with addition silicone and measuring the cement thicknesses of the pulpal and axial walls. Marginal adaptation was measured on the occlusal and proximal margins of the replica. The inlays were then cemented using resin cement (Panavia F2.0) and subjected to two million thermomechanical cycles in water (200 N load and 3.8-Hz frequency). The restored teeth were then cut into beams, using a lathe, for microtensile testing. The contact angles, marginal integrity, and surface patterns after etching were also observed. Statistical analysis was performed using two-way repeated measures analysis of variance (p<0.05), the Tukey test for internal fit and marginal adaptation, and the Student t-test for bond strength. The failure types (adhesive or cohesive) were classified on each fractured beam. The results showed that the misfit of the pulpal walls (p=0.0002) and the marginal adaptation (p=0.0001) of the feldspathic ceramic were significantly higher when compared to those of the polymer-infiltrated ceramic, while the bond strength values of the former were higher when compared to those of the latter. The contact angle of the polymer-infiltrated ceramic was also higher. In the present study, the hybrid ceramic presented improved internal and marginal adaptation, but the bond strengths were higher for the feldspathic ceramic.

Microtensile bond strength of resin composite to dentin treated with Er:YAG laser of bleached teeth

The objective of this study was to evaluate the influence of Er:YAG laser (lambda = 2.94 mu m) on microtensile bond strength (mu TBS) and superficial morphology of bovine dentin bleached with 16% carbamide peroxide. Forty bovine teeth blocks (7 x 3 x 3 mm(3)) were randomly assigned to four groups: G1- bleaching and Er:YAG irradiation with energy density of 25.56 J/cm(2) (focused mode); G2 - bleaching; G3 - no-bleaching and Er:YAG irradiation (25.56 J/cm(2)); G4 - control, non-treated. G1 and G2 were bleached with 16% carbamide peroxide for 6 h during 21 days. Afterwards, all blocks were abraded with 320 to 600-grit abrasive papers to obtain flat standardized dentin surfaces. G1 and G3 were Er:YAG irradiated. Blocks were immediately restored with 4-mm-high composite resin (Adper Single Bond 2, Z-250-3 M/ESPE). After 24 h, the restored blocks (n = 9) were serially sectioned and trimmed to an hour-glass shape of approximately 1 mm(2) at the bonded interface area, and tested in tension in a universal testing machine (1 mm/ min). Failure mode was determined at a magnification of 100x using a stereomicroscope. One block of each group was selected for scanning electron microscope (SEM) analysis. mu TBS data was analyzed by two-way ANOVA and Tukey test (alpha = 0.05). Mean bond strengths (SD) in MPa were: G1- 32.7 (5.9)(A); G2- 31.1 (6.3)(A); G3- 25.2 (8.3)(B); G4- 36.7 (9.9).(A) Groups with different uppercase letters were significantly different from each other (p < .05). Enamel bleaching procedure did not affect mu TBS values for dentin adhesion. Er:YAG laser irradiation with 25.56 J/cm(2) prior to adhesive procedure of bleached teeth did not affect mu TBS at dentin and promoted a dentin surface with no smear layer and opened dentin tubules observed under SEM. On the other hand, Er:YAG laser irradiation prior to adhesive procedure of non-bleached surface impaired mu TBS compared to the control group.

Shear bond strengths of glass-ionomer cements to sound and to prepared carious dentine

The aim of this study was determine whether bonding of glass-ionomer cements to non-carious dentine differed from that to carious dentine. Five commercial cements were used, namely Fuji IX GP, Fuji IX capsulated, Fuji IX Fast capsulated (all GC, Japan), Ketac-Molar and Ketac-Molar Aplicap (both 3M-ESPE, Germany). Following conditioning of the substrate with 10% poly (acrylic acid) for 10 s, sets of 10 samples of the cements were bonded to prepared teeth that had been removed for orthodontic reasons. The teeth used had either sound dentine or sclerotic dentine. Shear bond strengths were determined following 24 h storage. For the auto-mixed cements, shear bond strength to sound dentine was found not to differ statistically from shear bond strength to sclerotic dentine whereas for hand-mixed cements, shear bond to sound dentine was found to be higher than to carious dentine (to at least p < 0.05). This shows that the chemical effects arising from interactions of glass-ionomer cements with the mineral phase of the tooth are the most important in developing strong bonds, at least in the shorter term.