An investigation of atomic force microscopy,surface topography and adhesion of luting cements to zirconia: effect of silica coating,zirconia primer and laser

This study evaluated the effect various surface conditioning methods on the surface topography and adhesion of luting cements to zirconia. Zirconia blocks (N?=?25) were randomly assigned to five groups according to the surface conditioning methods: (a) No conditioning, control (CON), (b) tribochemical silica coating (TSC), (c) MDP-based zirconia primer (ZRP), (d) coating with nano aluminum nitride (ALN) (e) etching with Er: YAG laser (LAS). The conditioned zirconia blocks were further divided into five subgroups to receive the luting cements: (a) MDP-based resin cement (Panavia F2.0) (PAN), (b) 4-META-based cement (Super Bond) (SUB), (c) UDMA-based (GCem) (GCE), (d) bis-GMA based (Bifix QM) (BIF) and (e) polycarboxylate cement (Poly-F) (POL). Cements were applied in polyethylene moulds (diameter: 3?mm; height: 2?mm). The bonded specimens were first thermocycled for 5500 cycles (5–55?°C) and then adhesive interface was loaded under shear (0.5?mm/min). The data (MPa) were analyzed using 2-way ANOVA, Tukey’s and Bonneferroni tests (alpha?=?0.05). Regardless of the cement type, TSC resulted in significantly higher bond strength (p???0.05) (13.3?±?4.35–25.3?±?6.3) compared to other conditioning methods (2.96?±?1.5–5.4?±?5.47). Regardless of the surface conditioning method, no significant difference was found between MDP, 4-META and UDMA based cements (p?>?0.05) being significantly higher than those of bis-GMA and polycarboxylate cements (p???0.05). Failure types were frequently adhesive in all groups. Tribochemical silica coating provided superior bond results compared to other conditioning methods tested on zirconia especially in conjunction with UDMA- and 4-META-based resin cements.     

Effects of different particle deposition parameters on adhesion of resin cement to zirconium dioxide and phase transformation

This study evaluated the effect of air-abrasion parameters such as particle size, distance, and time on adhesion of resin cement to zirconium dioxide (Y-TZP) and t→m phase transformation. Y-TZP blocks (N = 80) (In-Ceram YZ, Vita) (4 mm^3?×?4 mm^3?×?3 mm³) were assigned into eight groups (n = 10): air-abrasion with 30 μm (CoJet Sand, S30) and 110 μm (Rocatec-Plus, S110) silica-coated alumina particles, applied for either for 10–20 s (T = time), from a distance of 10–20 mm (D = distance), composing the following groups: S₃₀T₁₀D₁₀, S₃₀T₁₀D₂₀, S₃₀T₂₀D₁₀, S₃₀T₂₀D₂₀, S₁₁₀T₁₀D₁₀, S₁₁₀T₁₀D₂₀, S₁₁₀T₂₀D₁₀, and S₁₁₀T₂₀D₂₀. Resin composite (RelyX ARC) was bonded to Y-TZP blocks in polyethylene molds. The specimens were aged (10,000 thermal cycles and water storage for 90 days) prior to shear bond test. Failure types were analyzed under stereomicroscope and SEM, and phase transformation was calculated. Data (MPa) were analyzed using 3-way ANOVA and Tukey’s tests. Air-abrasion with 110 μm silica particles (10.96) presented significantly higher bond strength (p = 0.0149) compared to 30 μm (8.96). Time (p = 0.403) and distance (p = 0.179) parameters did not affect the results significantly. Air-abrasion with 110 μm particles (12.3) promoted higher bond strength than that of 30 μm (6.4) when applied for 10 s from a distance of 10 mm (Tukey’s). Failure types were predominantly adhesive. Phase transformation ranged between 30.3 and 35.9% for 30 μm particles and 23.8–43.7% for 110 μm particles. While the size of silica-coated alumina particles were more relevant parameter for resin cement adhesion to Y-TZP, time (up to 20 s) and distance (up to 20 mm) appear to be less pertinent.     

Effect of different air-abrasion protocols on topography,surface wettability and adhesion of MDP monomer-based resin cement to zirconia

This study evaluated the effect of air-abrasion protocols on the topography, surface wettability and adhesion of resin cement to zirconia. Ceramic specimens (N?=?49; n?=?7) (15?mm × 2?mm) were randomly allocated to seven groups to be treated with: (1) Air-abrasion with 45?μm Al₂O₃ (A45), (2) 80?μm Al₂O₃ (A80), (3) 30?μm Al₂O₃ coated with SiO₂ (CoJet) (C30), (4) 30?μm Al₂O₃ coated with SiO₂ (Rocatec Soft) (R30), (5) 110?μm Al₂O₃ coated with SiO₂ (Rocatec Plus) (R110); (6) R110R30 (Rocatec) (R110R30) and (7) control, no conditioning (NC). Air-abrasion was performed using a chairside air-abrasion device (2.5?bar, 10?mm, 90?s). Contact angle measurements were performed using goniometry (n?=?5). MDP-based dual resin cement (Panavia F2.0) was bonded on four locations after air-abrasion protocols (n?=?20 per group). Half of the specimens were tested after 24?h and the other half after thermal cycling (×3000, 5–55?°C). Data were analyzed using 1-, 2-way ANOVA and Tukey’s test (alpha = 0.05). Significantly lower contact angle values were observed for groups C30 (62.6?±?0.91), R30 (61.91?±?1.05) and R110R30 (61.54?±?1.02) compared to those of other groups (65.5?±?0.9–110.61?±?0.9) (p?<?0.05). In dry conditions, surface conditioning methods tested did not show significant effect on bond strength (MPa) (10.57?±?1.42–16.86?±?2.54) (p?=?0.238). After thermocycling, bond strength results decreased significantly (p?<?0.05) (12.6–51.2%). R110 (7.18?±?1.34) and A80 (4.92?±?1.53) showed significantly higher bond strength compared to other groups (2.13?±?0.73–4.16?±?1.34) (p?<?0.05). The best wettability and adhesion results with MDP-based resin cement to zirconia was achieved with A80 and R110 air-abrasion.     

Adhesion of resin cement to contemporary hybrid ceramic and polymeric CAD/CAM materials: effect of conditioning methods and ageing

This study assessed the effect of different surface conditioning methods and ageing protocols on adhesion of resin cement to hybrid ceramic and polymeric CAD/CAM materials. CAD/CAM materials (n?=?360, n?=?30 per group), namely (a) Lithium disilicate (IPS e.max CAD-LIS), (b) Zirconia (IPS e.max ZirCAD-ZIR), (c) Polymer (Lava Ultimate-LAV), (d) Polymer infiltrated ceramic network (Enamic-ENA), (e) Polymer infiltrated ceramic (Experimental-1-CS1), (f) Polymer infiltrated ceramic (Experimental-2-CS2), (g) Lithium disilicate reinforced alumina (n!ce-NIC) were cut into slices (3?×?6 × 8?mm³) and conditioned: (a) Method 1: 5% hydrofluoric acid etching (H)+silane and (b) Method 2: Silica coating (CoJet (A)+silane). Group LIS was conditioned with only Method 1 and Group ZIR only with Method 2 (control). Resin cement (Variolink Esthetic II) was bonded onto the conditioned specimens and photopolymerized. One-half of the specimens was subjected to ageing (thermocycling 5–55°, 5000 cycles) and the other half was stored in distilled water (37?°C, 24?h). The resin-substrate interface was loaded under shear forces in a Universal Testing Machine (1?mm/min). Data (MPa) were analyzed using two-way ANOVA and Tukey`s tests (α?=?0.05). Substrate type, conditioning method and ageing had a significant effect on adhesion values (p?<?.05). In aged conditions, ENA-H, ENA-A, LAV-H, LAV-A, CS2-A (15?±?4 – 11.6?±?5) showed no significant difference (p?>?.05), with the CS2-A (15?±?4) showing the least reduction (5.5%) compared to all other groups (5.8–62.6%). CS1-A (100%) followed by ENA-H, ENA-A (93%), CS2-A (80%) presented the highest incidence of cohesive failures after ageing.     

Adhesion to zirconia as a function of primers/silane coupling agents,luting cement types,aging and test methods

This study evaluated the adhesion of resin cements to zirconia with different primers/silane coupling agents using two test methods with and without aging. Zirconia discs (Cercon) (N = 900, n = 15 per group) were ground finished to 2000 grit silicone carbide and randomly divided into seven groups: (a) C: No treatment (Control), (b) SG: Signum, (c) CL: Clearfil Ceramic Primer, (d) AP: Alloy Primer, (e) Monobond Plus, (f) ES-R: ESPE-Sil after Rocatec and (g) ES-C: ESPE-Sil after CoJet. Methacrylate (Variolink II-VL) and MDP based (Panavia F2.0-PN) dual-polymerized and self-adhesive resin cements (RelyX Unicem-RX) were adhered and polymerized accordingly. The specimens were further randomly divided into two groups to be tested after (a) 24-h dry storage at 37 °C and (b) thermocycling (×5000, 5–55 °C). Macroshear (MSB) and macrotensile bond tests (MTB) were conducted in an universal testing machine (crosshead speed: 1 mm/min) and failure types were analyzed after debonding. Data were analyzed using Univariate analysis and Tukey’s tests (α = 0.05). Two-parameter Weibull modulus, scale (m) and shape (0) were calculated. While primer/silane (p < 0.001), cement type (p < 0.001) and aging (p < 0.001) significantly affected the bond results, test method did not show significant difference (p = 0.237). In MSB test, Weilbul moduli were more favorable for MP-VL (4.2) and AP-PN (6) combinations and after aging for MP-VL (4.2) and AP-PN (5.66). In MTB test, after aging, Weilbul moduli were more favorable for AP-PN (5.41). Bond strength results mostly decreased with SG (24–92%) after aging. Cohesive failures in the cement were more frequent with PN (252) compared to VL (83).     

Analysis of structural,morphological alterations,wettability characteristics and adhesion to enamel after various surface conditioning methods

Minimal invasive dental reconstructions and orthodontic appliances are bonded to enamel without removing the enamel with rotating instruments but the top layer of enamel may be partially aprismatic and impair adhesion. The objectives of this study were to investigate the effect of mechanical surface conditioning methods for removing enamel on its structural, morphological alterations, wettability characteristics, and adhesion of resin-based cement to the conditioned surfaces. Maxillary human incisors (N = 40, n_quadrant = 160) were obtained and coronal sections were embedded in acrylic with their labial surfaces exposed. The teeth were randomly divided into four groups and the enamel surface of each tooth was divided into four quadrants. The surfaces were conditioned in a clockwise manner by one of the following methods: (1) Non-conditioned enamel acted as the control group (C); (2) Silicone-coated disk (Sof-Lex disc, Black, 3 M ESPE) (SD); (3) Diamond bur at slow speed (DB) and (4) Airborne particle abrasion (50 μm Al₂O₃, 2 bar, 5 s) (AA). Surface roughness was measured at each quadrant using a non-contact digital profilometer and contact angle measurements were performed using a goniometer. Enamel surfaces were then etched with 37% H₃PO₄ for 60 s and roughness and wettability measurements were repeated. The enamel surfaces in each quadrant received resin composite luting cement (Variolink II, Ivoclar Vivadent) incrementally in a polyethylene mold (diameter: 1 mm²; height: 4 mm) and photopolymerized. The specimens were stored in distilled water for 24 h at 37 °C until the testing procedures and then shear force was applied to the adhesive interface until failure occurred in a Universal Testing Machine (0.5 mm/min). Microshear bond (μSBS) was calculated by dividing the maximum load (N) by the bonding surface area of the resin cement. Representative enamel surfaces were analyzed under the scanning electron microscope (SEM) (x5000) to assess the surface morphology. Failure types were analyzed using optical microscope and SEM. Data (MPa) were analyzed using one-way ANOVA and Tukey`s test for each parameter and Linear model for group comparisons (α = 0.05). Surface conditioning method significantly affected the adhesion results (p < 0.001), surface roughness (p = 0.017), and contact angle (p < 0.001). Interaction terms were significant (p > 0.05). AA (338 ± 182) created significantly higher surface roughness compared to SD (308 ± 180) and DB (242 ± 197) (p < 0.05). After etching with 37% H₃PO₄, DB (307 ± 223) resulted in significantly lower roughness than those of SD (385 ± 173) and AA (414 ± 193) (p < 0.05). AA (40 ± 11) delivered significantly lower contact angle compared to those of SD (61 ± 9) and DB (59 ± 10). After etching with 37% H₃PO₄, AA (42 ± 10) and DB (50 ± 10) presented the lowest contact angle (p < 0.05). Mean μSBS results (MPa) showed significant difference between the experimental groups (p = 0.011) and were in descending order as follows: DB (20 ± 8)^a?a b < C (12 ± 5)^b. Failure types were predominantly mixed failure type between the enamel and the resin cement with more than half of the resin remained on the enamel surface (32 to 33 out of 40) in all groups. Cohesive failure in the enamel was not observed in any of the groups. SEM analysis showed that AA group leaves abundant particles on the enamel surface and after DB and AA, etching could not remove the particles completely and expose the enamel prisms.     

Effect of clinical and laboratory contamination media on the adhesion of luting cement to direct and indirect resin composite materials

This study evaluated the effect of contamination media on the adhesion of resin cement to resin composites. Specimens of direct (DRC) (Quadrant Photo Posterior) and indirect resin composite (IRC) (Gradia) (N = 300, n = 15 per group) were prepared. Except the control group (C), the specimens of DRC and IRC were contaminated with one of the following media: (a) saliva (S), (b) silicon (SI), (c) dental stone (D), and (d) isolation medium (I). While one half was only rinsed with water, the other half was silica coated (30 μm SiO₂, Siljet). All specimens were silanized (Monobond Plus) and coated with adhesive resin (Heliobond). Resin cement (Variolink II) was bonded to the substrates and photo-polymerized for 40 s. After thermocycling (x5.000, 5–55 °C), composite–cement interface was loaded under shear in a Universal Testing Machine (1 mm/min). Data (MPa) were analyzed using Univariate analysis, Tukey’s and Dunnett-T3 tests. Both contamination media (p = 0.000) and surface conditioning (p = 0.005) significantly affected adhesion to DRC and IRC. No significant difference was found between the DRC and IRC (without: p = 0.098; with: p = 0.084). Significantly lower results were obtained after SI (DRC: 0.66 ± 0.6; IRC: 0.8 ± 1.3) followed by I contamination (DRC: 2.1 ± 2.6; IRC: 0.8 ± 1.3) (p < 0.05). Regardless of contamination medium, surface conditioning significantly increased the results for both DRC (15.1 ± 6.1–23.6 ± 3.7) and IRC (20.3 ± 5.4–25.1 ± 3.6) (p < 0.05). Weibull distribution increased after surface conditioning for both DRC (without: 1.33–3.27; with: 2.55–9.34) and IRC (without: 1.07–3.75; with: 3.7–7.73). Predominantly adhesive (132 out of 150) failures were observed when surfaces were not conditioned.     

Effectiveness of different surface cleaning methods on the shear bond strength of resin cement to contaminated zirconia: an in vitro study

The purpose of this in vitro study was to evaluate and compare the effectiveness of different surface cleaning methods on the shear bond strength (SBS) of zirconia ceramic surfaces. Seventy polished and cleaned zirconia disk specimens of 8 mm in diameter and 3.4 mm in thickness were immersed in fresh saliva. They were then pressed into a freshly mixed silicone disclosing medium. Six different cleaning methods were applied to the tested groups; they were airborne-particle abraded (AA), covered with a cleaning paste (Ivoclean®) (IV), etched with orthophosphoric acid (PA), immersed in alcohol (AL), rinsed with tap water only (WA), or cleaned with steam (SC). No surface cleaning was done after saliva immersion and silicone disclosing medium contamination to the control group (CC). The specimens were then bonded to an adhesive resin cement using polyethylene tubes. SBS was determined using a universal testing machine at a crosshead speed of 1 mm/min. The specimens were also examined with a scanning electron microscope and a stereomicroscope. Group AA yielded the highest SBS value (7.01 ± 1.4 MPa) among the groups, while Group WA had the lowest SBS value (3.03 ± 0.8 MPa). The SBS values of Group AA (7.01 ± 1.4 MPa) and IV (6.2 ± 1.7 MPa) were also significantly higher than those of the remaining four groups (p < 0.05). Within the limitations of this in vitro study, it was concluded that among the various cleaning methods tested, airborne-particle abrasion and Ivoclean® paste were effective in cleaning the zirconia surface.     

Adhesion of resin cements to contaminated zirconia resin cements on zirconia: effect saliva-contamination and surface conditioning

This study evaluated the adhesion of resin cements to zirconia after saliva contamination using resin cements with different chemistries. Zirconia discs (N?=?240, n?=?10 per group) were randomly divided into three groups: (a) C: No contamination (Control), (b) S: Contamination with saliva, (c) S?+?AA: Contamination with saliva followed by air-abrasion (CoJet). While half of the specimens were not conditioned, the other half were conditioned with 37.5% H₃PO₄ for 60?s. After rinsing, all specimen surfaces were silanized (Monobond Plus). Resin cements based on either methacrylate (Variolink II–VL) or MDP monomer (Panavia 21-PN) were polymerized on the substrates. The specimens were randomly divided into two further groups to be tested either after (a) 24?h dry storage at 37?°C or (b) thermocycling (×5000, 5–55?°C). Microshear bond (MSB) tests were conducted in a Universal Testing Machine and failure types were analyzed. Data were analyzed using Univariate analysis and Tukey’s tests (alpha = 0.05). While saliva contamination, 37.5% H₃PO₄ application (p?<?.001) and aging (p?<?.05) significantly affected the bond results, cement type did not show significant difference after aging (p?>?.05). Adhesive strength of PN (1.2–4.4?MPa) on saliva contaminated and etched zirconia was more stable than that of VL (0–2.8?MPa). After aging, bond strength results decreased the most with VL (3–100%) compared to PN (32–71%) but the decrease was less in the air-abraded groups after aging (VL: 3%; PN: 32%). Exclusively adhesive failures were experienced in all groups.     

Biaxial flexural strength and Weilbull characteristics of adhesively luted hybrid and reinforced CAD/CAM materials to dentin: effect of self-etching ceramic primer versus hydrofluoric acid etching

Abstract

This study evaluated the influence of the surface treatment and aging on the biaxial flexural strength of ceramic materials cemented to a dentin analogue. One hundred twenty disc-shaped specimens were allocated into 12 groups considering three study factors: ceramic material (lithium disilicate, leucite-based ceramic and hybrid ceramic), surface treatment (10% hydrofluoric acid etching?+?silane or self-etching glass-ceramic primer) and Aging (with 10,000 thermocycles of 5–37–55?°C or without). A tri-layer assembly was designed to mimic a cemented restoration (Variolink N) into a dentin analogue. All samples were submitted to the biaxial flexural strength assay. The flexural strength in MPa was calculated using the finite element method for each sample considering thickness, material properties, and the load to fracture during the in vitro test. Fractographic analysis was also performed. The data was evaluated using three-way ANOVA and Tukey test (α?=?5%). ANOVA showed influence for the Material*Treatment*Aging interaction on the flexural strength (p?=?0.011). The highest strength was calculated for lithium disilicate ceramic?+?self-etching ceramic primer without aging (499?±?17?MPa)^A and the lowest value for hybrid ceramic material?+?acid etching with aging (424?±?48?MPa)^E. According to the Weibull modulus, the most predictable strength was calculated for lithium disilicate?+?acid etching after aging. Acid etching or self-etching ceramic primer promotes similar immediate biaxial flexural strength for each evaluated ceramic. In the long-term, superior strength was observed using acid etching for lithium disilicate and the self-etching ceramic primer for the hybrid ceramic while no difference was observed for leucite-based ceramic.

Clinical implications: Some protocols combining the CAD/CAM ceramic material and the surface treatment could present suitable and stable flexural strength.