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.

Durability of Microtensile Bond to Nonetched and Etched Feldspar Ceramic: Self-adhesive Resin Cements vs Conventional Resin

Purpose: The objective of this study was to evaluate the effect of thermocycling (TC), self-adhesive resin cements and surface conditioning on the microtensile bond strength (mu TBS) between feldspathic ceramic blocks and resin cements.Materials and Methods: Fifty-six feldspathic ceramic blocks (10 x 7 x 5 mm) (Vita Mark II) were divided into groups according to the factors "resin cement" (3 cements) and "surface conditioning" (no conditioning or conditioning [10% hydrofluoric acid etching for 5 min + silanization]) (n = 8): group 1: conditioning+Variolink II (control group); group 2: no conditioning+Biscem; group 3: no conditioning+RelyX U100; group 4: no conditioning+Maxcem Elite; group 5: conditioning+Biscem; group 6: conditioning+RelyX U100; group 7: conditioning+Maxcem Elite. The ceramic-cement blocks were sectioned to produce non-trimmed bar specimens (adhered cross-sectional area: 1 +/- 0.1 mm(2)), which were divided into two storage conditions: dry, mu TBS immediately after cutting; TC (12,000x, 5 degrees C/55 degrees C). Statistical significance was deterimined using two-way ANOVA (7 strategies and 2 storage conditions) and the post-hoc Tukey test (p<0.05).Results: Resin cement and thermocycling affected the mu TBS significantly (p = 0.001). In the dry condition, group 5 (18 +/- 6.5 MPa) presented the lowest values of mu TBS when compared to the other groups. TC decreased the mean mu TBS values significantly (p<0.05) for all resin cements tested (9.7 +/- 2.3 to 22.1 +/- 6.3 MPa), except for the resin cement RelyX U100 (22.1 +/- 6.3 MPa). In groups 3 and 4, it was not possible to measure mu TBS, since these groups had 100% pre-test failures during sectioning. Moreover, the same occurred in group 2 after TC, where 100% failure was observed during thermocycling (spontaneous failures).Conclusion: Hydrofluoric acid etching and silanization of the feldspathic ceramic surface are essential for bonding self-adhesive resin cement to a feldspathic ceramic, regardless of the resin cement used. Non-etched ceramic is not recommended.

Y-TZP ceramic processing from coprecipitated powders: A comparative study with three commercial dental ceramics

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

The effect of porcelain thickness and surface liner application on the fracture behavior of a ceramic system

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

Bond strength durability of a resin composite on a reinforced ceramic using various repair systems

Objectives. This study compared the durability of repair bond strength of a resin composite to a reinforced ceramic after three repair systems.Methods. Alumina-reinforced feldspathic ceramic blocks (Vitadur-alpha(R)) (N=30) were randomly divided into three groups according to the repair method: PR-Porcelain Repair Kit (Bisco) [etching with 9.5% hydrofluoric acid + silanization + adhesive]; CJ-CoJet Repair Kit (3M ESPE) [(chairside silica coating with 30 mu m SiO2 + silanization (ESPE(R)-Sil) + adhesive (Visio(TM)-Bond)]; CL-Clearfil Repair Kit [diamond surface roughening, etching with 40% H3PO4 + Clearfil Porcelain Bond Activator + Clearfil SE Bond)]. Resin composite was photo-polymerized on each conditioned ceramic block. Non-trimmed beam specimens were produced for the microtensile bond strength (mu TBS) tests. In order to study the hydrolytic durability of the repair methods, the beam specimens obtained from each block were randomly assigned to two conditions. Half of the specimens were tested either immediately after beam production (Dry) or after long-term water storage (37 degrees C, 150 days) followed by thermocyling (12,000 cycles, 5-55 degrees C) in a universal testing machine (1 mm/min). Failure types were analyzed under an optical microscope and SEM.Results. mu TBS results were significantly affected by the repair method (p=0.0001) and the aging conditions (p=0.0001) (two-way ANOVA, Tukey's test). In dry testing conditions, PR method showed significantly higher (p < 0.001) repair bond strength (19.8 +/- 3.8 MPa) than those of CJ and CL (12.4 +/- 4.7 and 9.9 +/- 2.9, respectively). After long-term water storage and thermocycling, CJ revealed significantly higher results (14.5 +/- 3.1 MPa) than those of PR (12.1 +/- 2.6 MPa) (p < 0.01) and CL (4.2 +/- 2.1 MPa) (p < 0.001). In all groups when tested in dry conditions, cohesive failure in the composite accompanied with adhesive failure at the interface (mixed failures), was frequently observed (76%, 80%, 65% for PR, CJ and CL, respectively). After aging conditions, while the specimens treated with PR and CJ presented primarily mixed failure types (52% and 87%, respectively), CL group presented mainly complete adhesive failures at the interface (70%).Significance. Hydrolytic stability of the repair method based on silica coating and silanization was superior to the other repair strategies for the ceramic tested. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Surface characterization of feldspathic ceramic using ATR FT-IR and ellipsometry after various silanization protocols

Objectives. This study characterized the feldspathic ceramic surfaces after various silanization protocols.Methods. Ceramic bars (2 mm x 4 mm x 10 mm) (N = 18) of feldpathic ceramic (VM7, VITA Zahnfabrik) were manufactured and finished. Before silane application, the specimens were ultrasonically cleaned in distilled water for 10 min. The ceramic specimens were randomly divided into nine groups (N = 2 per group) and were treated with different silane protocols. MPS silane (ESPE-Sil, 3M ESPE) was applied to all specimens and left to react at 20 degrees C for 2 min (G20). After drying, the specimens were subjected to heat treatment in an oven at 38 degrees C (G38), 79 degrees C (G79) or 100 degrees C (G100) for 1 min. Half of the specimens of each group were rinsed with water at 80 degrees C for 15 s (G20B, G38B, G79B, G100B). The control group (GC) received no silane. Attenuated total reflection infrared Fourier transform analysis (ATR FT-IR) was performed using a spectrometer. Thickness of silane layer was measured using a spectroscopic ellip-someter working in the lambda = 632.8 nm (He-Ne laser) at 70 degrees incidence angle. Surface roughness was evaluated using an optical profilometer. Specimens were further analyzed under the Scanning Electron Microscopy (SEM) to observe the topographic patterns.Results. ATR FT-IR analysis showed changes in Si-O peaks with enlarged bands around 940 cm(-1). Ellipsometry measurements showed that all post-heat treatment actions reduced the silane film thickness (30.8-33.5 nm) compared to G20 (40 nm). The groups submitted to rinsing in hot water (B groups) showed thinner silane films (9.8-14.4 nm) than those of their corresponding groups (without washing) (30.8-40 nm). Profilometer analysis showed that heat treatments (Ra approximate to 0.10-0.19 mu m; Rq approximate to 0.15-0.26 mu m) provided a smoother surface than the control group (Ra approximate to 0.48 mu m; Rq approximate to 0.65 mu m). Similar patterns were also observed in SEM images.Significance. Heat treatment after MPS silane application improved the silane layer network. Rinsing with boiling water eliminated the outmost unreacted regions of the silane yielding to thinner film thicknesses. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of Y-TZP ceramic treatment and different resin cements on bond strength to dentin

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

Opaque Layer Firing Temperature and Aging Effect on the Flexural Strength of Ceramic Fused to Cobalt-Chromium Alloy

Purpose: To evaluate the effect of the opaque layer firing temperature and mechanical and thermal cycling on the flexural strength of a ceramic fused to commercial cobalt-chromium alloy (Co-Cr). The hypotheses were that higher opaque layer temperatures increase the metal/ceramic bond strength and that aging reduces the bond strength.Materials and Methods: Metallic frameworks (25 x 3 x 0.5 mm(3); ISO 9693) (N = 60) were cast in Co-Cr and airborne-particle abraded (Al(2)O(3): 150 mu m) at the central area of the frameworks (8 x 3 mm(2)) and divided into three groups (N = 20), according to the opaque layer firing temperature: Gr1 (control)-900 degrees C; Gr2-950 degrees C; Gr3-1000 degrees C. The opaque ceramic (Opaque, Vita Zahnfabrick, Bad Sackingen, Germany) was applied, and the glass ceramic (Vita Omega 900, Vita Zahnfabrick) was fired onto it (thickness: 1 mm). While half the specimens from each group were randomly tested without aging (water storage: 37 degrees C/24 hours), the other half were mechanically loaded (20,000 cycles; 50 N load; distilled water at 37 degrees C) and thermocycled (3000 cycles; 5 degrees C to 55 degrees C, dwell time: 30 seconds). After the flexural strength test, failure types were noted. The data were analyzed using 2-way ANOVA and Tukey's test (alpha = 0.05).Results: Gr2 (19.41 +/- 5.5 N) and Gr3 (20.6 +/- 5 N) presented higher values than Gr1 (13.3 +/- 1.6 N) (p = 0.001). Mechanical and thermal cycling did not significantly influence the mean flexural strength values (p > 0.05). Increasing the opaque layer firing temperature improved the flexural bond strength values (p < 0.05). The hypotheses were partially accepted.Conclusion: Increasing of the opaque layer firing temperature improved the flexural bond strength between ceramic fused to Co-Cr alloy.

Effects of cement thickness and bonding on the failure loads of CAD/CAM ceramic crowns: Multi-physics FEA modeling and monotonic testing

Objective. To determine the influence of cement thickness and ceramic/cement bonding on stresses and failure of CAD/CAM crowns, using both multi-physics finite element analysis and monotonic testing.Methods. Axially symmetric FEA models were created for stress analysis of a stylized monolithic crown having resin cement thicknesses from 50 to 500 mu m under occlusal loading. Ceramic-cement interface was modeled as bonded or not-bonded (cement-dentin as bonded). Cement polymerization shrinkage was simulated as a thermal contraction. Loads necessary to reach stresses for radial cracking from the intaglio surface were calculated by FEA. Experimentally, feldspathic CAD/CAM crowns based on the FEA model were machined having different occlusal cementation spaces, etched and cemented to dentin analogs. Non-bonding of etched ceramic was achieved using a thin layer of poly(dimethylsiloxane). Crowns were loaded to failure at 5 N/s, with radial cracks detected acoustically.Results. Failure loads depended on the bonding condition and the cement thickness for both FEA and physical testing. Average fracture loads for bonded crowns were: 673.5 N at 50 mu m cement and 300.6 N at 500 mu m. FEA stresses due to polymerization shrinkage increased with the cement thickness overwhelming the protective effect of bonding, as was also seen experimentally. At 50 mu m cement thickness, bonded crowns withstood at least twice the load before failure than non-bonded crowns.Significance. Occlusal "fit" can have structural implications for CAD/CAM crowns; pre-cementation spaces around 50-100 mu m being recommended from this study. Bonding benefits were lost at thickness approaching 450-500 mu m due to polymerization shrinkage stresses. (C) 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of testing methods on the bond strength of resin to zirconia-alumina ceramic: microtensile versus shear test

This study tested the bond strength of a resin cement to a glass-infiltrated zirconia-alumina ceramic after three conditioning methods and using two test methods (shear-SBS versus microtensile-MTBS). Ceramic blocks for MTBS and ceramic disks for SBS were fabricated. Three surface conditioning (SC) methods were evaluated: (1) 110-mu m Al(2)O(3)+Silanization; (2) Chairside silica coating+silanization: (3) Laboratory silica coating+silanization. Following surface conditioning, the resin cement (Panavia F) was bonded to the conditioned ceramics. Although no statistically significant differences (p=0.1076) were seen between the test methods, results yielded with the different surface conditioning methods showed statistically significant differences (p<0.0001) (SC2=SC3>SC1.). As for the interaction between the factors, two-way ANOVA showed that it was not statistically significant (p=0.1443). MTBS test resulted in predominantly mixed failure (85%), but SBS test resulted in exclusively adhesive failure. on the effects of different surface conditioning methods, chairside and laboratory tribochemical silica coating followed by silanization showed higher bond strength results compared to those of aluminum oxide abrasion and silanization, independent of the test method employed.

Marginal and Internal Discrepancies Related to Margin Design of Ceramic Crowns Fabricated by a CAD/CAM System

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

Strength of a feldspar ceramic according to the thickness and polymerization mode of the resin cement coating

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

Effect of silica coating combined to a MDP-based primer on the resin bond to Y-TZP ceramic

The aim of this study was to evaluate the influence of silica coating and 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-based primer applications upon the bonding durability of a MDP-based resin cement to a yttrium stabilized tetragonal zirconia (Y-TZP) ceramic. Ninety-six Y-TZP tabs were embedded in an acrylic resin (free surface for adhesion: 5 x 5 mm(2)), ground finished and randomly divided into four groups (N = 24) according to the ceramic surface conditioning: (1) cleaning with isopropanol (ALC); (2) ALC + phosphoric acid etching + MDP-based primer application (MDP-primer); (3) silica coating + 3-methacryloyloxypropyl trimethoxysilane (MPS)-based coupling agent application (SiO(2) + MPS-Sil); and (4) SiO(2) + MDP-primer. The MDP-based resin cement was applied on the treated surface using a cylindrical mold (diameter=3 mm). Half of the specimens from each surface conditioning were stored in distilled water (37 C, 24 h) before testing. Another half of the specimens were stored (90 days) and thermo-cycled (12,000x) during this period (90d/TC) before testing. A shear bond strength (SBS) test was performed at a crosshead speed of 0.5 mm/min. Two factors composed the experimental design: ceramic conditioning strategy (in four levels) and storage condition (in two levels), totaling eight groups. After 90d/TC (Tukey; p < 0.05), SiO(2) + MDP-primer (24.40 MPa) promoted the highest SBS. The ALC and MDP-primer groups debonded spontaneously during 90d/TC. Bonding values were higher and more stable in the SiO2 groups. The use of MDP-primer after silica coating increased the bond strength. (C) 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part 8: Appl Biomater 95B: 69-74, 2010.

Nanosized lead lanthanum titanate (PLT) ceramic powders synthesized by the oxidant peroxo method

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

Synthesis and characterization of antimony tartrate for ceramic precursors

Synthesis and characterization of antimony tartrate used as a precursor of ceramic powders obtained by Pechini's method were carried out. Antimony tartrate was chosen as a substitute for the antimony citrate commonly used in this chemical processing, because of difficulties in preparing the citrate. FTIR and TGA/DTA analysis showed that antimony tartrate, H-2[Sb-2(C4H2O6)(2)]. forms a polymeric structure. The procedure described indicates that the antimony chelate obtained is adequate for Pechini's method.