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.

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.

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.

Effect of Cement Shade and Light-curing Unit on Bond Strength of a Ceramic Cemented to Dentin

Purpose: To evaluate the effect of cement shade, light-curing unit, and water storage on tensile bond strength (a) of a feldspathic ceramic resin bonded to dentin.Materials and Methods: The dentin surface of 40 molars was exposed and etched with 37% phosphoric acid, then an adhesive system was applied. Forty blocks of feldspathic ceramic (Vita VM7) were produced. The ceramic surface was etched with 10% hydrofluoric acid for 60 s, followed by the application of a silane agent and a dual-curing resin cement (Variolink II). Ceramic blocks were cemented to the treated dentin using either A3 or transparent (Tr) shade cement that was activated using either halogen or LED light for 40 s. All blocks were stored in 37 degrees C distilled water for 24 h before cutting to obtain non-trimmed bar-shaped specimens (adhesive area = 1 mm(2) +/- 0.1) for the microtensile bond strength test. The specimens were randomly grouped according to the storage time: no storage or stored for 150 days in 37 degrees C distilled water. Eight experimental groups were obtained (n = 30). The specimens were submitted to the tensile bond strength test using a universal testing machine at a crosshead speed of 1 mm/min. The data were statistically analyzed using ANOVA and Tukey's post-hoc tests (alpha = 0.05).Results: The mean bond strength values were significantly lower for the corresponding water stored groups, except for the specimens using A3 resin cement activated by halogen light. There was no significance difference in mean bond strength values among all groups after water storage.Conclusion: Water storage had a detrimental effect under most experimental conditions. For both cement shades investigated (Tr and A3) under the same storage condition, the light-curing units (QTH and LED) did not affect the mean microtensile bond strengths of resin-cemented ceramic to dentin.

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.

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)

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.

Nanopore size growth and ultrafiltration performance of SnO2 ceramic membranes prepared by sol-gel route

Supported ceramic membranes have been produced by the sol-casting procedure from aqueous colloidal suspensions prepared by the sol-gel route. Coatings on a tubular alumina support have been successfully performed leading to crack free layers. Samples have been sintered at 400, 500 and 600 degreesC, and the effect of heating treatment on the nanostructure and on the ultrafiltration properties are analyzed. The characterization has been done by high resolution scanning electron microscopy, nitrogen adsorption-desorption isotherms, water permeation and cut-off determination using polyethylene glycol standard solutions. The micrographs have revealed that grains and pore size increase with the temperature, whereas their shape remains invariant. This results is in agreements with N-2 adsorption-desorption analyses, which have revealed that the mean pore size diameter increases from 4 to 10 nm as the sintering temperature increases from 400 to 600 degreesC, while the total porosity remains constant. Furthermore, the tortuosity, calculated from water permeability, is essentially invariant with the sintering temperatures. The membranes cut-off, determined with a retention rate equal to 95%, are 3500, 6500 and 9000 g . mol(-1) for 400, 500 and 600 degreesC, respectively, showing that the permeation properties of SnO2 ultrafiltration membranes can easily be controlled by sintering condition.

Formation of TiO2 ceramic foams from the integration of the sol-gel method with surfactants assembly and emulsion

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Sol-gel synthesis and characterization of Fe(2)O(3) center dot CeO(2) doped with Pr ceramic pigments

Undoped x center dot alpha-Fe(2)O(3) y center dot CeO(2) and doped with praseodymium ceramic pigments were obtained by the sol-gel method after heat treatment at 800 degrees C for 2 h. These pigments were characterized by XRD, nitrogen adsorption, scanning electron microscopy, ultraviolet-visible absorption spectroscopy and colorimetrical measurements. Red and brown colors with several tonalities were observed after changes with Ce and Pr concentration.