Does Adhesive Resin Application Contribute to Resin Bond Durability on Etched and Silanized Feldspathic Ceramic?

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Does the Ultrasonic Cleaning Medium Affect the Adhesion of Resin Cement to Feldspathic Ceramic?

Purpose: To evaluate the effect of different cleaning media on the adhesion of resin cement to feldspathic ceramic after etching.Materials and Methods: The cementation surfaces of ceramic blocks (N = 20, n = 5 per group) were etched with 10% hydrofluoric acid (HF) gel for 20 s and rinsed for 60 s. They were then randomly assigned to 4 groups: G1: air-water spray+drying (control); G2: ultrasonic cleaning in distilled water for 4 min+drying; G3: ultrasonic cleaning in 99.5% acetone for 4 min+drying; G4: ultrasonic cleaning in 70% alcohol for 4 min+drying. The ceramic blocks were silanized and cemented (RelyX ARC) to the composite blocks. Subsequently, the microtensile bond strength test (mu TBS) was performed. In addition, EDS analysis was made to assess the elemental composition of the conditioned and cleaned ceramic surfaces.Results: A significantly higher mean mu TBS was obtained when specimens had been ultrasonically cleaned in distilled water (G2: 18.8 +/- 0.4 MPa) (p < 0.05) compared to other groups (G1: 16.6 +/- 0.5; G3: 16.1 +/- 0.9; G4: 15.8 +/- 1.4) (one-way ANOVA). EDS analysis indicated the presence of F- only in G1. Dissolved precipitates after HF etching were removed by ultrasonic cleaning.Conclusion: Cleaning the HF-etched ceramic surface ultrasonically in distilled water is recommended, instead of rinsing it with air-water spray only.

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 ceramic surface conditioning and resin cements on microtensile bond strength to a glass ceramic

Statement of problem. It is not clear how different glass ceramic surface pretreatments influence the bonding capacity of various luting agents to these surfaces.Purpose. The purpose of this study was to evaluate the microtensile bond strength (mu TBS) of 3 resin cements to a lithia disilicate-based ceramic submitted to 2 surface conditioning treatments.Material and methods. Eighteen 5 X 6 X 8-mm ceramic (IPS Empress 2) blocks were fabricated according to manufacturer's instructions and duplicated in composite resin (Tetric Ceram). Ceramic blocks were polished and divided into 2 groups (n=9/treatment): no conditioning (no-conditioning/control), or 5% hydrofluoric acid etching for 20 seconds and silanization for 1 minute (HF + SIL). Ceramic blocks were cemented to the composite resin blocks with I self-adhesive universal resin cement (RelyX Unicem) or 1 of 2 resin-based luting agents (Multilink or Panavia F), according to the manufacturer's instructions. The composite resin-ceramic blocks were stored in humidity at 37 degrees C for 7 days and serially sectioned to produce 25 beam specimens per group with a 1.0-mm(2) cross-sectional area. Specimens were thermal cycled (5000 cycles, 5 degrees C-55 degrees C) and tested in tension at 1 mm/min. Microtensile bond strength data (MPa) were analyzed by 2-way analysis of variance and Tukey multiple comparisons tests (alpha=.05). Fractured specimens were examined with a stereomicroscope (X40) and classified as adhesive, mixed, or cohesive.Results. The surface conditioning factor was significant (HF+SIL > no-conditioning) (P<.0001). Considering the unconditioned groups, the mu TBS of RelyX Unicem was significantly higher (9.6 +/- 1.9) than that of Multilink (6.2 +/- 1.2) and Panavia F (7.4 +/- 1.9). Previous etching and silanization yielded statistically higher mu TBS values for RelyX Unicem (18.8 +/- 3.5) and Multilink (17.4 +/- 3.0) when compared to Panavia F (15.7 +/- 3.8). Spontaneous debonding after thermal cycling was detected when luting agents were applied to untreated ceramic surfaces.Conclusion. Etching and silanization treatments appear to be crucial for resin bonding to a lithia disilicate-based ceramic, regardless of the resin cement used.

Effect of surface treatments on the resin bond to zirconium-based ceramic

Purpose: This study tested the hypothesis that the tribochemical silica coating on ceramic surfaces increases the bond strength of resin cement to a glass-infiltrated zirconium-based ceramic. Materials and Methods: Fifteen blocks of In-Ceram Zirconia from CEREC InLab (5 per group) and 15 composite blocks (Z-250) 5 mm x 5 mm x 4 mm were made. The ceramic surfaces were polished, and the blocks were divided into three groups: (1) airborne abrasion with 110-μm aluminum oxide particles; (2) Rocatec system, tribochemical silica coating; and (3) CoJet system, tribochemical silica coating. The ceramic blocks were cemented to the composite blocks using Panavia F according to the manufacturer's specifications. All samples were stored in 37°C distilled water for 7 days and later sectioned in two axes using a diamond disk under cooling to obtain specimens with a cross-sectional area of approximately 1 mm2 (n = 45). Each specimen was then attached with cyanoacrylate glue to an adapted device for the microtensile test, which was carried out on a universal testing machine. Results: The results were subjected to ANOVA and Tukey's test. Group 2 (23.0 ± 6.7 MPa) and group 3 (26.8 ± 7.4 MPa) showed greater bond strength than group 1 (15.1 ± 5.3 MPa). There was no significant difference between groups 2 and 3. All failures were in the adhesive zone. Conclusion: The hypothesis was confirmed - the tribochemical systems increased the bond strength between Panavia F and In-Ceram Zirconia.

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.

Polishing methods of an alumina-reinforced feldspar ceramic

The purpose of this study was to test the hypothesis that mechanical polishing methods of ceramic surfaces allow similar superficial roughness to that of glazed surfaces. Twenty-five Vitadur Alpha ceramic discs (5 mm x 2 mm) were prepared according to the manufacturer's specifications. All specimens were glazed and randomly assigned to 5 groups (n=5), according to finishing and polishing protocols: G1: glazed (control); G2: diamond bur finishing; G3: G2 + silicon rubber tip polishing; G4: G3 + felt disc/diamond polishing paste; G5: G3 + felt disc impregnated with fine-particle diamond paste. Next, surface roughness means (Ra - μm) were calculated. Qualitative analysis was made by scanning electron microscopy. Surface roughness data were submitted to ANOVA and Tukey's test at 5% significance level. G1 and G4 were statistically similar (p>0.05). G2 presented the highest roughness means (p<0.05) followed by groups G3, G5, G4 and G1 in a decreasing order. The hypothesis was partially confirmed as only the mechanical polishing (G4) produced similar superficial roughness to that of surface glazing, although finishing and polishing are technically critical procedures.

Silica coating on alumina ceramic: comparison of three chairside air-abrasion devices working for different times and distances.

This study evaluated, by scanning electron microscope (SEM) and EDS, the effect of different strategies for silica coating (sandblasters, time and distance) of a glass-infiltrated ceramic (In-Ceram Alumina). Forty-one ceramic blocks were produced. For comparison of the three air-abrasion devices, 15 ceramic samples were divided in three groups (N.=5): Bioart, Microetcher and Ronvig (air-abrasion parameters: 20 s at a distance of 10 mm). For evaluation of the time and distance factors, ceramic samples (N.=5) were allocated in groups considering three applied times (5 s, 13 s and 20 s) and two distances (10 mm and 20 mm), using the Ronvig device. In a control sample, no surface treatment was performed. After that, the micro-morphologic analyzes of the ceramic surfaces were made using SEM. EDS analyzes were carried out to detect the % of silica on representative ceramic surface. ANOVA and Tukey tests were used to analyze the results. One-way ANOVA showed the silica deposition was different for different devices (P=0.0054). The Ronvig device promoted the highest silica coating compared to the other devices (Tukey test). Two-way ANOVA showed the distance and time factors did not affect significantly the silica deposition (application time and distance showed no statistical difference). The Ronvig device provided the most effective silica deposition on glass-infiltrated alumina ceramic surface and the studied time and distance for air-abrasion did not affect the silica coating.

Effect of hydrofluoric acid etching duration on the roughness and flexural strength of a lithium disilicate-based glass ceramic

The aim of this study was to examine the effect of different acid etching times on the surface roughness and flexural strength of a lithium disilicate-based glass ceramic. Ceramic bar-shaped specimens (16 mm x 2 mm x 2 mm) were produced from ceramic blocks. All specimens were polished and sonically cleaned in distilled water. Specimens were randomly divided into 5 groups (n=15). Group A (control) no treatment. Groups B-E were etched with 4.9% hydrofluoric acid (HF) for 4 different etching periods: 20 s, 60 s, 90 s and 180 s, respectively. Etched surfaces were observed under scanning electron microscopy. Surface profilometry was used to examine the roughness of the etched ceramic surfaces, and the specimens were loaded to failure using a 3-point bending test to determine the flexural strength. Data were analyzed using one-way ANOVA and Tukey's test (α=0.05). All etching periods produced significantly rougher surfaces than the control group (p<0.05). Roughness values increased with the increase of the etching time. The mean flexural strength values were (MPa): A=417 ± 55; B=367 ± 68; C=363 ± 84; D=329 ± 70; and E=314 ± 62. HF etching significantly reduced the mean flexural strength as the etching time increased (p=0.003). In conclusion, the findings of this study showed that the increase of HF etching time affected the surface roughness and the flexural strength of a lithium disilicate-based glass ceramic, confirming the study hypothesis.

Effect of ceramic surface treatment on the shear bond strength of a resin cement to different ceramic systems

This study evaluated three surface treatments and their effects on the shear bond strength between a resin cement and one of three ceramics. The ceramic surfaces were evaluated with scanning electron microscopy (SEM ) as well. Specimens were treated with 50 μm aluminum oxide airborne particles, 10% hydrofluoric acid etching, or a combination of the two. Using a matrix with a center hole (5.0 mm × 3.0 mm), the ceramic bonding areas were filled with resin cement following treatment. The specimens were submitted to thermal cycling (1,000 cycles) and the shear bond strength was tested (0.5 mm/minute). The failure mode and the effect of surface treatment were analyzed under SEM . Data were submitted to ANOVA and a Tukey test (α = 0.05). Duceram Plus and IPS Empress 2 composite specimens produced similar shear bond strength results (p > 0.05), regardless of the treatment method used. Hydrofluoric acid decreased the shear bond strength of In-Ceram Alumina specimens. For all materials, surface treatments changed the morphological surface. All treatments influenced the shear bond strength and failure mode of the ceramic/resin cement composites.

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.

Durability of Adhesion between Feldspathic Ceramic and Resin Cements: Effect of Adhesive Resin, Polymerization Mode of Resin Cement, and Aging

Purpose: Adhesive cementation is an important step for restorations made of feldspathic ceramic as it increases the strength of such materials. Incorrect selection of the adhesive resin and the resin cement to adhere to the ceramic surface and their durability against aging can affect the adhesion between these materials and the clinical performance. This study evaluated the effect of adhesive resins with different pHs, resin cements with different polymerization modes, and aging on the bond strength to feldspathic ceramic. Materials and Methods: One surface of feldspathic ceramic blocks (VM7) (N = 90) (6.4 × 6.4 × 4.8 mm3) was conditioned with 10% hydrofluoric acid for 20 seconds, washed/dried, and silanized. Three adhesive resins (Scotchbond Multi-Purpose Plus [SBMP], pH: 5.6; Single Bond [SB], pH: 3.4; and Prime&Bond NT [NT], pH: 1.7) were applied on the ceramic surfaces (n = 30 per adhesive). For each adhesive group, three resin cements with different polymerization modes were applied (n = 10 per cement): photo-polymerized (Variolink II base), dual polymerized (Variolink II base + catalyst), and chemically polymerized (C&B). The bonded ceramic blocks were stored in water (37°C) for 24 hours and sectioned to produce beam specimens (cross-sectional bonded area: 1 ± 0.1 mm2). The beams of each block were randomly divided into two conditions: Dry, microtensile test immediately after cutting; TC, test was performed after thermocycling (12,000×, 5°C to 55°C) and water storage at 37°C for 150 days. Considering the three factors of the study (adhesive [3 levels], resin cement [3 levels], aging [2 levels]), 18 groups were studied. The microtensile bond strength data were analyzed using 3-way ANOVA and Tukey's post hoc test (α= 0.05). Results: Adhesive resin type (p < 0.001) and the resin cement affected the mean bond strength (p= 0.0003) (3-way ANOVA). The NT adhesive associated with the chemically polymerized resin cement in both dry (8.8 ± 6.8 MPa) and aged conditions (6.9 ± 5.9 MPa) presented statistically lower bond strength results, while the SBMP adhesive resin, regardless of the resin cement type, presented the highest results (15.4 to 18.5 and 14.3 to 18.9 MPa) in both dry and aged conditions, respectively (Tukey's test). Conclusion: Application of a low-pH adhesive resin onto a hydrofluoric acid etched and silanized feldspathic ceramic surface in combination with chemically polymerized resin cement did not deliver favorable results. The use of adhesive resin with high pH could be clinically advised for the photo-, dual-, and chemically polymerized resin cements tested. © 2012 by the American College of Prosthodontists.

Effect of Post-silanization Heat Treatments of Silanized Feldspathic Ceramic on Adhesion to Resin Cement

Purpose: To evaluate the effect of post-silanization heat treatment of a silane agent and rinsing with hot water of silanized CAD/CAM feldspathic ceramic surfaces on the microtensile bond strength between resin cement and the ceramic, before and after mechanical cycling.Materials and Methods: Blocks measuring 10 x 5.7 x 3.25 mm(3) were produced from feldspathic ceramic cubes (VITA Mark II, VITA Zanhfabrik). Each ceramic block was duplicated in composite resin using a template made of polyvinylsiloxane impression material. Afterwards, ceramic and corresponding resin composite blocks were ultrasonically cleaned and randomly divided according to the 5 strategies used for conditioning the ceramic surface (n = 10): GHF: etching with hydrofluoric acid 10% + rinsing with water at room temperature + silanization at 20 degrees C; G20: silanization; G77: silanization + oven drying at 77 degrees C; G20r: silanization + hot water rinsing; G77r: silanization + oven drying at 77 C + hot water rinsing. The resin and ceramic blocks were cemented using a dual-curing resin cement. Every group was divided in two subgroups: aging condition (mechanical cycling, designated as a) or non-aging (designated as n). All the bonded assemblies were sectioned into microsticks for microtensile bond strength (mu TBS) testing. The failure mode of the tested specimens was assessed and mu TBS data were statistically analyzed in two ways: first 2-way ANOVA (GHF, G20 and G77 in non-aging/aging conditions) and 3-way ANOVA (temperature x rinsing x aging factors, excluding GHF), followed by Tukey's test (p = 0.05).Results: The 2-way ANOVA revealed that the mu TBS was significantly affected by the surface treatment (p < 0.001) but not by aging (p = 0.68), and Tukey's test showed that G77-n/G77-a (18.0 MPa) > GHF-n/GHF-a (12.2 MPa) > G20-n/G20-a (9.1 MPa). The 3-way ANOVA revealed that the mu TBS was significantly affected by the heat treatment and rinsing factors (p < 0.001), but not affected by aging (p = 0.36). The rinsing procedure decreased, while oven drying increased the bond strengths. Group G77, in both non-aging and aging conditions (18.6-17.4 MPa), had the highest bond values. Failure modes were mainly mixed for all groups.Conclusion: Oven drying at 77 degrees C improved the bond strength between the resin cement and feldspathic ceramic, but hot water rinsing reduced the bond strength and should not be recommended.

Effect of ceramic etching protocols on resin bond strength to a feldspar ceramic

This study sought to evaluate the resin micro-tensile bond strength (MTBS) stability of a leucite-reinforced ceramic after different ceramic etching protocols. The microtensile test had 40 ceramic blocks (5x5x6 mm) assigned to five groups (n=8), in accordance with the following surface etching protocols: NE nonetched (control); 9HF: hydrofluoric (HF) acid etching (9% HF)+wash/dry; 4HF: 4%HF+wash/dry; 5HF: 5%HF+wash/dry; and 5HF+N: 5%HF+neutralizer+wash/dry+ultrasonic-cleaning. Etched ceramic surfaces were treated with a silane agent. Next, resin cement blocks were built on the prepared ceramic surface and stored for 24 hours in distilled water at 37 degrees C. The specimens were then sectioned to obtain microtensile beams (32/block), which were randomly assigned to the following conditions, nonaged (immediate test) and aged (water storage for 150 days plus 12,000 thermal cycles), before the microtensile test. Bond strength data were submitted to one-way analysis of variance and Tukey test (alpha=0.05). Additional ceramic samples were subjected to the different ceramic etching protocols and evaluated using a scanning electron microscope (n=2) and atomic force microscopy (n=2). Aging led to a statistically significant decrease in the MTBS for all groups, except the untreated one (NE). Among the groups submitted to the same aging conditions, the untreated (NE) revealed inferior MTBS values compared to the 9HF and 4HF groups. The 5HF and 5HF+N groups had intermediate mean values, being statistically similar to the higher values presented by the 9HF and 4HF groups and to the lower value associated with the NE group. The neutralization procedure did not enhance the ceramic/resin cement bond strength. HF acid etching is a crucial step in resin/ceramic bonding.

Estudo da influência da temperatura de brasagem nas uniões zircônia/aço inox 304 utilizando metalização mecânica

Metal-Ceramic (M/C) Zirconia-stainless steel interfaces have been processed through brazing techniques due to the excellent combination of properties such as high temperature stability, high corrosion resistance and good mechanical properties. However, some M/C interfaces show some defects, like porosity and cracks results in the degradation of the interfaces, leading even to its total rupture. Most of time, those defects are associated with an improper brazing parameters selection to the M/C system. In this work, ZrO2 Y-TZP and ZrO2 Mg - PSZ were joint with the stainless steel grade 304 by brazing using a eutectic silver-copper (Ag28Cu) interlayer alloy with different thermal cycles. Ceramic surfaces were previous mechanically metallized with titanium to improve adhesion of the system. The effect of temperature on the M/C interface was studied. SEM-EDS and 3 point flexural bend test were performed to evaluate morphology, chemical composition and mechanical resistance of the M/C interfaces. Lower thermal cycle temperatures produced better results of mechanical resistance, and more regular/ homogeneous reaction layers between braze alloy and metal-ceramic surfaces. Also was proved the AgCu braze alloy activation in situ by titanium