Can Heat Treatment Procedures of Pre-hydrolyzed Silane Replace Hydrofluoric Acid in the Adhesion of Resin Cement to Feldspathic Ceramic?

Purpose: To evaluate the influence of heat treatment (HT) procedures of a pre-hydrolyzed silane on bond strength of resin cement to a feldspathic ceramic.Materials and Methods: Ceramic and composite blocks (N = 30) were divided into six groups (n = 5) and subjected to the following conditioning procedures: G1: 9.6% hydrofluoric acid (HF) for 20 s + silane (RelyX Ceramic Primer, 3M ESPE) + resin cement (Panavia F2.0, Kuraray) (control); G2: HF (20 s) + silane + heat treatment in furnace (HTF) (100 degrees C, 2 min) + resin cement; G3: silane + HTF + resin cement; G4-HF (20 s) + silane + heat treatment with hot air (HTA) (50 +/- 5 degrees C for 1 min) + resin cement; G5: silane + HTA + resin cement; G6: silane + resin cement. The microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using a stereomicroscope and SEM to categorize the failure types. The data were statistically evaluated using one-way ANOVA and Tukey's test (5%).Results: The control group (G1) showed no pre-test failures and presented significantly higher mean MTBS (16.01 +/- 1.12 MPa) than did other groups (2.63 +/- 1.05 to 12.55 +/- 1.52 MPa) (p = 0.0001). In the groups where HF was not used, HTF (G3: 12.55 +/- 1.52 MPa) showed significantly higher MTBS than did HTA (G5: 2.63 +/- 1.05 MPa) (p < 0.05). All failure types were mixed, ie, adhesive between the resin cement and ceramic accompanied by cohesive failure in the cement.Conclusion: Heat treatment procedures for the pre-hydrolyzed silane either in a furnace or with the application of hot air cannot replace the use of HF gel for the adhesion of resin cement to feldspathic ceramic. Yet when mean bond strengths and incidence of pre-test failures are considered, furnace heat treatment delivered the second best results after the control group, being considerably better than hot air application.

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 Resin Cement Type on the Microtensile Bond Strength to Lithium Disilicate Ceramic and Dentin Using Different Test Assemblies

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of the Etching Duration and Ultrasonic Cleaning on Microtensile Bond Strength Between Feldspathic Ceramic and Resin Cement

This study assessed the effect of different etching durations of feldspathic ceramic with hydrofluoric acid (HF) and ultrasonic cleaning of the etched ceramic surface on the microtensile bond strength stability of resin to a feldspathic ceramic. The research hypotheses investigated were: (1) different etching times would not affect the adhesion resistance and (2) ultrasonic cleaning would improve the adhesion. Ceramic blocks (6 x 6 x 5 mm) (N = 48) were obtained. The cementations surfaces were duplicated in resin composite. The six study groups (n = 8) were: G1Etching with 10% aqueous HF (30 s) + silane; G 210% HF (1 min) + silane; G3-10% HF (2 min) + silane; G4-10% HF (30 s) + ultrasonic cleaning (4 min) in distilled water + silane; G5-10% HF (1 min) + ultrasonic cleaning + silane; G6-10% HF (2 min) ultrasonic cleaning + silane. The cemented blocks were sectioned into microbars for the microtensile test. The etching duration did not create significant difference among the groups (p = .156) but significant influence of ultrasonic cleaning was observed (p = .001) (Two-way ANOVA and Tukey's test, p > 0.05). All the groups after ultrasonic cleaning presented higher bond strength (19.38-20.08 MPa) when compared with the groups without ultrasonic cleaning (16.2117.75 MPa). The bond strength between feldspathic ceramic and resin cement was not affected by different etching durations using HF. Ultrasonic cleaning increased the bond strength between ceramic surface and resin cement, regardless of the etching duration.

Influence of air-particle deposition protocols on the surface topography and adhesion of resin cement to zirconia

Objectives: This study evaluated the influence of air-particle abrasion protocols on the surface roughness (SR) of zirconia and the shear bond strength (SBS) of dual-polymerized resin cement to this ceramic. Materials and methods. Sintered zirconia blocks (n = 115) (Lava, 3M ESPE) were embedded in acrylic resin and polished. The specimens were divided according to the 'particle type' (Al: 110 mu m Al2O3; Si: 110 mu m SiO2) and 'pressure' factors (2.5 or 3.5 bar) (n = 3 per group): (a) Control (no air-abrasion); (b) Al2.5; (c) Si2.5; (d) Al3.5; (e) Si3.5. SR (Ra) was measured 3-times from each specimen after 20 s of air-abrasion (distance: 10 mm) using a digital optical profilometer. Surface topography was evaluated under SEM analyses. For the SBS test, 'particle type', 'pressure' and 'thermocycling' (TC) factors were considered (n = 10; n = 10 per group): Control (no air-abrasion); Al2.5; Si2.5; Al3.5; Si3.5; Control(TC); Al2.5(TC); Si2.5(TC); Al3.5(TC); Si3.5(TC). After silane application, resin cement (Panavia F2.0) was bonded and polymerized. Specimens were thermocycled (6.000 cycles, 5-55 degrees C) and subjected to SBS (1 mm/min). Data were analyzed using ANOVA, Tukey's and Dunnett tests (5%). Results. 'Particle' (p = 0.0001) and 'pressure' (p = 0.0001) factors significantly affected the SR. All protocols significantly increased the SR (Al2.5: 0.45 +/- 0.02; Si2.5: 0.39 +/- 0.01; Al3.5: 0.80 +/- 0.01; Si3.5: 0.64 +/- 0.01 mu m) compared to the control group (0.16 +/- 0.01 mu m). For SBS, only 'particle' factor significantly affected the results (p = 0.015). The SiO2 groups presented significantly higher SBS results than Al2O3 (Al2.5: 4.78 +/- 1.86; Si2.5: 7.17 +/- 2.62; Al3.5: 4.97 +/- 3.74; Si3.5: 9.14 +/- 4.09 MPa) and the control group (3.67 +/- 3.0 MPa). All TC specimens presented spontaneous debondings. SEM analysis showed that Al2O3 created damage in zirconia in the form of grooves, different from those observed with SiO2 groups. Conclusions. Air-abrasion with 110 mu m Al2O3 resulted in higher roughness, but air-abrasion protocols with SiO2 promoted better adhesion.

Bonding of Y-TZP to Dentin: Effects of Y-TZP Surface Conditioning, Resin Cement Type, and Aging

Purpose: To evaluate the effects of two surface treatments, aging, and two resin cements on shear bond strength between dentin and yttrium-stabilized tetragonal zirconia polycrystal ceramic (Y-TZP).Materials and Methods: Eighty human molars were embedded in acrylic resin and sectioned 3 mm below the occlusal plane. These teeth and 80 cylindrical Y-TZP specimens (height, 4 mm; diameter, 3.4 mm) were divided into eight groups (n=10) using the following factors: Y-TZP surface treatment (Vi: low-fusing porcelain [vitrification] + hydrofluoric acid etching + silanization or Si: tribochemical silicatization); cementation strategies (PF: Pan avia or CC: Clearfil); and storage (nonaging or aging). Bonding surfaces of 40 Y-TZP specimens received Vi treatment, and the rest received Si treatment. Half of the ceramic-tooth assemblies were cemented with Panavia, the rest with Clearfil. Shear tests were executed using 0.4-mm-thick wire at 0.5 mm/min. Data were analyzed by three-way analysis of variance and Tukey test (alpha=0.05). Fractures were analyzed.Results: Y-TZP surface treatments did not affect bond strength (p=0.762, Vi = Si), while resin cements (p<0.001, Panavia > Clearfil) and aging (p=0.006, nonaging > aging) showed a significant effect. Most failures were in adhesive at dentin-cement interfaces; no failure occurred between zirconia and cement.Conclusion: When Y-TZP ceramic is bonded to dentin, the weakest interface is that between dentin and resin cement. The resin cement/Y-TZP interface was less susceptible to failures, owing to Y-TZP surface treatments.

Microparticulated and nanoparticulated zirconium oxide added to calcium silicate cement: Evaluation of physicochemical and biological properties

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Biocompatibility of New Calcium Aluminate Cement: Tissue Reaction and Expression of Inflammatory Mediators and Cytokines

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

Effect of surface treatment on the bond strength between yttria partially stabilized zirconia ceramics and resin cement

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Iliac osteosynthesis with nylon clamp associated to polymethylmethacrylate bone cement - experimental study in dogs cadavers

Fractures of iliac body are generally consequences of traumas of great impact. These fractures lead to a lack of locomotor response and in specific cases, surgery is needed. Among the possible therapeutic lines, implants become a good option. In this paper, the authors used dog corpses to develop a surgery technique of iliac osteosynthesis, employing nylon clamps and bone cement of polymethylmethacrylate (PMMA). Sixteen hemi pelvises of eight dog corpses, which had its iliac bodies totally fractured previously, were utilized. The osteosynthesis was reached through the implantation of six nylon clamps, distributed equally between the bone fragments. With the use of the nylon clamps there were bone realignment and a contact surface to fixation of the biomaterial. The technique developed in corpses was easily executed, effective in reduction, alignment and stabilization of the fracture. The authors suggest more studies in vitro to evaluate immobilization resistance and functionality in dogs with this condition.

Incorporation of chlorhexidine gluconate or diacetate into a glass-ionomer cement: porosity, surface roughness, and anti-biofilm activity

To evaluate the porosity, surface roughness and anti-biofilm activity of a glass-ionomer cement (GIC) after incorporation of different concentrations of chlorhexidine (CHX) gluconate or diacetate. Methods: For the porosity and surface roughness tests, 10 test specimens were fabricated of the GIC Ketac Molar Easy Mix (KM) and divided into the following groups: Control, GIC and 0.5% CHX diacetate; GIC and 1.0% CHX diacetate; GIC and 2.0% CHX diacetate; GIC and 0.5% CHX gluconate; GIC and 1.0% CHX gluconate; GIC and 2.0% CHX gluconate. To evaluate porosity, the test specimens were fractured. The fragments were photographed by scanning electron microscopy (SEM), and the images analyzed with the aid of the software program Image J. The surface roughness (Ra) was obtained by the mean value of three readouts performed on the surface of each specimen, always through the center. To analyze the anti-biofilm activity, strains of S. mutans ATCC 35688 were used, and the groups control and GIC +CHX diacetate 1% were divided as follows: GIC (1 day); GIC (7 days), GIC (14 days), GIC (21 days); GIC+CHX (1 day), GIC+CHX (7 days), GIC+CHX (14 days), GIC+CHX (21 days); GIC+ CHX (1 day), GIC+ CHX (7 days), GIC+ CHX (14 days) and GIC+ CHX (21 days) using 10 test specimens per group. For biofilm growth, the specimens were placed in a vertical position in 24-well plates and incubated overnight 10 times. The culture medium was renewed every 24 hours. The suspension was diluted and seeded on BHI agar for quantification of the bacteria present. For evaluation of all the tests the two-way ANOVA was used, and if necessary, the Tukey test was applied, with a level of significance of 5%. Results: Regarding GIC porosity, the ANOVA showed that the presence of CHX increased the porosity (P< 0.001) proportionally to the increase in concentrations (P= 0.001), without however, presenting interaction between material and concentration (P= 0.705). Regarding the number of pores, a significant increase in pores was observed with the increase in CHX concentration (P= 0.003). The surface roughness test demonstrated no statistically significant effect as to increase or reduction in roughness at any of the CHX concentrations used (P> 0.05). Anti-biofilm activity analysis pointed out a significant effect of the factors material (P= 0.006) and time (P< 0.001), with CHX diacetate CHX presenting greater effectiveness in reducing microorganisms.

Repair of Bone Defects Filled with New Calcium Aluminate Cement (EndoBinder)

The aim of this study was to evaluate and compare the repair of bone defects filled with calcium aluminate cement (EndoBinder), mineral trioxide aggregate (MTA), and calcium hydroxide. Methods After mixing, the cements were inserted into bone defects (3.3 mm) mechanically created in the right and left tibias of 30 rats (Rattus norvegicus, Wistar). In the control group, the bone defects were filled with blood clot of the animal itself. After time intervals of 7, 30, and 90 days had elapsed, bone tissue biopsies (n = 5) were surgically obtained and submitted to laboratory processing. The response of bone tissue in contact with the materials was microscopically analyzed. The percentage of neoformed bone tissue in the defect was determined by means of planimetry counting points superimposed on the histologic image. Results Significant increase in the percentage of neoformed bone tissue was observed throughout the experimental periods in all groups (P < .05). For the cements EndoBinder and MTA (30 and 90 days), these percentage values were statistically higher than those of the control group (P < .05); however, they were similar to those of calcium hydroxide (P > .05). Conclusions EndoBinder and MTA allowed complete repair of bone defects created in rat tibias.

Air abrasion before and/or after zirconia sintering: surface characterization, flexural strength, and resin cement bond strength

The purpose of this in vitro study was to evaluate the effect of air-abrasion/zirconia sintering order on the yttria partially stabilized tetragonal zirconia polycrystal (Y-TZP) surface characterization (roughness, morphology, and phase transformation), flexural strength (FS), and shear bond strength (SBS) to a resin cement. Y-TZP specimens were air abraded with 50-μm Al2O3 particles after (AS), before (BS), or before and after zirconia sintering (BAS). For roughness (Ra), 30 block specimens (12×12×3.0 mm; n=10) had their surfaces analyzed by a profilometer. Next, on the air-abraded surfaces of these specimens, composite resin discs (n=30) were bonded with RelyX ARC. The bonded specimens were stored for 24 hours in distilled water at 37°C before shear testing. Failure mode was determined with a stereomicroscope (20×). The surface morphology (n=2) was evaluated by SEM (500×). For the four-point flexural strength test (EMIC DL2000), 39 bar-shaped specimens (20×4.0×1.2 mm; n=13) were air abraded according to the three conditions proposed, and an additional group (nonabraded) was evaluated (n=13). The quantitative analysis of phase transformation (n=1) was completed with Rietveld refinement with X-ray diffraction data. Ra (μm) and SBS (MPa) data were analyzed by one-way analysis of variance (ANOVA) and the Tukey test (α=0.05). Pearson correlation analysis was used to determine if there was a correlation between roughness and SBS. For FS (MPa) data, one-way ANOVA and the Dunnett C-test (α=0.05) were used. The air-abrasion/zirconia sintering order influenced significantly (p<0.001) Ra, SBS, and FS. The BS and AS groups presented the highest (1.3 μm) and the lowest (0.7 μm) Ra. The highest SBS (7.0 MPa) was exhibited by the BAS group, followed by the AS group (5.4 MPa) and finally by the BS group (2.6 MPa). All groups presented 100% adhesive failure. A weak correlation (r=−0.45, p<0.05) was found between roughness and SBS. The air-abrasion/zirconia sintering order provided differences in the surface morphology. The nonabraded (926.8 MPa) and BS (816.3 MPa) groups exhibited statistically similar FS values but lower values than the AS (1249.1 MPa) and BAS (1181.4 MPa) groups, with no significant difference between them. The nonabraded, AS, BS, and BAS groups exhibited, respectively, percentages of monoclinic phase of 0.0 wt%, 12.2 wt%, 0.0 wt%, and 8.6 wt%. The rougher surface provided by the air-abrasion before zirconia sintering may have impaired the bonding with the resin cement. The morphological patterns were consistent with the surface roughness. Considering the short-term SBS and FS, the BAS group exhibited the best performance. Air abrasion, regardless of its performance order, provides tetragonal to monoclinic transformation, while sintering tends to zero the monoclinic phase content.

Interference of the assessment method in pH values of an epoxy-based cement

Introduction: Alkalinization potential is a fundamental property of endodontic epoxy-based cements containing calcium hydroxide. Studies have shown discrepant pH results for same materials at different evaluation periods. A possible reason accounting for these differences may be the assessment procedures. Objective: To evaluate the pH value of an epoxy-based cement (Sealer 26) in different periods of analysis, using two assessment methods. Material and methods: Sealer 26 was manipulated and immediately placed into polyethylene tubes (n=10, each group) and immersed in distilled water. In G1, the tubes were kept in the same water during all experiment; and in G2, the tubes were removed and placed into another flask with an equal amount of water after the pH evaluation. The pH of these solutions was measured at 24 hours, 7, 14 and 28 days. Analysis were made within the same group according to the experimental periods and between groups in each experimental period. Data were submitted to ANOVA (α = 5%) and t test, respectively. Results: For G1 and G2, all periods showed different pH values (p < 0.05), except between 14 and 28 days (p > 0.05) and between 7 and 14 days (p > 0.05), respectively. In each period, no significant differences were observed between the groups. Conclusion: The method to obtain the pH values in different experimental periods no interfered in the final results. However, difference was observed when the results were analyzed at same group.

Evaluation of the physicochemical properties and push-out bond strength of mta-based root canal cement

Aim: This study investigated the flowability, setting time, pH, calcium release and bond strength of a MTA-based cement (MTA Fillapex®) compared to AH Plus and Sealapex. Materials and methods: For the flowability test, the ISO 6876:2001 specification was utilized and for the setting time test, the ASTM C266-03 specification was utilized. For the pH and calcium release measurements, 10 samples were prepared for each group and analyzed for several different periods. For the push-out test, dentin disks were distributed into three groups, according to the cement utilized and into three subgroups, according to the root third (n = 10). After obturation, the specimens underwent push-out testing. The data were compared statistically using a significance level of 5%. Results: The flowability of all materials was found to be similar (p > 0.05). The setting times were different among the groups tested (MTA Fillapex < Sealapex < AH Plus) (p < 0.05). At days 7 and 28, the MTA Fillapex presented the higher pH values (p < 0.05). At 24 hours and at 14 days, the calcium release of the MTA Fillapex was similar to that of Sealapex (p > 0.05). AH Plus presented the lowest pH and calcium release values (p < 0.05). In all root thirds, the adhesion to the dentin of the MTA Fillapex and Sealapex were significantly lower than that of AH Plus (p < 0.05). Conclusion: MTA Fillapex and Sealapex presented several similar properties and both were found to be different than AH Plus. Clinical significance: This study evaluated the physicochemical and mechanical properties of new MTA-based root canal cement, in order to use this scaler in root canal fillings. MTA Fillapex showed satisfactory properties for clinical use.