Temporal evolution of sulfated zirconia sol-gel during dip coating: Analysis of mass drainage with time-varying refractive index

The formation of sulfated zirconia films from a sol-gel derived aqueous suspension is subjected to double-optical monitoring during batch dip coating. Interpretation of interferometric patterns, previously obscured by a variable refractive index, is now made possible by addition of its direct measurement by a polarimetric technique in real time. Significant sensitivity of the resulting physical thickness and refractive index curves (uncertainties of ±7 nm and ±0.005, respectively) to temporal film evolution is shown under different withdrawal speeds. As a first contribution to quantitative understanding of temporal film formation with varying nanostructure during dip coating, detailed analysis is directed to the stage of the process dominated by mass drainage, whose simple modeling with temporal t-1/2 dependence is verified experimentally. © 2006 Elsevier B.V. All rights reserved.

Microtensile bond strength of a resin cement to silica-coated and silanized in-ceram zirconia before and after aging

Purpose: This study compared the microtensile bond strength of resin-based cement (Panavia F) to silica-coated, silanized, glass-infiltrated high-alumina zirconia (In-Ceram Zirconia) ceramic in dry conditions and after various aging regimens. Materials and Methods: The specimens were placed in 1 of 4 groups: group 1: dry conditions (immediate testing without aging); group 2: water storage at 37°C for 150 days; group 3: 150 days of water storage followed by thermocycling (× 12,000, 5°C to 55°C); group 4: water storage for 300 days; group 5: water storage for 300 days followed by thermocycling. Results: Group 1 showed a significantly higher microtensile bond strength value (26.2 ± 1 MPa) than the other aging regimens (6.5 ± 1, 6.2 ± 2, 4.5 ± 1, 4.3 ± 1 MPa for groups 2, 3, 4, and 5, respectively) (P < .01). Conclusion: Satisfactory results were seen in dry conditions, but water storage and thermocycling resulted in significantly weaker bonds between the resin cement and the zirconia.

Adhesive cementation of zirconia posts to root dentin: Evaluation of the mechanical cycling effect

This study evaluated the effect of mechanical cycling on the bond strength of zirconia posts to root dentin. Thirty single-rooted human teeth were transversally sectioned to a length of 16 mm. The canal preparation was performed with zirconia post system drills (CosmoPost, Ivoclar) to a depth of 12 mm. For post cementation, the canals were treated with total-etch, 3-steps All-Bond 2 (Bisco), and the posts were cemented with Duolink dual resin cement (Bisco). Three groups were formed (n = 10): G1 - control, no mechanical cycling; G2 - 20,000 mechanical cycles; G3 - 2,000,000 mechanical cycles. A 1.6-mm-thick punch induced loads of 50 N, at a 45° angle to the long axis of the specimens and at a frequency of 8 Hz directly on the posts. To evaluate the bond strengths, the specimens were sectioned perpendicular to the long axis of the teeth, generating 2-mm-thick slices, approximately (5 sections per teeth), which were subjected to the push-out test in a universal testing machine at a 1 mm/min crosshead speed. The push-out bond strength was affected by the mechanical cycling (1-way ANOVA, p = .0001). The results of the control group (7.7 ± 1.3 MPa) were statistically higher than those of G2 (3.9 ± 2.2 MPa) and G3 (3.3 ± 2.3 MPa). It was concluded that the mechanical cycling damaged the bond strength of zirconia posts to root dentin.

Functional and esthetic rehabilitation with In-Ceram alumina and zirconia system: A multidisciplinary approach

The development of all-ceramic systems following metalceramics restorations allowed simulation of natural dentition due to favorable esthetics and resistance. In-Ceram is an alternative when esthetics is primordial as well as resistance required in rehabilitation. However, an ideal smile is associated to not only shape, color, texture and translucency but also harmony with gingival tissue. So, the aim of this study is to report a clinical case based on periodontal and fixed partial dentures principles to perform periodontal plastic surgery followed by esthetic rehabilitation. A female patient, 40-year-old, presented complaint about dental esthetics. After clinical and radiographic exams, metal-ceramics crowns (teeth 11, 12, 13, 21, 22 and 23) were considered unsatisfactory due to marginal leakage, color change in gingival tissue associated to metallic margin, and gummy smile. So, a crown lengthening surgery of anterior teeth was performed followed by rehabilitation of superior teeth with In-Ceram single crowns. Clinical significance: The interaction between periodontics and fixed prosthodontic area is the key of an adequated treatment planning which involves gingival smile to provide function and an esthetic condition in association with an esthetic, resistant and predictable material.

Design of microstructure of zirconia foams from the emulsion template properties

In this work, we investigate the correlations between structural and rheological properties of emulsified aqueous sol and the porous microstructure of monolithic zirconia foams, manufactured by the integrative combination of the sol-gel and emulsification processes. Macroporous zirconia ceramics prepared using different amounts of decahydronaphthalene, as oil phase, are compared in terms of the emulsion microstructure and ceramic porosity. A combination of electrical conductivity, oil droplet diameter, and rheological measurements was used to highlight the key effect of the dynamic structural properties of the emulsion on the porosity of the ceramic zirconia foam. The minimization of drying shrinkage by appropriate sol-gel mineralization of the oil droplet wall enabled versatile and easy tuning of the ceramic foam microstructure, by fine adjustment of the emulsion characteristics. The foam with the highest porosity (90%) and the lowest bulk density (0.40 g cm-3) was prepared from emulsion with 80 wt% of decahydronaphthalene, which also showed a bicontinuous structure and elevated flow consistency. © The Royal Society of Chemistry 2013.

Effect of air-particle abrasion protocols on the biaxial flexural strength, surface characteristics and phase transformation of zirconia after cyclic loading

This study evaluated the effect of air-particle abrasion protocols on the biaxial flexural strength, surface characteristics and phase transformation of zirconia after cyclic loading. Disc-shaped zirconia specimens (Ø: 15mm, thickness: 1.2mm) (N=32) were submitted to one of the air-particle abrasion protocols (n=8 per group): (a) 50μm Al2O3 particles, (b) 110μm Al2O3 particles coated with silica (Rocatec Plus), (c) 30μm Al2O3 particles coated with silica (CoJet Sand) for 20s at 2.8bar pressure. Control group received no air-abrasion. All specimens were initially cyclic loaded (×20,000, 50N, 1Hz) in water at 37°C and then subjected to biaxial flexural strength testing where the conditioned surface was under tension. Zirconia surfaces were characterized and roughness was measured with 3D surface profilometer. Phase transformation from tetragonal to monoclinic was determined by Raman spectroscopy. The relative amount of transformed monoclinic zirconia (FM) and transformed zone depth (TZD) were measured using XRD. The data (MPa) were analyzed using ANOVA, Tukey's tests and Weibull modulus (m) were calculated for each group (95% CI). The biaxial flexural strength (MPa) of CoJet treated group (1266.3±158A) was not significantly different than that of Rocatec Plus group (1179±216.4A,B) but was significantly higher than the other groups (Control: 942.3±74.6C; 50μm Al2O3: 915.2±185.7B,C). Weibull modulus was higher for control (m=13.79) than those of other groups (m=4.95, m=5.64, m=9.13 for group a, b and c, respectively). Surface roughness (Ra) was the highest with 50μm Al2O3 (0.261μm) than those of other groups (0.15-0.195μm). After all air-abrasion protocols, FM increased (15.02%-19.25%) compared to control group (11.12%). TZD also showed increase after air-abrasion protocols (0.83-1.07μm) compared to control group (0.59μm). Air-abrasion protocols increased the roughness and monoclinic phase but in turn abrasion with 30μm Al2O3 particles coated with silica has increased the biaxial flexural strength of the tested zirconia. © 2013 Elsevier Ltd.

Photoluminescence of core-shell nanoparticles made from yttrium stabilized zirconia powder grain coated with alumina

A YSZ@Al2O3 nanocomposite was obtained by Al 2O3 coating on the surface of yttrium stabilized zirconia via a polymeric precursor method. The resulting core-shell structures were characterized by X-ray diffraction, scanning electron microscopy, transmission electronic microscopy and PL spectra. The TEM micrographs clearly show a homogeneous Al2O3 shell around the ZrO2 core. The observed PL is related to surface-interface defects. Such novel technologies can, in principle, explore materials which are not available in the bulk single crystal form but their figure-of-merit is dramatically dependent on the surface-interface defect states. © 2013 This journal isThe Royal Society of Chemistry.

Liquid foam templates associated with the sol-gel process for production of zirconia ceramic foams

The unique properties of ceramic foams enable their use in a variety of applications. This work investigated the effects of different parameters on the production of zirconia ceramic foam using the sol-gel process associated with liquid foam templates. Evaluation was made of the influence of the thermal treatment temperature on the porous and crystalline characteristics of foams manufactured using different amounts of sodium dodecylsulfate (SDS) surfactant. A maximum pore volume, with high porosity (94%) and a bimodal pore size distribution, was observed for the ceramic foam produced with 10% SDS. Macropores, with an average size of around 30 μm, were obtained irrespective of the SDS amount, while the average size of the supermesopores increased systematically as the SDS amount was increased up to 10%, after which it decreased. X-ray diffraction analyses showed that the sample treated at 500 °C was amorphous, while crystallization into a tetragonal metastable phase occurred at 600 °C due to the presence of sulfate groups in the zirconia structure. At 800 and 1000 °C the monoclinic phase was observed, which is thermodynamically stable at these temperatures. © 2013 by the authors; licensee MDPI, Basel, Switzerland.

Air-particle abrasion on zirconia ceramic using different protocols: Effects on biaxial flexural strength after cyclic loading, phase transformation and surface topography

This study evaluated the effect of different air-particle abrasion protocols on the biaxial flexural strength and structural stability of zirconia ceramics. Zirconia ceramic specimens (ISO 6872) (Lava, 3M ESPE) were obtained (N=336). The specimens (N=118, n=20 per group) were randomly assigned to one of the air-abrasion protocols: Gr1: Control (as-sintered); Gr2: 50 μm Al2O3 (2.5 bar); Gr3: 50 μm Al2O3 (3.5 bar); Gr4: 110 μm Al2O3(2.5 bar); Gr5: 110 μm Al2O3 (3.5 bar); Gr6: 30 μm SiO2 (2.5 bar) (CoJet); Gr7: 30 μm SiO2(3.5 bar); Gr8: 110 μm SiO2 (2.5 bar) (Rocatec Plus); and Gr9: 110 μm SiO2 (3.5 bar) (duration: 20 s, distance: 10 mm). While half of the specimens were tested immediately, the other half was subjected to cyclic loading in water (100,000 cycles; 50 N, 4 Hz, 37 °°C) prior to biaxial flexural strength test (ISO 6872). Phase transformation (t→m), relative amount of transformed monoclinic zirconia (FM), transformed zone depth (TZD) and surface roughness were measured. Particle type (p=0.2746), pressure (p=0.5084) and cyclic loading (p=0.1610) did not influence the flexural strength. Except for the air-abraded group with 110 μm Al2O3 at 3.5 bar, all air-abrasion protocols increased the biaxial flexural strength (MPa) (Controlnon-aged: 1030±153, Controlaged: 1138±138; Experimentalnon-aged: 1307±184-1554±124; Experimentalaged: 1308±118-1451±135) in both non-aged and aged conditions, respectively. Surface roughness (Ra) was the highest with 110 μm Al2O3(0.84 μm. FM values ranged from 0% to 27.21%, higher value for the Rocatec Plus (110 μm SiO2) and 110 μm Al2O3 groups at 3.5 bar pressure. TZD ranged between 0 and 1.43 μm, with the highest values for Rocatec Plus and 110 μm Al2O3 groups at 3.5 bar pressure. © 2013 Elsevier Ltd.

Processo de preparação de zirconia dopada e não dopada pela rota sol-gel usando nitrato de zirconila como material de partida

Processo de Preparação de Zirconia Dopada e não Dopada pela Rota Sol-Gel Usando Nitrato de Zirconila como Material de Partida compreendendo as etapas de preparação de uma solução de nitratos de zirconila e outros nitratos metálicos em solução aquosa com composto orgânico de etanol metanol ou acetona, através do controle de molaridade. Embora não limitantes, valores ideais para molaridade das soluções são: entre 1,00 e 0,29 para obtenção de pó entre 0,29 e 0,18 para obtenção de superfície recoberta e entre 0,18 e 0,13 para obtenção de filmes finos. Manter a solução a 0°C para formação de filmes finos por imersão do substrato ou monocristal com velocidade constante ("dip-coating") ou por rotação a velocidade constante ("spinning"), ou para recobrimento de superfícies metálicas através de imersões sucessivas do substrato metálico a velocidade constante ("dip-coating"). Elevar a solução a 50°C para hidrolização e formação de um gel em forma de pó, secagem de pó ou liofilização, calcinação e moagem dos aglomerados.

Efficacy of Surface Treatments on the Bond Strength of Resin Cements to Two Brands of Zirconia Ceramic

Purpose: To compare the shear bond strength (SBS) of two cements to two Y-TZP ceramics subjected to different surface treatments.Materials and Methods: Zirconia specimens were made from Lava (n = 36) and IPS e.max ZirCAD (n = 36), and their surfaces were treated as follows: no treatment (control), silica coating with 30-mu m silica-modified alumina (Al2O3) particles (CoJet Sand), or coating with liners Lava Ceram for Lava and Intensive ZirLiner for IPS e.max ZirCAD. Composite resin cylinders were bonded to zirconia with Panavia F or RelyX Unicem resin cements. All specimens were thermocycled (6000 cycles at 5 degrees C/55 degrees C) and subjected to SBS testing. Data were analyzed by post-hoc test Tamhane T2 and Scheffe tests (alpha = 0.05). Failure mode was analyzed by stereomicroscope and SEM.Results: With both zirconia brands, CoJet Sand showed significantly higher SBS values than control groups only when used with RelyX Unicem (p = 0.0001). Surface treatment with liners gave higher SBS than control groups with both ceramic brands and cements (p < 0.001). With both zirconia brands, the highest SBS values were obtained with the CoJet and RelyX Unicem combination (> 13.47 MPa). Panavia F cement showed significantly better results when coupled with liner surface treatment rather than with CoJet (p = 0.0001, SBS > 12.23 MPa). In untreated controls, Panavia F showed higher bond strength than RelyX Unicem; the difference was significant (p = 0.016) in IPS e.max ZirCAD. The nontreated specimens and those treated with CoJet Sand exhibited a high percentage of adhesive and mixed A (primarily adhesive) failures, while the specimens treated with liners presented an increase in mixed A and mixed C (primarily cohesive) failures as well as some cohesive failure in the bulk of Lava Ceram for both cements.Conclusion: CoJet Sand and liner application effectively improved the SBS between zirconia and luting cements. This study suggests that different interactions between surface treatments and luting cements yield different SBS: in clinical practice, these interactions should be considered when combining luting cements with surface treatments in order to obtain the maximum bond strength to zirconia restorations.

Evaluation of Resin Bond Strength to Yttria-stabilized Tetragonal Zirconia and Framework Marginal Fit: Comparison of Different Surface Conditionings

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

Effect of Surface Conditioning Modalities on the Repair Bond Strength of Resin Composite to the Zirconia Core / Veneering Ceramic Complex

Purpose: This study evaluated the effect of different surface conditioning protocols on the repair strength of resin composite to the zirconia core / veneering ceramic complex, simulating the clinical chipping phenomenon.Materials and Methods: Forty disk-shaped zirconia core (Lava Zirconia, 3M ESPE) (diameter: 3 mm) specimens were veneered circumferentially with a feldspathic veneering ceramic (VM7, Vita Zahnfabrik) (thickness: 2 mm) using a split metal mold. They were then embedded in autopolymerizing acrylic with the bonding surfaces exposed. Specimens were randomly assigned to one of the following surface conditioning protocols (n = 10 per group): group 1, veneer: 4% hydrofluoric acid (HF) (Porcelain Etch) + core: aluminum trioxide (50-mu m Al2O3) + core + veneer: silane (ESPE-Sil); group 2: core: Al2O3 (50 mu m) + veneer: HF + core + veneer: silane; group 3: veneer: HF + core: 30 mu m aluminum trioxide particles coated with silica (30 mu m SiO2) + core + veneer: silane; group 4: core: 30 mu m SiO2 + veneer: HF + core + veneer: silane. Core and veneer ceramic were conditioned individually but no attempt was made to avoid cross contamination of conditioning, simulating the clinical intraoral repair situation. Adhesive resin (VisioBond) was applied to both the core and the veneer ceramic, and resin composite (Quadrant Posterior) was bonded onto both substrates using polyethylene molds and photopolymerized. After thermocycling (6000 cycles, 5 degrees C-55 degrees C), the specimens were subjected to shear bond testing using a universal testing machine (1 mm/min). Failure modes were identified using an optical microscope, and scanning electron microscope images were obtained. Bond strength data (MPa) were analyzed statistically using the non-parametric Kruskal-Wallis test followed by the Wilcoxon rank-sum test and the Bonferroni Holm correction (alpha = 0.05).Results: Group 3 demonstrated significantly higher values (MPa) (8.6 +/- 2.7) than those of the other groups (3.2 +/- 3.1, 3.2 +/- 3, and 3.1 +/- 3.5 for groups 1, 2, and 4, respectively) (p < 0.001). All groups showed exclusively adhesive failure between the repair resin and the core zirconia. The incidence of cohesive failure in the ceramic was highest in group 3 (8 out of 10) compared to the other groups (0/10, 2/10, and 2/10, in groups 1, 2, and 4, respectively). SEM images showed that air abrasion on the zirconia core only also impinged on the veneering ceramic where the etching pattern was affected.Conclusion: Etching the veneer ceramic with HF gel and silica coating of the zirconia core followed by silanization of both substrates could be advised for the repair of the zirconia core / veneering ceramic complex.

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.

Silica-based Nano-coating on Zirconia Surfaces Using Reactive Magnetron Sputtering: Effect on Chemical Adhesion of Resin Cements

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