João Paulo Barros Machado

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, Tukeys tests and Weibull modulus (m) were calculated for each group (95% CI). The biaxial flexural strength (MPa) of CoJet treated group (1266.3±158(A)) was not significantly different than that of Rocatec Plus group (1179±216.4(A,B)) but was significantly higher than the other groups (Control: 942.3±74.6(C); 50μm Al2O3: 915.2±185.7(B,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.

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: 1,030 ± 153, Controlaged: 1,138 ± 138; Experimentalnon-aged: 1,307 ± 184-1,554 ± 124; Experimentalaged: 1,308 ± 118-1,451 ± 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.

Effects of aging procedures on the topographic surface, structural stability, and mechanical strength of a ZrO2-based dental ceramic

OBJECTIVE To determine the effects of different aging methods on the degradation and flexural strength of yttria-stabilized tetragonal zirconia (Y-TZP) METHODS: Sixty disc-shaped specimens (∅, 12mm; thickness, 1.6mm) of zirconia (Vita InCeram 2000 YZ Cubes, VITA Zahnfabrik) were prepared (ISO 6872) and randomly divided into five groups, according to the aging procedures (n=10): (C) control; (M) mechanical cycling (15,000,000 cycles/3.8Hz/200N); (T) thermal cycling (6,000 cycles/5-55°C/30s); (TM) thermomechanical cycling (1,200,000 cycles/3.8Hz/200N with temperature range from 5°C to 55°C for 60s each); (AUT) 12h in autoclave at 134°C/2bars; and (STO) storage in distilled water (37°C/400 days). After the aging procedures, the monoclinic phase percentages were evaluated by X-ray diffraction (XRD), and topographic surface analysis was performed by 3D profilometry. The specimens were then subjected to biaxial flexure testing (1mm/min, load 100kgf, in water). The biaxial flexural strength data (MPa) were analyzed by 1-way ANOVA and Tukeys test (α=0.05). The data for monoclinic phase percentage and profilometry (Ra) were analyzed by Kruskal-Wallis and Dunns tests. RESULTS ANOVA revealed that flexural strength was affected by the aging procedures (p=0.002). The M (781.6MPa) and TM (771.3MPa) groups presented lower values of flexural strength than did C (955MPa), AUT (955.8MPa), T (960.8MPa) and STO (910.4MPa). The monoclinic phase percentage was significantly higher only for STO (12.22%) and AUT (29.97%) when compared with that of the control group (Kruskal-Wallis test, p=0.004). In addition, the surface roughnesses were similar among the groups (p=0.165). SIGNIFICANCE Water storage for 400 days and autoclave aging procedures induced higher phase transformation from tetragonal to monoclinic; however, they did not affect the flexural strength of Y-TZP ceramic, which decreased only after mechanical and thermomechanical cycling.

Microstructure characterization and SCG of newly engineered dental ceramics.

OBJECTIVES The aim of this study was to characterize the microstructure of four dental CAD-CAM ceramics and evaluate their susceptibility to stress corrosion. METHODS SEM and EDS were performed for microstructural characterization. For evaluation of the pattern of crystallization of the ceramics and the molecular composition, XRD and FTIR, respectively, were used. Elastic modulus, Poissons ratio, density and fracture toughness were also measured. The specimens were subjected to biaxial flexure under five stress rates (0.006, 0.06, 0.6, 6 and 60MPa/s) to determine the subcritical crack growth parameters (n and D). Twenty-five specimens were further tested in mineral oil for determination of Weibull parameters. Two hundred forty ceramic discs (12mm diameter and 1.2mm thick) were made from four ceramics: feldspathic ceramic - FEL (Vita Mark II, Vita Zahnfabrik), ceramic-infiltrated polymer - PIC (Vita Enamic, Vita Zahnfabrik), lithium disilicate - LD (IPS e.max CAD, Ivoclar Vivadent) and zirconia-reinforced lithium silicate - LS (Vita Suprinity, Vita Zahnfabrik). RESULTS PIC discs presented organic and inorganic phases (n=29.1±7.7) and Weibull modulus (m) of 8.96. The FEL discs showed n=36.6±6.8 and m=8.02. The LD discs showed a structure with needle-like disilicate grains in a glassy matrix and had the lowest value of n (8.4±0.8) and m=6.19. The ZLS discs showed similar rod-like grains, n=11.2±1.4 and m=9.98. SIGNIFICANCE The FEL and PIC discs showed the lowest susceptibility to slow crack growth (SCG), whereas the LD and ZLS discs presented the highest. PIC presented the lowest elastic modulus and no crystals in its composition, while ZLS presented tetragonal zirconia. The overall strength and SCG of the new materials did not benefit from the additional phase or microconstituents present in them.

Sonocatalytic Degradation of Methylene Blue in the Presence of TiO2 Doped Carbon Nanostructures—Catalytic and Adsorption Comparison by Different Carbon Forms

The main objective of this work was to evaluate nanocomposites formed by TiO2-CNT (carbon nanotube) and TiO2-C (resorcinol/formaldehyde) via a sonocatalytic process. The synthesis of composites was performed by the sol-gel method using titanium isopropoxide (Ti(OPr)4-TTIP), acetic acid and ethylene glycol as dispersing medium. Ultrasound was used as the irradiation source and methylene blue was chosen as a model substance. In addition, the adsorption capacity was studied in an attempt to achieve greater ratio degradation/adsorption. The methylene blue concentration after adsorption and sonocatalysis was investigated by UV–vis spectroscopy. It was found that adsorption was an important factor to achieve high degradation capacity. However, the sonocatalytic activity decreased when adsorption was too intense.

Development, heat treatment optimization and microstructural characterization of Nb/sub 3/Sn superconductor wire

The optimization of the heat treatment profile for Nb/sub 3/Sn superconductor wires is one of the most difficult steps to process this material. The present work had the objective to optimize the heat treatment profile to form the Nb/sub 3/Sn phase. It was developed an internal-tin Nb/sub 3/Sn strand with 1.0 mm in diameter, 12 065 Nb filaments with average diameter of 3.4 /spl mu/m, 26 cores of Sn and internal stabilization of Cu surrounded by Ta diffusion barrier. Samples were removed for heat treatment optimization using different profiles to analyze the Sn diffusion and CuSn formation at temperatures up to 575 /spl deg/C. A final treatment at 700 /spl deg/C was used to form the Nb/sub 3/Sn phase. After the heat treatments, samples were removed for microstructural characterization. Measurements of T/sub c/ and J/sub c/ were performed to analyze the influence of the heat treatments on the superconducting phase and on the transport properties. It was concluded that the use of a two step heat treatment of 575 /spl deg/C/100 h + 700 /spl deg/C/100 h is as efficient as the use of a heat treatment with more low temperature steps.

Quantitative phase analysis from X-ray diffraction in Y-TZP dental ceramics: A critical evaluation

UNLABELLED The dentistry literature shows consensus to use the Garvie and Nicholson equation modified by Toraya to quantify the Y-TZP phase transformation. However, this method does not include the possibility of cubic phase transformation and crystallographic texture after artificial ageing, and in this case, it is possible to observe errors of quantification. OBJECTIVES The aim of this study was to evaluate a dental Y-TZP ageing kinetic of phase transformation under pressure and hydrothermal conditions (130°C, 2bar) and to compare the methods of quantification by the equation of Garvie and Nicholson modified by Toraya and the Rietveld refinement method. METHODS Discs of Y-TZP (12mm Ø×1.2mm in height) were divided into groups (n=4) according to the ageing times (in the range of 6 and 138h). The superficial characterisation was made using SEM and the XDR for crystallographic analysis. RESULTS An aggressive superficial degradation process at the beginning of phase transformation in 6-10h of ageing was observed by SEM. The phase transformation quantification showed differences between the methods. It was observed the increase and stabilisation of monoclinic phase until 80% at 40h of ageing by the Garvie and Nicholson modified by Toraya equation, compared to 60% of monoclinic phase and approximately 30% of cubic phase observed by the Rietveld method. CONCLUSION The Toraya equation showed an overestimated result of monoclinic quantification compared to the Rietveld method. CLINICAL SIGNIFICANCE The overestimated result of monoclinic phase could lead to different interpretation about the dental Y-TZP ageing process.

A new silica-infiltrated Y-TZP obtained by the sol-gel method

OBJECTIVE The aim of this study was to evaluate silica infiltration into dental zirconia (VITA In-Ceram 2000 YZ, Vita Zahnfabrik) and its effects on zirconias surface characteristics, structural homogeneity and bonding to a resin cement. METHODS Infiltration was performed by immersion of the pre-sintered zirconia specimens in silica sols for five days (ZIn). Negative (pure zirconia specimens, ZCon-) and positive controls (specimens kept in water for 5 days, ZCon+) were also performed. After sintering, the groups were evaluated by X-ray diffraction (XRD), grazing angle X-ray diffraction (DRXR), scanning electron microscopy (SEM), contact angle measurements, optical profilometry, biaxial flexural test and shear bonding test. Weibull analysis was used to determine the Weibull modulus (m) and characteristic strength (σ0) of all groups. RESULTS There were no major changes in strength for the infiltrated group, and homogeneity (m) was also increased. A layer of ZrSiO4 was formed on the surface. The bond strength to resin cement was improved after zirconia infiltration, acid conditioning and the use of an MDP primer. CONCLUSION The sol-gel method is an efficient and simple method to increase the homogeneity of zirconia. Infiltration also improved bonding to resin cement. CLINICAL SIGNIFICANCE The performance of a zirconia infiltrated by silica gel improved in at least two ways: structural homogeneity and bonding to resin cement. The infiltration is simple to perform and can be easily managed in a prosthesis laboratory.

Beta Ti-45Nb and Ti-50Nb Alloys Produced by Powder Metallurgy for Aerospace Application

Beta titanium alloys parts are used on advanced aerospace systems because of their high strength to weight ratio and excellent corrosion resistance. Production of powder metallurgy titanium alloys components may lead to a substantial reduction in the cost, compared to those produced by conventional cast and wrought processes, because additional working operations and material waste can be avoided. In this work, beta Ti-45Nb and Ti-50Nb were produced by the blended elemental technique, followed by uniaxial and cold isostatic pressing with subsequent densification by sintering. Sintered samples were characterized for phase composition by XRD, microstructure by SEM, hardness by Vickers indentation, specific mass by the Archimedes method and elastic modulus by resonance ultrasound. The sintered samples presented only the beta phase, higher hardness and lower elastic modulus when compared to Ti6Al4V alloy and experimental specific mass value near theoretical specific mass. These characteristics are adequate for application on several aerospace parts.

Development of (Nb,Ta)3Sn multifilamentary superconductor wire for high current applications

The optimization of the energy generated by a MagnetoHydroDynamic (MHD) channel using a superconducting magnet demands the optimization of the magnetic field of the system and of the critical points on the magnet winding. This work must include the development of a high performance superconductor wire suitable for this system. Aiming to the construction of improved performance MHD channel, it was developed a low cost superconductor wire, with the required characteristics. The wire was made using a technology compatible with the assembling steps and heat treatment conditions of the MHD superconducting magnets fabrication. It was used the internal Sn method in Nb-7.5wt%Ta tube to fabricate a 271-filament wire with a diameter of 0.81 mm and a Cu/nonCu ratio of 2.3. The wire was heat treated at 200 °C to diffuse the Sn into the Cu shell, producing bronze, followed by the final reaction at temperatures ranging from 670 °C to 730 °C during 25 to 150 h, to produce (Nb,Ta)3Sn. The superconducting wire characterization was made measuring the critical current Ic versus the applied magnetic field in the range of 5 to 20 T, the critical temperature Tc and the residual resistivity ratio (RRR). The wire transported critical currents above those available in commercial superconducting wires. These values of Ic are higher than the expected values for the optimization of the MHD channel.