Tiago Moreira Bastos Campos

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.

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.

Characterization of SiC thin films deposited by HiPIMS

In this work thin films of silicon carbide (SiC) were deposited on silicon wafers by High Power Impulse Magnetron Sputtering (HiPIMS) technique varying the average power of the discharge on a stoichiometric SiC target. X-ray diffraction, Raman spectroscopy, scanning electron microscopy and profilometry were used to analyze the films. It was observed that high values of the average electric power favors the formation of C-C bonds, while low values of the power promote the formation of Si-C bonds. At high power, we have also observed higher deposition rates, but the samples present surface imperfections, causing increase in the roughness and decrease in the film uniformity.

Impact of crystallization firing process on the microstructure and flexural strength of zirconia-reinforced lithium silicate glass-ceramics

OBJECTIVES The aim of this study was to characterize the microstructure of two zirconia-reinforced lithium silicate (ZLS) glass-ceramics and evaluate their mechanical properties before and after the crystallization firing process (CFP). METHODS Field emission-scanning electron microscope (FE-SEM) and energy-dispersive X-ray spectroscopy (EDS) analyses were performed for microstructural characterization. To evaluate the pattern of crystallization and the molecular composition of ZLS glass-ceramics, was used X-ray diffraction (XRD). Vickers hardness, fracture toughness by the indentation method, and biaxial flexural strength were also measured. One hundred and forty ceramic discs were produced (diameter=12mm; thickness=1.2mm) and allocated among four groups (n=30): Sfir, Sunf-ZLS Vita Suprinity; and Cfir and Cunf-ZLS Celtra Duo; fired and unfired, respectively. Statistical analysis was performed and Weibull failure probabilities were calculated. RESULTS Cfir showed the highest characteristic strength (251.25MPa) and hardness (693.333±10.85GPa). Conversely, Sunf presented the lowest characteristic strength (106.95MPa) and significantly lowest hardness (597.533±33.97GPa). According to Weibull analysis, Sunf had the highest structural reliability (m=7.07), while Sfir presented the lowest (m=5.38). The CFP was necessary to crystallize zirconia in the partially crystallized ZLS glass-ceramics. Sfir had a lower percentage of crystallized zirconia than did Cfir. Fractographic analyses showed that all failures initiated from an inherent critical defect in Sunf and from processing defects in the remaining groups. SIGNIFICANCE The CFP had a direct influence on the flexural strength and microstructural characteristics of both ZLS materials.

Bioinspired silica-infiltrated zirconia bilayers: Strength and interfacial bonding

Conventionally veneered zirconia restorations are susceptible to chipping and spalling of the veneering material. The novel translucent zirconias were developed to overcome such issues, although layered zirconia restorations can be re-designed to improve mechanical performance. Thus, the aim of this study was to analyze the strength and structural reliability of zirconia bilayers using conventional (porcelain ceramic under tensile stress) and bioinspired (zirconia under tensile stress) configurations. Sol-gel silica infiltration served as a smooth transition between the zirconia and veneering porcelain. Failure mode and interfacial adhesive mechanism were analyzed using scratch test and interfacial indentation. Bilayered specimens were produced for biaxial flexural testing with Y-TZP and pressed ceramic, which were further divided into four groups (n = 30): Conventional (C), Infiltrated conventional (IC), Bioinspired (B) and Infiltrated bioinspired (IB). The results of biaxial flexural strength tests were analyzed by Weibull analysis (95% CI) for determination of the Weibull modulus (m). The infiltration layer was characterized by XRD and SEM, FEG-SEM and EDS. The bioinspired infiltrated group was the most reliable (m = 9.59), although the fine damage of veneered conventional (conventional) zirconia demonstrated its superior resistance to scratching and debonding. Therefore, the filling of superficial defects by zirconia silicate demonstrated the need for mechanical retention for better porcelain adhesion.

The performance of sol-gel silica coated Y-TZP for veneered and monolithic dental restorations

OBJECTIVES The purpose of the study was to characterize the microstructure, constituents, and mechanical properties of mono and bilayered zirconia specimens infiltrated with silica by the sol gel method. METHODS 180 zirconia discs (14-mm diameter) were divided in 3 groups (n = 60) according to thickness (1.2, 0.5 mm) and further divided in two groups (n = 30) according to treatment (infiltrated or not). Disk thickness was 1.2 mm for the control samples. Veneering feldspathic porcelain had two thicknesses (0.5 mm and 1 mm) at the tops of the zirconia discs. All groups were subjected to the biaxial flexural test in an aqueous medium. Weibull analysis was performed for determination of the Weibull modulus (m) and characteristic strength (σ0). The specimens were characterized by SEM and EDS and XRD. Hardness and elastic modulus were measured by nano-indentation and pulse-echo methods, respectively. Fracture toughness was determined by the nano-indentation technique. A scratch test was used for evaluation of the adhesion between the zirconia and porcelain. RESULTS There was less variability (higher Weibull modulus) in the infiltrated monolithic specimens; biaxial flexural strength was not statistically higher in the veneered infiltrated specimens and was decreased for the 1-mm veneered infiltrated group. The diffractograms showed formation of ZrSiO4 crystal phase. Hardness also increased in the infiltrated monolithic zirconia, whereas fracture toughness decreased. Adhesion between zirconia and porcelain was superior in the non-infiltrated monolithic specimens. CONCLUSIONS Infiltration increased the structural homogeneity and hardness of the monolithic zirconia, but it reduced fracture toughness, and the adhesion to porcelain. CLINICAL SIGNIFICANCE Within the limitations of the present study, it is possible to recommend the infiltration of silica gel in zirconia only for monolithic restorations.

Novel synthetic route for low-cost carbon-modified TiO2 with enhanced visible light photocatalytic activity: carbon content and calcination effects

AbstractThe aim of this study was the development of low-cost tannin-formaldehyde xerogel/TiO2 (XTi-w) and carbon xerogel/TiO2 (XTiC-w) photocatalysts. The materials used as precursors were recycled titanium scraps and black wattle tannin extract, highlighting the low-cost approach employed in the synthesis. The materials were characterized by diffuse reflectance spectroscopy, scanning electron microscopy, dispersive energy spectrophotometry, X-ray diffractometry, infrared and Raman spectroscopy. X-ray diffractometry showed that the XTiC-w have tetragonal crystalline structure (anatase), whereas the XTi-w has an amorphous structure. The Raman and infrared analysis also showed the presence of titanium dioxide in the composition of both XTi-w and XTiC-w. XTi-w and XTiC-w showed photocatalytic activity at the visible wavelength. Titanium dioxide displayed no photocatalytic activity at the visible wavelength. The XTi-60 composite displayed the highest efficiency in the removal of the methylene blue from the system, as well as good reusability properties. The radicals with higher influence in the photocatalytic reaction mechanism are the photo generated electron and the singlet oxygen molecule. The effect of the heat treatment is negative on the photocatalytic properties of the hybrids produced, due to the removal of acid sites, adsorbed water and OH surface groups. The graphical abstract displays an illustration of the materials obtained in this work and their respective efficiency in the adsorption and photocatalytic degradation of methylene blue under visible light.HighlightsHybrids were produced using low-cost materials, such as titanium scraps and tanninBoth hybrid materials showed photocatalytic activity at the visible wavelengthHeat treatment is negative on the photocatalytic properties of the hybridsReaction mechanism is controlled by trapped electrons and singlet oxygen molecules

Aging Behavior of Commercial and Synthesized Dental Y-TZP Ceramics

Yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) is used for dental prosthodontics, however, it can present accelerated tetragonal to monoclinic phase transformation in oral environment. The aim of this study was to compare the behavior of a Y-TZP synthesized in laboratory by the coprecipitation method to a commercial Y-TZP, after hydrothermal aging in pressurized reactor (150°C/ 35 hours). The discs were sintered at 1520°C for two hours. The kinetics curve of phase transformation was determined through the data collect by XRD diffractograms treated by the Rietveld method. The experimental and commercial control groups did not present monoclinic phase. After 35 hours of aging, the experimental group presented 69% of monoclinic phase compared to 67% for the commercial group. Scanning electron microscopy and atomic force microscopy images suggested that the commercial group presented heterogeneity of grain size and that the experimental group was more homogeneous. All groups presented superficial degradation process.