Characterization of ceramic powders used in the inCeram systems to fixed dental Prosthesis

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

Mechanochemical synthesis of ceramic powders with perovskite structure

The mechanical activation is one of the most effective method for obtaining highly disperse system due to mechanical action stress fields form in solids during milling procedure. This effect results in changes of free energy, leading to release of heat, formation of a new surface, formation of different crystal lattice defects and initiation of solid-state chemical reaction. The accumulated deformation energy determines irreversible changes of crystal structure and consequently microstructure resulting in the change of their properties. Mechanochemical processing route has been developed recently for the production of intermetallic and alloy compounds. The intrinsic advantage of this process is that the solid-state reaction is activated due to mechanical energy instead of the temperature. It was shown that the chemical reactivity of starting materials could be improved significantly after mechanochemical activation and, subsequently, the calcination temperature was reduced. Besides, it was apparent that the mechanochemical treatment could enhance the reactivity of constituent oxides; however, the sintering process could not be avoided to develop the desired ceramics. A novel mechanochemical technique for synthesis of fine-grained perovskite structured powders has shown that it is possible to form perovskite at room temperature. The effect of milling on the formation of perovskite structure of barium titanate (BT), lead titanate (PT), PZT, PZN, magnesium niobate (PMN) and LM ceramic materials was analyzed. The dielectric properties of sintered ceramics are comparable with those prepared by other methods in the literature. (C) 2003 Elsevier B.V. B.V. All rights reserved.

Pore size evolution during sintering of ceramic oxides

This paper reviews the influence of particle size distribution, agglomerates, rearrangement, sintering atmospheres and impurities on the pore evolution of some commonly studied oxides. These factors largely affect sintering mechanisms due to modifications of diffusion coefficients or evaporation-condensation. Very broad particle size distribution leads to grain growth and agglomerates densify first. Rearrangement of particles due to neck asymmetry mainly in the early stage of sintering is responsible for a high rate of densification in the first minutes of sintering by collapse of large pores. Sintering atmospheres play an important role in both densification and pore evolution. The chemical interaction of water molecules with several oxides like MgO, ZnO and SnO2 largely affects surface diffusion. As a consequence, there is an increase in the rates of pore growth and densification for MgO and ZnO and in the rate of pore growth for SnO2. Carbon dioxide does not affect the rate of sintering of MgO but greatly affects both rates of pore growth and densification of ZnO. Oxygen concentration in the atmosphere can especially affect semiconductor oxides but significantly affects the rate of pore growth of SnO2. Impurities like chlorine ions increase the rate of pore growth in MgO due to evaporation of HCl and Mg(OH)Cl, increasing the rate of densification and particle cuboidization. CuO promotes densification in SnO2, and is more effective in dry air. The rate of densification decrease and pore widening are promoted in argon. An inert atmosphere favors SnO2 evaporation due to reduction of CuO. © 1990.

MnO2 influence on the electrical properties of SnO2-based ceramic systems

Tin dioxide is an n-type semiconductor that when doped with other metallic oxides exhibits non-linear electric behavior with high non-linear coefficient values typical of a varistor. In this work, electrical properties of the SnO2.CoO.Ta2O5 and SnO2.CoO.MnO2.Ta2O5 ceramics systems were studied with the objective of analyzing the influence of MnO2 on sintering behavior and electrical properties of these systems. The compacts were prepared by powder mixture process and sintered at 1300°C for 1 hour, in air, using a constant heating rate of 10°C/min. The morphological and structural properties were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The densities of the sintered ceramics were measured using the Archimedes method. The SnO2.CoO.Ta2O5 and SnO2.CoO.MnO2.Ta2O5 systems presented breakdown fields (Eb) about 3100 V.cm-1 and 3800 V.cm-1, respectively, and non-linear coefficient (α) about 10 and 20, respectively.

A method for the digital image analysis of ceramic grains based on shape factor segmentation

A very simple and robust method for ceramics grains quantitative image analysis is presented. Based on the use of optimal imaging conditions for reflective light microscopy of bulk samples, a digital image processing routine was developed for shading correction, noise suppressing and contours enhancement. Image analysis was done for grains selected according to their concavities, evaluated by perimeter ratio shape factor, to avoid consider the effects of breakouts and ghost boundaries due to ceramographic preparation limitations. As an example, the method was applied for two ceramics, to compare grain size and morphology distributions. In this case, most of artefacts introduced by ceramographic preparation could be discarded due to the use of perimeter ratio exclusion range.

Ceramic Crucible Corrosion by Heavy Metal Oxide Glasses, Part I: Phenomenological Study

Heavy metal oxide (HMO) glasses have received special attention due to their optical, electrical and magnetic properties. The problem with these glasses is their corrosive nature. In this work, three ceramic crucibles (Al 2O 3, SnO 2 and ZrO 2) were tested in the melting of the system 40 PbO-35 BiO 1.5-25 GaO 1.5 (cation-%). After glass melting, crucibles were transversally cut and analyzed by scanning electronic microscopy (SEM), coupled to microanalysis by energy dispersive spectroscopy (EDS). Results indicated that zirconia crucibles presented the highest corrosion, probably due to its smallest grain size. Tin oxide crucibles presented a low corrosion with small penetration of the glass into the crucible. This way, these crucibles are an interesting alternative to melt corrosive glasses in instead of gold or platinum crucibles. It is important to emphasize the lower cost of tin oxide crucibles, compared to gold or platinum ones.

Ceramic Crucible Corrosion by Heavy Metal Oxide Glasses, Part II: Diffusion Study

Due to their low cost and high resistance to corrosion, ceramic crucibles can be used for the melting of PBG glasses (PbO-BiO 1.5GaO 1.5). These glasses present good window transmission from ultra-violet to infrared, making their use as optical fibres promising. However, their disadvantage is the high reactivity, leading to the corrosion of different crucibles, including gold and platinum ones. In this work, the corrosion of Al 2O 3, SnO 2 and ZrO 2 crucibles after melting at temperatures varying from 850 to 1000°C, was evaluated by Scanning Electronic Microscopy (SEM) in conjunction with microanalysis by EDS. The lead diffusion profile in the crucible material was obtained. Diffusion coefficients were calculated according to the Fick and Fisher theories. Results indicated that the different crucibles presented similar behaviour: in the region near the interface, diffusion occurs in the volumetric way and in regions away from the interface, diffusion occurs through grain boundary.

Effect of ceramic surface treatment on the microtensile bond strength between a resin cement and an alumina-based ceramic

Purpose: The objective of this study was to test the following hypothesis: the silica coating on ceramic surface increases the bond strength of resin cement to a ceramic. Materials and Methods: In-Ceram Alumina blocks were made and the ceramic surface was treated: G1 - sandblasting with 110-μm aluminum oxide particles; G2 - Rocatec System: tribochemicai silica coating (Rocatec-Pre powder + Rocatec-Plus powder + Rocatec-Sil); G3 - CoJet System: silica coating (CoJet-Sand) + ESPE-Sil. The ceramic blocks were cemented to composite blocks with Panavia F resin cement (under a load of 750 g/1 min). The cemented blocks were stored in distilled water at 37°C for 7 days and sectioned along the x and y axes with a diamond disk. Samples with an adhesive area of ca 0.8 mm 2 (n = 45) were obtained. The samples were attached to an adapted device for the microtensile test, which was performed in a universal testing machine (EMIC) at a crosshead speed of 1 mm/min. Results: The obtained results were submitted to ANOVA and Tukey's test. Mean values of tensile strength (MPa) and standard deviation values were: (G1) 16.8 ± 3.2; (G2) 30.6 ± 4.5; (G3) 33.0 ± 5.0. G2 and 63 presented greater tensile strength than G1. There was no significant difference between G2 and G3. All the failures took place at the ceramic/resin cement interface. Conclusion: The silica coating (Rocatec or CoJet systems) of the ceramic surface increased the bond strength between the Panavia F resin cement and alumina-based ceramic.

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.

Structural and dielectric properties of relaxor Sr0.5Ba 0.5Bi2Nb2O9 ceramic

Sr0.5Ba0.5Bi2Nb2O 9 ceramic was prepared by a conventional solid state reaction method and studied using X-ray powder diffraction and dielectric measurements. At room temperature, an orthorhombic structure was confirmed and their parameters were obtained using the Rietveld method. Dielectric properties were studied in a broad range of temperatures and frequencies. Typical relaxor behaviour was observed with strong dispersion of the complex relative dielectric permittivity. The temperature of the maximum dielectric constant Tm decreases with increasing frequency, and shifts towards higher temperature side. The activation energy Ea≈0·194±0·03 eV and freezing temperature Ta≈371±2 K values were found using the Vogel-Fulcher relationship. Conduction process in the material may be due to the hopping of charge carriers at low temperatures and small polarons and/or singly ionised oxygen vacancies at higher temperatures. © 2010 Maney Publishing.

Development of ceramic cutting tools for future application on dry machining

Advanced ceramic materials constitute a mature technology with a very broad base of current and potential applications and a growing list of material compositions. Within the advanced ceramics category, silicon nitride based ceramics are wear-resistant, corrosion-resistant and lightweight materials, and are superior to many materials with regard to stability in high-temperature environments. Because of this combination the silicon nitride ceramics have an especially high potential to resolve a wide number of machining problems in the industries. Presently the Si3N4 ceramic cutting tool inserts are developed using additives powders that are pressed and sintered in the form of a cutting tool insert at a temperature of 1850 °C using pressureless sintering. The microstructure of the material was observed and analyzed using XRD, SEM, and the mechanical response of this array microstructure was characterized for hardness Vickers and fracture toughness. The results show that Si3N4/20 wt.% (AlN and Y 2O3) gives the best balance between hardness Vickers and fracture toughness. The Si3N4/15 wt.% (AlN and Y 2O3) composition allows the production of a very fine-grained microstructure with low decreasing of the fracture toughness and increased hardness Vickers. These ceramic cutting tools present adequate characteristics for future application on dry machining. © (2010) Trans Tech Publications.

Glass-ceramic material from the SiO 2-Al 2O 3-CaO system using sugar-cane bagasse ash (SCBA)

Brazil is the world's largest producer of alcohol and sugar from sugarcane. Currently, sugarcane bagasse is burned in boilers to produce steam and electrical energy, producing a huge volume of ash. The major component of the ash is SiO 2, and among the minor components there are some mineralizing agents or fluxing. Published works have shown the potential of transforming silicate-based residues into glass-ceramic products of great utility. This work reports the research results of SCBA use to produce glass-ceramics with wollastonite, rankinite and gehlenite as the major phases. These silicates have important applications as building industry materials, principally wollastonite, due to their special properties: high resistance to weathering, zero water absorption, and hardness among others. The glasses (frits) were prepared mixing ash, calcium carbonate and sodium or potassium carbonates as flux agents, in different concentrations. X-ray fluorescence was used to determine the chemical composition of the glasses and their crystallization was assessed by using thermal analysis (DTA/DSC/TGA) and X-ray diffraction. The crystallization kinetics was evaluated using the Kissinger method, giving activation energies ranging from 200 to 600 kJ/mol. © 2011 Ceramic Society of Japan.

Effect of green machining on distortion and surface finishing in advanced ceramic

An alternative for grinding of sintered ceramic is the machining on the green state of the ceramic, which presents easy cutting without the introduction of harmful defects to its mechanical resistance. However, after sintering there are invariably distortions caused by the heterogeneous distribution of density gradients, which are located in the most outlying portions of the compacted workpiece. In order to minimize these density gradients, this study examined the influence of different allowance values and their corresponding influence in distortion after sintering alumina specimens with 99.8 % purity by turning operation using cemented carbide tool. Besides distortion, other output variables were analyzed, such as tool wear, cutting force and surface roughness of green and sintered ceramics. Results showed a distortion reduction up to 81.4%. Green machining is beneficial for reducing surface roughness in both green and sintered states. Cutting tool wear has a direct influence on surface roughness and cutting force.

Effect of ceramic shade on the degree of conversion of a dual-cure resin cement analyzed by FTIR

Objectives: The aim of this research was to evaluate the degree of monomer conversion of different resin cement shades when photocured under different feldspathic ceramic shades. The photocuring time was also evaluated as well as the translucency of each ceramic shade. Methods: Three VITA VM7 ceramic shades (Base Dentin 0M1, Base Dentin 2M2 and Base Dentin 5M3) were used to determine the translucency percentage. A spectrophotometer MiniScan was used to measure the opacity percentage of each specimen (2-mm-thick) and then the translucency was calculated. To measure the degree of conversion (DC), the resin cement (Variolink II; A3 Yellow and transparent) specimens (thickness: 100 μm) were photocured under a ceramic block (2-mm-thick) for 20 or 40 s. Specimens photocured without the ceramic block were used as control. Sixteen groups (n = 3) were evaluated. Micro-ATR/FTIR spectrometry was used to evaluate the extent of polymerization of all specimens after 24 h. The %DC was calculated of experimentally polymerized versus maximally polymerized composite. Results: The translucency percentages of 0M1, 2M2 and 5M3 ceramics were 12.41 (1.02)%, 5.75 (1.91)% and 1.07 (0.03)%, respectively. The %DC of both resin cement shades cured under ceramic 5M3 was significantly lower than the other groups (p < 0.05). The %DC of 0M1 groups exhibited no significant difference from 2M2 groups (p > 0.05), with the exception of the transparent cement photocured for 40 s. Conclusion: Photocuring under 2 mm ceramic showed that the increase in chroma saturation significantly decreased Variolink II resin cement %DC (100-μm-thick). © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of convergence angle of tooth preparation on the fracture resistance of Y-TZP-based all-ceramic restorations

Objective: To investigate the influence of the convergence angle of tooth preparation on the fracture load of Y-TZP-based ceramic (YZ-Vita YZ) substructure (SB) veneered with a feldspathic porcelain (VM9-Vita VM9). Methods: Finite element stress analysis (FEA) was performed to examine the stress distribution of the system. Eighty YZ SB were fabricated using a CAD-CAM system and divided into four groups (n = 20), according to the total occlusal convergence (TOC) angle: G6-6° TOC; G12-12° TOC; G20-20° TOC; and G20MOD-20° TOC with modified SB. All SB were veneered with VM9, cemented in a fiber reinforced epoxy resin die, and loaded to failure. Half of the specimens from each group (n = 10) were cyclic fatigued (106 cycles) before testing. Failure analysis was performed to determine the fracture origin. Data were statistically analyzed using Anova and Tukey's tests (α = 0.05). Results: The greatest mean load to fracture value was found for the G20MOD, which was predicted by the FEA. Cyclic fatigue did not significantly affect the load of fracture. Catastrophic failure originating from the internal occlusal surface of the SB was the predominant failure mode, except for G20MOD. Significance: The YZ-VM9 restorations resisted greater compression load than the usual physiological occlusal load, regardless of the TOC angle of preparations. Yet, the G20MOD design produced the best performance among the experimental conditions evaluated. © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.