Comparison of fracture surface and plane section analysis for ceramic grain size characterisation

A method has been developed to obtain quantitative information about grain size and shape from fractured surfaces of ceramic materials. One elaborated a routine to split intergranular and transgranular grains facets of ceramic fracture surfaces by digital image processing. A commercial ceramic (ALCOA A-16, Al2O3-1.5% of CrO) was used to test the proposed method. Microstructural measurements of grain shape and size taken from fracture surfaces have been compared through descriptive statistics of distributions, with the corresponding measurements from polished and etched surfaces. The agreement between results, with the expected bias on grain size values from fractures, obtained for both types of surfaces allowed to infer that this new technique can be used to extract the relevant microstructural information from fractured surfaces, thus minimising the time consuming steps of sample preparation. (C) 2003 Elsevier Ltd. All rights reserved.

Caracterização dos eletrocatalisadores LaMnO3, LaFeO3, LaFe0,2Mn0,8O3 E La0,5Fe0,5MnO3 preparados por autocombustão assistida por microondas para cátodos de células a combustível do tipo SOFC

Materials consisting of perovskite-type oxides (ABO3) have been developed in this work for applications in fuel cell cathodes of solid oxide type (SOFC). These ceramic materials are widely studied for this type of application because they have excellent electrical properties, conductivity and electrocatalytic. The oxides LaMnO3, LaFeO3, LaFe0.2Mn0.8O3 e La0.5Fe0.5MnO3 were synthesized by the method of microwave assisted combustion and after sintering at 800°C in order to obtain the desired phases. The powders were characterized by thermogravimetry (TG), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and voltammetric analysis (cyclic voltammetry and polarization curves). The results obtained by XRF technique showed that the microwave synthesis method was effective in obtaining doping oxides with values near stoichiometric. In general, powders were obtained with particle size less than 0.5 μm, having a porous structure and uniform particle size distribution. The particles showed spherical form, irregular and crowded of varying sizes, according to the analysis of SEM. The behavior of the oxides opposite the thermal stability was monitored by thermogravimetric curves (TG), which showed low weight loss values for all samples, especially those of manganese had its structure. By means of Xray diffraction of the samples sintered at 800°C was possible to observe the formation of powders having high levels of crystallinity. Furthermore, undesirable phases such as La2O3 and MnOx were not identified in the diffractograms. These phases block the transport of oxygen ions in the electrode/electrolyte interface, affecting the electrochemical activity of the system. The voltammetric analysis of the electrocatalysts LF-800, LM-800, LF2M8-800 e L5F5M-800 revealed that these materials are excellent electrical conductors, because it increased the passage of electrical current of the working electrode significantly. Best performance for the oxygen reduction reaction was observed with iron-rich structures, considering that the materials obtained have characteristics suitable for use in fuel cell cathodes of solid oxide type

Effect of Sodium Ascorbate and the Time Lapse before Cementation after Internal Bleaching on Bond Strength between Dentin and Ceramic

Purpose: To evaluate the effects of the elapsed time (ET) after nonvital bleaching (NVB) and sodium ascorbate application (10%) (SAA) on the shear bond strength of dentin to ceramic.Materials and Methods: Bovine incisors were selected, internally bleached (35% carbamide peroxide) for 9 days and submitted to the following treatments (n = 10): G1, G2, G3-luting after 1, 7, and 14 days; G4, G5, and G6-luting after SAA, 1, 7, and 14 days, respectively. G7 and G8 were not bleached: G7-luting 24 hours after access cavity sealing; G8-luting 24 hours after access cavity sealing after SAA. After NVB, the vestibular dentin was exposed and flattened. The SAA was applied to the dentin (G4, G5, G6, G8) for 10 minutes, and it was then washed and dried. The dentin was etched (37% phosphoric acid), and an adhesive system (Single Bond 2) was applied. Feldspathic ceramic discs (VM7; 4-mm diameter, 3-mm thick) were luted with a dual-resin agent (RelyX ARC, 3M ESPE Dental Products, St. Paul, MN). After 24 hours, specimens were submitted to shear test on a universal testing machine. The data (MPa) were submitted to ANOVA and Dunnet's test (5%).Results: The means (+/- SD) obtained were (MPa): G1 (14 +/- 4.5), G2 (14.6 +/- 3.1), G3 (14 +/- 3.7), G4 (15.5 +/- 4.6), G5 (19.87 +/- 4.5), G6 (16.5 +/- 3.7), G7 (22.8 +/- 6.2), and G8 (18.9 +/- 5.4). SAA had a significant effect on bond strength (p = 0.0054). The effect of ET was not significant (p = 0.1519). G5 and G6 presented higher values than the other bleached groups (p < 0.05) and similar to G7 and G8 (p > 0.05).Conclusions: After NVB, adhesive luting to dentin is recommended after 7 days if sodium ascorbate has been applied prior to dentin hybridization.

Does Adhesive Resin Application Contribute to Resin Bond Durability on Etched and Silanized Feldspathic Ceramic?

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Y-TZP ceramic processing from coprecipitated powders: A comparative study with three commercial dental ceramics

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

Demulsification of water/sunflower oil emulsions by a tangential filtration process using chemically impregnated ceramic tubes

A tangential filtration process was implemented in this study using porous ceramic tubes made of alpha-alumina produced by the slip-casting technique. These tubes were sintered at 1450 degrees C and characterized by mercury intrusion porosimetry, which revealed a mean pore size of 0.5 mu m. The tubes were chemically impregnated with a zirconium citrate solution, after which they were calcined and heat treated at temperatures of up to 600 and 900 degrees C to eliminate volatile organic compounds and transform the zirconium citrate into zirconium oxide impregnated in the alumina in the form of nanoparticle agglomerates. The microporous pipes were tested on a microfiltration hydraulic system to analyze their performance in the demulsification of sunflower oil and water mixtures. The fluid-dynamic parameters of Reynolds number and transmembrane pressure were varied in the process. The volume of permeate was analyzed by measuring the Total Organic Carbon concentration (TOC), which indicated 99% of oil phase retention. The emulsified mixture was characterized by optical microscopy, while the morphology and composition of the impregnated microporous tubes were analyzed by scanning electron microscopy (SEM). Quantification of the TOC values for the tube impregnated once at 600 degrees C showed the best demulsification performance, with the concentration on permeate smaller than 10 mg/L. The impregnated tube sintered once at 900 degrees C presented low carbon concentration (smaller than 20 mg/L), has the advantage of presenting the greatest trans-membrane flux in relation to the other microporous tube. (c) 2006 Elsevier B.V. All rights reserved.

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.