Preparation and characterization of glass-ceramic materials in the BaO-Li2O-ZrO2-SiO2 system and their dependence on treatment temperatures

The preparation and characterization of transparent glass-ceramics in the composition of 30Li2O:5ZrO2:xBaO:(100-x) SiO2 with x = 0, 5, 10, 15, and 20 mol% are described. Glasses were melted in a platinum crucible at 1100°C for 2 h and then heat-treated at 900°C for 3 h. The characterizations were performed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman and infrared spectroscopy, and scanning electron microscopy (SEM). The experimental results indicate that there was a structural change in the glass-ceramics as the BaO concentration in the mixture increased. In the XRD patterns of samples without heat treatment, only the halo was observed. After heat treatment, the appearance of the materials was verified by X-ray diffraction peaks. The reorganization of the amorphous solid was confirmed by Raman and IR spectroscopy along with XPS and SEM, with a more homogeneous phase formation being observed.

Sintering of tin oxide processed by slip casting

Sintering of SnO 2 compacts, obtained through slip casting, was studied by means of dilatometry, Hg porosimetry, scanning electron microscopy, and density measurement (Archimedes method). Sintering is strongly influenced by the green microstructure. Moreover, the sintering mechanisms are not dependent on the slurries' solid content up to 50% of solids in volume. Above this value, agglomerates are formed, leading to differential sintering inside and among the agglomerates. Another important point is the reduction of the temperature of maximum shrinkage rate when compared to tin oxide processed by isostatic pressing. This reduction is more accentuated when ammonium hydroxide is added to the suspension. (C) 2000 Published by Elsevier Science Ltd. All rights reserved.

Preparation and characterization of BaBi2Nb2O9(BBN) ceramics synthetized by polymeric precursors method

Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.

Fractal approach to ac impedance spectroscopy studies of ceramic materials

A novel fractal model for grain boundary regions of ceramic materials was developed. The model considers laterally inhomogeneous distribution of charge carriers in the vicinity of grain boundaries as the main cause of the non-Debye behaviour and distribution of relaxation times in ceramic materials. Considering the equivalent circuit the impedance of the grain boundary region was expressed. It was shown that the impedance of the grain boundary region has the form of the Davidson-Cole equation. The fractal dimension of the inhomogeneous distribution of charge carriers in the region close to the grain boundaries could be calculated based on the relation ds = 1 + β, where β is the constant from the Davidson-Cole equation.

Optimization of the mechanical properties of low-carbon steels by formation of a multiphase microstructure

In this work five methods of heat treatments are investigated in order to obtained convenient volume fractions of ferrite, bainite, martensite and retained austenite, starting with a low carbon steel and seeking the distinction of the phases, through optical microscopy. Specific chemical etching is improved. The results in tensile and fatigue tests were accomplished and the results were related with the microstructural parameters. The results show that the mechanical properties are closely related with the phases, grains size and the phases morphology. Copyright © 2001 Society of Automotive Engineers, Inc.

The use of pulsed electric acoustic technique for measuring the polarization reversal in ferroelectric ceramic samples

The pulsed electric acoustic technique, PEA, has been usually applied to probe space charge profiles in polymers. Preliminary PEA results using a ferroelectric ceramic are presented. If the reverse applied electric field i of the order of the coercive field the switching polarization process occurs in a period larger than hundreds of seconds. Such a slow process allows one to use the PEA setup to follow the polarization switching dynamics and determine the electric field profile. The PEA signal obtained in the lead zirconate-titanate doped with niobium ceramic, PZTN, indicates that the polarization distribution and field are not uniform during the switching period. We were also able to observe that the acoustic wave velocity and attenuation depends on the stage of the polarization switching, which agrees with results obtained using the ultrasonic method.

The use of pulsed electric acoustic technique for measuring electric field profiles in ferroelectric ceramic

The pulsed electric acoustic technique, PEA, have been usually applied to probe space charge profiles in polymers. In this work we show preliminary results obtained with lead zirconate-titanate and niobium, PZTN, ferroelectric ceramic samples. Experiments showed that induced charge densities on sample electrodes are mainly due to the ferroelectric polarization of the sample. We present results of the typical PEA response and the procedure to deconvolute the signal in order to obtain the charge densities and the electric field profiles. The PEA setup allows us to show a non-uniform polarization during ferroelectric switching.

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.

The influence of the sintering system on PMN properties

PMN powder samples with PbO excess of 0, 1,2 and 3% were submitted to the pressing and sintering at 1200°C for 4h with a heating rate of 3°C/min. A new sintering system, developed at our laboratories, was used. It allows obtaining more information on the sintering process. The sintered samples in the new system were compared to sintered samples in the C system. The microstructure, dielectric properties and the effect of the PbO excess in different sintering systems were compared. The N system permitted to obtain a ceramic with better properties, such density, dielectric constant and very homogeneous microstructure.

Sintering and mass transport features of (Sn,Ti)O2 polycrystalline ceramics

Different (Sn,Ti)O2 compositions were sintered at 1450 °C for 2 h with the purpose of investigating their sintering and mass transport properties. Highly dense ceramics were obtained and their structural properties studied by X-ray diffraction and scanning electron microscopy. The changes in lattice parameters were analyzed by the Rietveld method and two mass transport mechanisms were observed during sintering in different temperature ranges, evidenced by the linear shrinkage rate as a function of temperature. The effect of the concentration of TiO2 on mass transport and densiffication during sintering was analyzed by considering the intrinsic defects. System densiffication was attributed to a mass transport mechanism in the SnO2 matrix, caused by the presence of TiO2, which formed a solid solution phase. The change in the mass transport mechanism was attributed to chemical bonding between SnO2 and TiO2, which improves ionic difusion as the concentration of TiO2 increased in (Sn,Ti)O2 compositions. © 2002 Elsevier Science Ltd. All rights reserved.

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.

Temperature and stoichiometry effect on microstructural and ferroelectric properties of Pb(Zr1-xTix)O3 thin films prepared by chemical soulution deposition

Lead zirconate titanate (PZT) solutions were prepared using a polymeric precursor method, Zr n-propoxide and Ti i-propoxide were used as starting materials with ethylene glycol and water as solvents. The PZT solution was spin-coated on Pt/Ti/SiO2/Si substrates, baked on a hot plate, and finally heat-treated in a tube furnace between 400 and 800°C. The surface morphology and grain size of the films were characterized by atomic force microscopy (AFM), using a tapping mode with amplitude modulation. The films, thermal annealed at temperatures higher than 500°C, exhibited a dense microstructure, without noticeable cracks or voids. Electrical properties were investigated as a function of composition and annealing temperature.

Estudio de la adición de K+ y LiNbO3 en las propiedades finales del relaxor PMN procesado por mezcla de polvos

PMN ceramic relaxor has been investigated by several researchers and many aspects of this material, like powder morphology, phase decomposition, weight loss during sintering process, densification, between others, still are investigated. PMN powder preparation has been shown more efficient when synthesized by columbite route, however lead addition stage for the PMN powder synthesis remains problematical. Therefore, this work proposes a new association of methodologies, using columbite route and the hydroxide precipitation method. Through use of the powder mixture technique, which permitted to obtain good green and sintered densities, was possible to observe K+ y Li + dopants reduce weight loss in sintering process and change significantly the dielectric properties. Addition of LiNbO3 seeds in conformation stage, which react in a distinct way as a function of the particle size, promotes the formation of differenced grains in the ceramic bulk. Consequently, very different dielectrics properties from conventional PMN ceramic were obtained.

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.