Effect of aging on the stability of ceramic foams prepared by thermostimulated sol-gel process

This work presents a new route of preparation of zirconium ceramic foams based on the thermostimulated sol-gel process. This method produces gelled bodies with up to 90% of porosity in the wet gel and can be used to make complex-shaped components. Unfortunately, the shrinkage during the drying step allows to a catastrophic reduction (50%) of the foam porosity. To improve the foam stability we carried out a systematic study of the effect of gel foam aging on the drying process. Samples were aged in closed vessel at 25 C during different time period (from 6 to 240 h). The shrinkage and the mass loss during drying at 50 C were measured in situ, using a non-contact technique performed with a special apparatus. The results show that the total linear shrinkage decreases from 46% to 8% as the aging period increase from 6 to 240 h. This behavior is followed by a small change of total mass loss, from 42 to 54%. It indicates that by aging the structural stiffness of the foams increases due to secondary condensation reactions. Thus, by controlling the aging period, the porosity can be increased from 67 to 75% and the average size of mesopores of dried foams can be screened from 0.3 to 0.9 mum. Finally, these results demonstrate that the thermostimulated sol-gel transition provides a potential route to ceramic foams manufacture.

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.

Vertical marginal discrepancy of ceramic copings with different ceramic materials finish lines and luting agents: An in vitro evaluation

Statement of problem. Prosthetic restorations that fit poorly may affect periodontal health and occlusion. Studies that have evaluated the accuracy of fit of ceramic restorations before and after cementation assessed primarily intracoronal restorations.Purpose. This in vitro study evaluated the effect of different finish lines, ceramic manufacturing techniques, and luting agents on the vertical discrepancy of ceramic copings.Material and methods. Two stainless steel molars were prepared for complete crowns with 2 different finish lines (heavy chamfer and rounded shoulder); each molar was duplicated to fabricate 90 copings. A total of 180 copings generated 18 groups (n=10 for each finish line-coping material-luting agent combination). Luting agents tested included zinc phosphate, resin-modified glass ionomer (Fuji Plus), and resin composite cements (Panavia F). A metal frame was developed on which to screw the stainless steel model and a ceramic coping; the distance (mum) between 2 predetermined points was measured before and after cementation by a profile projector under a torquing force. A 4-way ANOVA with repeated measurements was performed to assess the influence of each factor in the vertical marginal discrepancy: 3 between-coping factors (finish line-coping material-luting agent) and 1 within-coping factor (before and after cementation) (alpha=.05).Results. Procera copings presented the lowest mean values (P<.05) of vertical marginal discrepancy before and after cementation (25/44 mum) when compared to Empress 2 (68/110 mum) and InCeram Alumina copings (57/117 mum), regardless of any combinations among all finish lines and luting agents tested.Conclusion. Considering each factor separately, the ceramic manufacturing technique appeared to be the most important factor tested for the definitive vertical discrepancy of all-ceramic copings, with lower mean values for Procera copings.

Can the chemical composition of the whole body of a goat be estimated from parts of its body?

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

Influence of ceramic surface conditioning and resin cements on microtensile bond strength to a glass ceramic

Statement of problem. It is not clear how different glass ceramic surface pretreatments influence the bonding capacity of various luting agents to these surfaces.Purpose. The purpose of this study was to evaluate the microtensile bond strength (mu TBS) of 3 resin cements to a lithia disilicate-based ceramic submitted to 2 surface conditioning treatments.Material and methods. Eighteen 5 X 6 X 8-mm ceramic (IPS Empress 2) blocks were fabricated according to manufacturer's instructions and duplicated in composite resin (Tetric Ceram). Ceramic blocks were polished and divided into 2 groups (n=9/treatment): no conditioning (no-conditioning/control), or 5% hydrofluoric acid etching for 20 seconds and silanization for 1 minute (HF + SIL). Ceramic blocks were cemented to the composite resin blocks with I self-adhesive universal resin cement (RelyX Unicem) or 1 of 2 resin-based luting agents (Multilink or Panavia F), according to the manufacturer's instructions. The composite resin-ceramic blocks were stored in humidity at 37 degrees C for 7 days and serially sectioned to produce 25 beam specimens per group with a 1.0-mm(2) cross-sectional area. Specimens were thermal cycled (5000 cycles, 5 degrees C-55 degrees C) and tested in tension at 1 mm/min. Microtensile bond strength data (MPa) were analyzed by 2-way analysis of variance and Tukey multiple comparisons tests (alpha=.05). Fractured specimens were examined with a stereomicroscope (X40) and classified as adhesive, mixed, or cohesive.Results. The surface conditioning factor was significant (HF+SIL > no-conditioning) (P<.0001). Considering the unconditioned groups, the mu TBS of RelyX Unicem was significantly higher (9.6 +/- 1.9) than that of Multilink (6.2 +/- 1.2) and Panavia F (7.4 +/- 1.9). Previous etching and silanization yielded statistically higher mu TBS values for RelyX Unicem (18.8 +/- 3.5) and Multilink (17.4 +/- 3.0) when compared to Panavia F (15.7 +/- 3.8). Spontaneous debonding after thermal cycling was detected when luting agents were applied to untreated ceramic surfaces.Conclusion. Etching and silanization treatments appear to be crucial for resin bonding to a lithia disilicate-based ceramic, regardless of the resin cement used.

The effect of ceramic surface treatment on bonding to densely sintered alumina ceramic

Statement of problem. Ceramic surface treatment is crucial for bonding to resin. High crystalline ceramics are poorly conditioned using traditional procedures.Purpose. The purpose of this study was to evaluate the effect of silica coating on a densely sintered alumina ceramic relative to its bond strength to composite, using a resin luting agent.Material and methods. Blocks (6 X 6 X 5 mm) of ceramic and composite were made. The ceramic (Procera AllCeram) surfaces were polished, and the blocks were divided into 3 groups (n = 5): SB, airborne-particle abrasion with 110-mu m Al(2)O(3); RS, silica coating using Rocatec System; and CS, silica coating using CoJet System. The treated ceramic blocks were luted to the composite (W3D Master) blocks using a resin luting agent (Panavia F). Specimens were stored in distilled water at 37 degrees C for 7 days and then Cut in 2 axes, x and y, to obtain specimens with a bonding area of approximately 0.6 mm(2) (n = 30). The specimens were loaded to failure in tension in a universal testing machine, and data were statistically analyzed using a randomized complete block design analysis of variance and Tukey's test (alpha=.05). Fractured surfaces were examined using light microscopy and scanning electron microscopy to determine the type of failure. Energy-dispersive spectroscopy was used for surface compositional analysis.Results. Mean bond strength values (MPa) of Groups RS (17.1 +/- 3.9) (P = .00015) and CS (18.5 +/- 4.7) (P=.00012) were significantly higher than the values of Group SB (12.7 +/- 2.6). There was no statistical difference between Groups RS and CS. All failures occurred at the adhesive zone.Conclusion. Tribochemical silica coating systems increased the tensile bond strength values between Panavia F and Procera AllCeram ceramic.

Preparation of ceramic membranes from surface modified tin oxide nanoparticles

The preparation of crack-free SnO2 supported membranes requires the development of new strategies of synthesis capable to allow controlled changes of surface chemistry and to improve the processability of supported layers. In this way, the controlled modification of the SnO2 nanoparticle surface by adding capping molecules like Tiron(R) ((OH)(2)C6H2(SO3Na)(2)) during the sol-gel process was studied, aiming to obtain high performance membranes. Colloidal suspensions were prepared by hydrolyzing SnCl4.5H(2)O aqueous solution with NH4OH in presence of Tiron(R). The effect of the amount of Tiro(R) (from I to 20 wt.%) on the structural features of nanoparticles, powder redispersability and particle-solution interface properties was investigated by X-ray powder diffraction (XRPD), extended X-ray absorption fine structure (EXAFS), quasi-elastic light scattering and electrophoretic mobility measurements. XRPD and EXAFS results showed that the addition of Tiron(R) up to 20 wt.% to colloidal suspensions does not affect the crystallite size of SnO2 primary particles, determined around 2-3 nm. This value is comparable to the hydrodynamic size measured after redispersion of powder prepared with amount of Tiro(R) higher than 7.5 wt.%, indicating the absence of condensation reactions between primary particles after the initial precipitation step. As a consequence the powder with amount of Tiron(R) > 7.5 wt.%, can be fully redispersed in aqueous solution at pH greater than or equal to I I until a nanoparticle concentration of 6 vol.%. The electrophoresis measurements showed a decrease of the isoelectric point by increasing the amount of grafted Tiron(R) at the SnO2 nanoparticle surface, resulting in negatively charged particle-solution interface in all the studied pH range (2-11). These features govern the gelation process favoring the preparation of crack-free SnO2 supported membranes. The control exercised by Tiron(R) modifying agent in the aggregation process allows the fine-tuning of the porosity, from 0.124 to 0.065 cm(3) g(-1), and mean pore size, from 6.4 to 1.9 nm, as the amount of grafted molecules increases from 0 to 10 wt.%. In consequence, the membrane cut-off determined by filtration of polyethylene glycol standard solutions can be screened from 1500 to 3500 g mol(-1). (C) 2002 Elsevier B.V. B.V. All rights reserved.

Comparison of subcutaneous connective tissue responses among three different formulations of gutta-percha used in thermatic techniques.

A study of the subcutaneous connective tissue response of 24 white rats to three different formulations of gutta-percha was undertaken. The prepared specimens were examined under the light microscope after intervals of 7, 21, 60 and 120 days. The results showed identical tissue responses after the initial period of 7 days. However, after 120 days the gutta-percha supplied with the Ultrafil system presented mature granulation tissue with neither oedema nor vascular congestion, in contrast to the responses observed with the McSpadden and Obtura formulations.

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.