Densification and coarsening of SnO2-based materials containing manganese oxide

The present work presents results on natural sintering of tin dioxide ceramics, prepared by a chemical route or by conventional mixing and containing manganese (X-Mn = Mn/(Mn + Sn)(atomic) with 0 less than or equal to X(Mn)less than or equal to 0.15). This cation, which is practically insoluble in SnO2 network, stays at the grain surface. During thermal treatment (500 degrees C less than or equal to T-s less than or equal to 1400 degrees C), as long as the manganese surface concentration is lower than a critical value, equal to 5.10(-6) mol m(-2), no densification takes place. As soon as this value is reached, densification and grain growth occur simultaneously. The shrinkage kinetics is fast and high rho/rho(t) values can be obtained (for example. rho/rho(t)=0.95 for T-s=1300 degrees C and X-Mn=0.004). The dependence between manganese content, manganese distribution, grain size and sintering behaviour is also discussed. (C) 1998 Published by Elsevier B.V. Limited.

Preparation of SnO2 supported membranes with ultrafine pores

The colloidal route of the sol-gel process was used to prepare supported SnO2 membranes. The influence of the sol and monoelectrolyte concentrations on the formation of the gel layer by sol-casting on the top of macroporous alpha-Al2O3 support was described. The stability of the colloidal suspension as a function of the concentrations was analyzed from creep-recovery measurements. The calcined supported membranes were characterized by nitrogen adsorption-desorption isotherms and scanning electron microscopy. The set of results show that homogeneous membrane layers containing the smallest quantity of cracks are formed in a critical interval of sol (1.01 less than or equal to[SnO2]less than or equal to 1.4 M) and electrolyte (2.O less than or equal to[Cl-]less than or equal to 4.0 mM) concentrations. The samples prepared from concentrated suspensions present a lot of interconnected cracks which favors the peeling of the coated layer. The membranes have pores of average diameter of about 1 nm.

Sintering of ultrafine undoped SnO2 powder

The sintering process of nanometric undoped SnO2 powder was studied. No macroscopic shrinkage was observed during the sintening process. Grain growth kinetics investigation showed that surface diffusion is the dominant mechanism in the temperature range 500-1300 degreesC. For temperatures higher than 1300 degreesC, high weight loss was measured, suggesting evaporation-condensation as the dominant mass-transport mechanism. Thermogravimetric analysis (TG) and mass spectroscopy studies showed that the surface contamination of the SnO2 particles by chemical species like H2O, OH- and CO2, has a strong influence on the role of mass transport controlled by surface diffusion. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Planar waveguides based on nanocrystalline and Er3+ doped SnO2

Luminescent SnO2: x%mol Er3+ (x=0.1-2.0) thin films have been spin coated on borosilicate and silica substrates from water colloidal suspensions that could be prepared containing up to 40% in weight SnO2 nanocrystalline powders. High Resolution Transmission Electron Microscopy results show the well known SnO2 cassiterite structure and nanocrystallites around 10 nm in diameter, corroborating results from X-ray diffraction. Mono and multi layers have been prepared from the stable colloidal suspensions and films thickness was observed to increase linearly, up to 200 nm, with the colloidal suspensions nanoparticles amount. Excitation and emission spectra have been measured and Er3+ ions were found to be essentially incorporated into the cassiterite structure, substituting for Sn4+, for doping concentration lower than 0.05 mol%. Er3+ ions also appear segregated at the grains surface for higher doping concentration. The optical parameters (refractive index, thickness and propagating modes) of a waveguide sample were measured at 632.8 and 543.4 nm by the prism coupling technique. A monomodal waveguide was obtained with attenuation loss of 3.5 dB/cm along a 2.5 cm optical path.

Influence of fluoride-containing solutions on the translucency of flowable composite resins

The aim of this study was to evaluate the influence of fluoride-containing solutions on the translucency of flowable composite resins, with respect the immersion time. Flow-It! (FI) and Natural Flow (NF) composite resins and three commercial brands of fluoride-containing solutions (Fluordent, Fluorgard and Oral B) were used. Specimens were prepared and stored in the solutions at 37degreesC, until the measurements were made after the following treatments: T1 - after 1 hour in relative humidity; T2 - after 1 h in solution; T3 - 24 h; T4 - 48 h; T5 - after a week; from T9, the measurements were accomplished weekly, up to 30-day immersion. To obtain translucency values an electrophoresis equipment was employed. Data were submitted to ANOVA and Tukey tests. The results disclosed that NF showed highest values of translucency and was statistically different from FI (p < 0.001). As regards the solutions, Fluordent and Oral B presented similar values and were statistically superior to Fluorgard (p < 0.05). Concerning the immersion time, similar results were observed for the different evaluation periods. It may be concluded that the fluoride-containing solutions affected the translucency of the composite resins, independently of the materials used. Among the tested resins, NF presented the best performance. (C) 2003 Kluwer Academic Publishers.

Sintering mechanisms of ZrO2 center dot MgO with addition of TiO2 and CuO

Substitutions of Ti and Cu in ZrO2.MgO (Z), cause transformation from monoclinic (m) to cubic (c) and tetragonal (t). According to the vacancy model and solid Solution formation models, neither CuO nor TiO2 cause zirconia stabilization, which derives front other phenomena. Data analysis by TMA using the CRH (constant rate of heating) method shows a solid state reaction of ZrO2.MgO.TiO2 (Z.TiO2) demonstrating a dominant mechanism of volume diffusion (n = 1). However, the sintering of ZrO2.MgO.CuO (Z.CuO) shows a viscous flow mechanism (n = 0), a similar phenomena to that of by sintering of glass. Transformations, such as: CuO to Cu2O at 1000 degreesC, ZrO2 (m) to ZrO2 (t) at 1100 degreesC and Cu2O (s) to Cu2O (l) at 1230 degreesC cause successive rearrangements of microstructure inside of region I (sintering process) and lead to interpretation errors when the Bannister equation is used. (C) 2003 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Polymerization shrinkage: effects of boundary conditions and filling technique of resin composite restorations

Objective: To evaluate the linear polymerization shrinkage (LPS) and the effect of polymerization shrinkage of a resin composite and resin-dentin bond strength under different boundary conditions and filling techniques.Methods: Two cavities (4 x 4 x 2 MM) were prepared in bovine incisors (n = 30). The teeth were divided into three groups, according to boundary conditions: In group TE, the total-etch technique was used. In group EE, only enamel was conditioned, and in group NE, none of the watts of the cavities were conditioned. A two-step adhesive system was applied to all cavities. The resin composite was inserted in one (B) or three increments (1), and tight-cured with 600 mW/cm(2) (80 s). The LPS (%) was measured in the top-bottom direction, by placing a probe in contact with resin composite during curing. Enamel and total mean gap widths were measured (400 x) in three slices obtained after sectioning the restorations. Then, the slices were sectioned again, either to obtain sticks from the adhesive interface from the bottom of the cavity or to obtain resin composite sticks (0.8 mm(2)) to be tested for tensile strength (Kratos machine, 0.5 mm/min). The data was subjected to a two-way repeated measures ANOVA and Tukey's test for comparison of the means (alpha = 0.05).Results: the highest percentage of LPS was found for the TE when bulk fitted, and the lowest percentage of LPS was found in the Hand NE when incrementally fitted. The resin dentin bond strength was higher and the total mean gap width was tower for TE group; no significant effect was detected for the main factor fitting techniques. No difference was detected for the tensile strength of resin composite among the experimental groups.Conclusions: the filling technique is not able to minimize effects of the polymerization shrinkage, and bonding to the cavity watts is necessary to assure reduced mean gap width and high bond strength values. (C) 2004 Elsevier Ltd. All rights reserved.

Evaluation of color removal and degradation of a reactive textile azo dye on nanoporous TiO2 thin-film electrodes

The feasibility of the photobleaching of a textile azo dye, reactive orange 16 (C.I. 17757), in aqueous solution using titanium dioxide thin-film electrodes prepared by the sol-gel method was investigated. The best conditions for maximum photoelectrocatalytic degradation were found to be pH > 10 for Na2SO4 medium and pH < 6 for NaCl. In both situations, an applied potential of +1.0 V and low dye concentration are recommended, when 100% of color removal is obtained after 20 min of photoelectrocatalysis. The effects of side reaction pathway on the degradation rate of dye in sulfate and chloride medium were presented and the best performance are optimized to situations closed to that verified in the textile effluent. The influence of variables as applied potential, pH, supporting electrolyte and dye concentration on the kinetics of photoelectrochemical degradation also were investigated. Oxalic acid is identified by HPLC and UV-Vis spectrophotometric methods as the main degradation product generated after 180 min of photoelectrocatalysis of 4 x 10(-5) mol l(-1) dye in sodium sulphate pH 12 and NaCl pH 4.0 and a maximum reduction of 56 and 62% TOC was obtained, respectively. (C) 2004 Elsevier Ltd. All rights reserved.

Tibial segmental bone defect treated with bone plate and cage filled with either xenogeneic composite or autologous cortical bone graft

Tibia segmental defect healing in sheep were clinically, radiographically and histologically evaluated. Twelve young sheep aged four to five months were divided into two groups, G1 and G2. A 3.5 cm long segmental defect was created in the right tibial diaphysis with maintenance of the periosteum. The bone defects in both groups were stabilized with a bone plate combined with a titanium cage. In G1 the cage was filled with pieces of autologous cortical bone graft. In G2 it was filled with a composite biomaterial which consisted of inorganic bovine bone, demineralized bovine bone, a pool of bovine bone morphogenetic proteins bound to absorbable ultra-thin powdered hydroxyapatiteand bone-derived denaturized collagen. Except for one G1 animal, all of them showed normal limb function 60 days after surgery. Radiographic examination showed initial formation of periosteal callus in both groups at osteo-tomy sites, over the plate or cage 15 days postoperatively. At 60 and 90 days callus remodeling occurred. Histological and morphometric analysis at 90 days after surgery showed that the quantity of implanted materials in G1 and G2 were similar, and the quantity of new bone formation was less (p = 0.0048) and more immature in G1 than G2, occupying 51 +/- 3.46% and 62 +/- 6.26% of the cage space, respectively. These results suggest that the composite biomaterial tested was a good alternative to autologous cartical bone graft in this experimental ovine tibial defect. However, additional evaluation is warranted prior to its clinical usage.

Electron scattering and effects of sources of light on photoconductivity of SnO2 coatings prepared by sol-gel

Electro-optical properties of sol-gel derived 2 mol% antimony or niobium doped tin dioxide films have been measured. The electron density has been calculated considering all the relevant scattering mechanisms and experimental conductivity data measured in the range -197 to 25 degrees C. The results support the hypothesis that both ionised impurity scattering and grain boundary scattering have comparable effects in the resistivity of coatings, for free electron density congruent to 5 x 10(18) cm(-3). We have measured variation of photoconductivity excitation with wavelength using xenon and deuterium lamp as light sources. Results show that the main band in the photoconductivity spectrum is dependent on the spectral light source emission, the excitation peak reaching 5 eV (deuterium lamp). This band is due to the recombination process involving oxygen species and photogenerated electron-hole pairs. (C) 1999 Elsevier B.V. B.V. All rights reserved.