Formation of zirconia foams using the thermostimulated sol-gel transition

In this paper we describe the production of zirconia-based foams by a novel thermostimulated sol-gel route, that employs the foaming of colloidal suspensions prior to the sol-gel transition promoted by small increase of temperature (congruent to3 degreesC). This method produces gelled bodies having porosity >70% in the wet stage, and can be used to produce complex-shaped components. The effect of a foaming agent (Freon11 or CCl3F) and surfactant content on the formation and stability of the foams was analyzed. The rheologic measurements demonstrate that by increasing the surfactant concentration, the gelation time decreases increasing foam stability. As the surfactant concentration and quantity of foaming agent increase, the density decreases and the porosity increases. Hg porosimetry results show that the dry foam presents a bimodal pore size distribution. The family of sub-micrometer pores was attributed to the formation of a microemulsion between Freon11 and water. Scanning electron microscopy analysis shows that the foam structure consists of a three-dimensional network of spherical pores, which may be open and interconnected or closed, at larger or smaller porosities, respectively. Finally these results show that the thermostimulated sol-gel transition provides a potential route for ceramic foam manufacture. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Ultraviolet excitation of photoconductivity in thin films of sol-gel SnO2

Tin dioxide (SnO2) thin film photoconductivity spectra were measured for a large temperature range using a deuterium source, the intensity of photocurrent spectra in the range 200-400 nm is temperature dependent, and the photocurrent increases in the ultraviolet even for illumination with photon energies much higher than the bandgap transition. This behavior is related to recombination of photogenerated electron-hole pairs with oxygen adsorbed at grain boundaries, which is consistent with nanoscopic crystallite size of sol-gel deposited films. (c) 2005 Elsevier Ltd. All rights reserved.

Comparative efficacy evaluation of moxidectin gel and ivermectin paste against internal parasites of equines in Brazil

A total of 24 male and female equines of mixed breed, 10-20 months of age and naturally infected with internal parasites was utilized in a controlled test to evaluate the efficacy of a moxidectin 2% gel formulation at the dosage of 0.4 mg moxidectin per kg of live weight and an ivermectin 1.87% commercial paste formulation at the dosage 0.2 mg ivermectin per kg applied orally Animals were allocated into three groups of eight horses each based on pre-treatment eggs per gram (EPG) counts and treatments were randomized among the groups. One group was kept as untreated controls. One animal in the moxidectin-treated group died before the end of the trial from a cause unrelated to treatment leaving a total of seven animals in this group. Fecal egg counts were performed three times post-treatment and the number of parasites remaining in each animal was determined. Statistical analyses using geometric means were performed at the 1% level of significance. Both moxidectin and ivermectin preparations reduced initial EPG from a mean of 1600 to 0 on Days 5, 7 and at the end of the trial on Day 14. Efficacy percentages of moxidectin and ivermectin against immature and adult nematodes were as follows: Trichostrongylus axel, Parascaris equorum, Strongylus edentatus, S. vulgaris, Triodontophorus spp. and Gyalocephalus capitatus, 100% for both products; Habronema muscae 99.5 and 99.6%, respectively, Strongyloides westeri, 100 and 99.2%, respectively; Oxyuris equi, 99.6 and 100%, respectively; small strongyles, 99.7% for both products. of the latter, the most numerous were: Cylicocyclus insigne, Cylicostephanus longibursatus and Cyathostomum catinatum. No Gasterophilus nasalis were found in horses from either treated group, while two of eight control horses had infections with this parasite. Moxidectin showed greater efficacy (84.9%) than ivermectin (67.8%) against Strongylus vulgaris larvae found in the mesenteric artery aneurisms, but the difference was not statistically significant. Total parasite counts for both treated groups were significantly lower (p<0.01) than in the non-treated group. No significant differences were noted between moxidectin and ivermectin. Efficacy against the 30 nematode species found in this study was very evident for both products. As expected, neither moxidectin nor ivermectin was effective in controlling the tapeworm Anoplocephala perfoliata. No adverse reactions were observed during the experimental period. (C) 1998 Elsevier B.V. B.V. All rights reserved.

Clinical performance of a self-etching adhesive at 18 months

Purpose: To test the null hypothesis that beveling and/or etching enamel would not affect the 18-month clinical performance of the self-etching adhesive Clearfil SE Bond (CSEB) in noncarious cervical lesions (NCCL). Methods: With Institutional Review Board approval, 34 patients were enrolled in this study. A total of 120 NCCL was selected and assigned to four groups: (1) CSEB was applied without any cavity preparation; (2) CSEB was applied after beveling enamel; (3) CSEB was applied after etching enamel for 15 seconds with 35% phosphoric acid; (4) CSEB was applied after beveling and etching enamel. A microfilled composite resin was used for all restorations. Resuts: At 6 months after initial placement, 120 restorations (a 100% recall rate) were evaluated. At 18 months, 87 restorations (a 72.5% recall rate) were available for evaluation. A survival rate of 100% was measured for all groups at both 6 and 18 months. Sensitivity to air decreased significantly only for Group 3 (no bevel+acid etch) from baseline to 18 months without statistical changes from 6 months to 18 months. None of the other parameters resulted in significant differences for any of the four groups. However, when data were pooled, both the overall marginal discoloration and the overall marginal adaptation were significantly worse at 18 months than at baseline, while sensitivity to air decreased significantly from baseline to 18 months. The 18-month survival rate of the self-etching adhesive Clearfil SE Bond was not improved by enamel bevel or by enamel etching. Both overall marginal adaptation and overall marginal discoloration were worse at 18 months than at baseline.

O processo sol-gel: uma visão físico-química

The aim of this work was to revise the main concepts involved in the physical-chemistry of the sol-gel process. First, the preparation and its influence on the gel's structure are focalized; the sol-gel transition is revised under the thermodynamics of crytical phenomena point of view and by considering the kinetic models of aggregation. Second, the experimental methods usually used to characterize the sol-gel transition are discussed.

Catalysis and temperature dependence on the formation of ZnO nanoparticles and of zinc acetate derivatives prepared by the sol-gel route

The chemical and structural nature of powders prepared from the zinc acetate-derived precursor using the sol-gel route is discussed. The influence of the synthesis temperature and of the hydrolytic catalyst on the structural features of the powder is focused on the basis of X-ray powder diffraction (XRPD) and extended X-ray absorption fine structure (EXAFS) measurements and complemented with density and thermoanalysis (TG-DTA) results. EXAFS and XRPD results show that no-washed nanoparticulate powders are composed of a mixture of ZnO (wurtzite), zinc acetate, and zinc hydroxyacetate. The latter has a layered structure typical of hydroxy double salts (HDS). The main component of no-washed powders is always unreacted zinc acetate solid but the relative amount of the zinc-based compounds depends on the nature of the hydrolytic catalyst, hydrolysis ratio, and of synthesis temperature. According to the proportion of the three zinc-based compounds, three families of powders could be distinguished. The amount of ZnO nanoparticles (1.6 +/- 0.6 nm) decreases as the synthesis temperature increases, as the hydrolysis ratio decreases, or by changing from basic to acid catalysis. This finding suggests that the formation of zinc compounds is controlled by the equilibrium between hydrolysis-condensation and complexation-reprecipitation reactions.

Influence of age on the behavior of dental pulp of dog teeth after capping with an adhesive system or calcium hydroxide

This study evaluated histomorphologically the influence of chronological age of the dog on the dental pulp-healing process after capping with the All Bond 2 system or with calcium hydroxide paste. The animals were divided according to age into young and adult groups. Class 5-type cavities were prepared, and the pulp was submitted to an exposure of a diameter of 0.5 mm. The pulp of the teeth was then protected with the adhesive system or with a calcium hydroxide paste. Sixty days after treatment, the results obtained with the adhesive system in the young group were significantly better than those in the adult group. With calcium hydroxide, the results were similar for both groups. The pulp treated with calcium hydroxide exhibited a complete hard tissue bridge and a pulp without inflammatory reaction, a fact not observed when the adhesive system was used. In conclusion, the chronological age of the pulp influenced the comparative results only for the adhesive system (P = 0.1), and the total results were better with calcium hydroxide than with the All Bond 2 system (P = 0.01).

Small-angle X-ray scattering study of gelation and aging of Eu3+-doped sol-gel-derived siloxane-poly(oxyethylene) nanocomposites

The aggregation, gelation, and aging of urea-cross-linked siloxane-poly(oxyethylene) nanohybrids [(U600)-n] containing two different amounts of europium triflate initially dissolved in an ethanol-water mixture were investigated by in situ small-angle X-ray scattering (SAXS). For both low (n = [O]/[Eu] = 80) and high (n = 25) europium contents, the SAXS intensity was attributed to the formation of siloxane clusters of about 8-11 Angstrom in size. Siloxane cluster formation and growth is a rapid process in hybrids with low Eu contents and slow in Eu-rich hybrids. An additional contribution to the scattering intensity at very low angles was attributed to the formation of a coarse structure level. At this secondary level, the structure can be described as a set of dense domains containing siloxane clusters embedded in a depleted matrix composed of unfolded polymer chains and solvent. By fitting a theoretical function for this model to the experimental SAXS curves, relevant structural parameters were determined as functions of time during the sol-gel transition and gel aging. For hybrids with low europium contents (n = 80), the size of the siloxane clusters remains essentially invariant, whereas the dense segregation domains progressively grow. In hybrids with high doping contents (n = 25), the preponderant structure variation during the first stages of the sol-gel transformation is the slow growth of siloxane clusters. For these hybrids, the segregation of siloxane clusters forming dense domains occurs only during advanced stages of the process.

Characterization of the porosity developed in a new titania-alumina catalyst support prepared by the sol gel route

Titanium oxide (TiO2) is a good candidate for support of hydrotreating catalysts but has the disadvantage of presenting a low surface area and a poor thermal stability when compared with Al2O3. A mixed TiO2-Al2O3 support was proposed as an alternative that is expected to be free from these drawbacks. The variation during firing of the nanoporous texture of supports composed of TiO2-Al2O3, TiO2 and Al2O3 was studied by small angle X-ray scattering (SAXS). The supports were prepared by the sol-gel route using Ti and Al isopropoxides. We have particularly analyzed the effects of acid and basic hydrolysis on the nanostructural features of catalyst supports fired at different temperatures. The nanopore radius distribution functions were determined from SAXS results assuming a simple model of spherical nanopores embedded in a homogeneous solid matrix. The modal pore radius in both pure TiO2 and pure Al2O3 supports grows from 1.3 to 2.2 nm as the firing temperature increases from 673 to 973 K. on the other hand, the modal pore radius in the mixed TiO2-Al2O3 support remains below 1.2 nm over the same range of firing temperatures. These results demonstrate the good thermal stability of the nanoporous texture of mixed TiO2-Al2O3 supports.

Study of structural surface modified tin oxide membrane prepared by sol-gel route sintered at 400 degrees C

This work describes the chemical modification by Tiron(R) molecules of the surface of SnO2 nanoparticles used to prepare nanoporous membranes. Samples prepared with Tiron(R) content between 1 and 20 wt% and fired at 400 C were characterised by X-Ray Powder Diffraction (XRPD), Extended X-ray Absorption Fine Structure (EXAFS), N-2 adsorption isotherms analysis and permeation experiments. XRPD and EXAFS results show a continuous reduction of crystallite size by increasing the Tiron(R) contents until 7.5 wt%. The control exercised by Tiron(R) modifying agent in crystallite growth allows the fine tuning of the average pore size that can be screened from 0.4 to 4 nm as the amount of grafted molecules decreases from 10 to 0 wt%. In consequence, the membrane cut-off can be screened from 1500 to 3500 g.mol(-1).