Zirconia foams prepared by integration of the sol-gel method and dual soft template techniques

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Sol-gel synthesis of mesoporous CaCu3Ti4O12 thin films and their gas sensing response

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

SnO2:Eu nanocrystallites in SnO2 monolithic xerogels

By simple room temperature broad band time-resolved spectroscopy it was possible to discriminate different Eu3+ spectra in SnO2 monolithic gels obtained by a sol-gel synthetic route. Nanocrystalline domains of the cassiterite-like SnO2:Eu could be easily identified in the transparent medium. From X-ray diffraction profiles a mean particle radius of 2.2 nm was estimated. © 1992.

Pore size distribution of unsupported SnO2 membranes prepared by sol-gel process - Code: EP21

Unsupported SnO2 membranes were prepared by sol-gel process and characterized by N2 adsorption-desorption isotherms and X-ray diffraction. Results show that the texture of dried samples does not change appreciably with the concentration of electrolyte. All of the pore size range used in ultrafiltration process was screened using sintering temperature between 300 and 700°C. © 1994 Kluwer Academic Publishers.

Evolution of the fractal structure during sintering of SnO2 compacted sol-gel powder

The structural evolution during sintering of compacted SnO2 sol-gel powder was investigated using nitrogen adsorption isotherm analysis. Results show that for sintering temperatures up to 400°C the samples have a fractal pore size distribution. As the sintering temperature increases, a structural rearragement occurs, allowing an increase of the efficiency of particle packing and the reduction of fractality. Above 400°C, the pore size growth associated with grain coalescence is the main structural change observed as the sintering temperature increases. © 1995.

Time evolution of the structure function and dynamical scaling in porous SnO2 dry gels

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Short Range Order Evolution in the Preparation of SnO2 Based Materials

The evolution of Eu3+ doped SnO2 xerogels to the cassiterite structure observed during sintering was studied by means of Eu3+ spectroscopy, XRD and EXAFS at the Sn K-edge. Eu3+ ions adsorbed at the surface of colloidal particles present a broad distribution of sites, typical of oxide glasses. With sintering at 300°C, this distribution is still broadened. Crystallization is clearly observed by the three techniques with increasing sintering temperature. It is found that the addition of Eu3+ limits the crystallite growth.

EXAFS and XRD Study of the Structural Evolution during Isothermal Sintering of SnO2 Xerogels

The formation of an ordered (crystalline) phase during isothermal sintering of SnO2 monolithic xerogels, at 200, 250, 300, 400, 500, 600 and 700°C, has been analyzed by the combined use of EXAFS and XRD techniques. For the desiccated gel (110°C), EXAFS results show the formation of small microcrystallites with the incipient cassiterite structure. Between 110 and 250°C, the dehydratation reaction leads to an amorphization evidenced by a decrease of the long and short range crystallographic order. It is due to fissure formation in the xerogel network. For higher temperatures, a continuous coagulation of the crystallites occurs, leading to grain growth. Grain and pore growth obeys the same kinetic relation, so that the microstructure grows by simple enlargement while its morphology is static.

Evolution of the viscoelastic properties of SnO2 colloidal suspensions during the sol-gel transition

This paper describes the effect of the concentration of electrolyte and pH on the kinetics of aggregation and gelation processes of SnO2 colloidal suspensions. Creep, creep-recovery, and oscillatory rheological experiments have been done in situ during aggregation and gelation. A phenomenological description of the structure of the colloidal system is given from the time evolution of rheological parameters. The dependence of the equilibrium steady-state shear compliance on the terminal region of clusters or aggregates seems to be a way to determine the beginning of interconnection of aggregates and the gel point. We propose that at this point the equilibrium steady-state compliance is a minimum. The steady-state viscosity determined from creep experiment can be fit with a power law with the extent of the transformation, giving critical exponent s = 0.7 ± 0.1. The value of the critical exponent Δ = 0.78 ± 0.05 was determined from oscillatory experiment. These results indicate that gelation of SnO2 colloidal suspension exhibits the typical scale expected from the scalar percolation theory. © 2000 Elsevier Science B.V. All rights reserved.

Synthesis of manganese porphyrinosilica imprinted with templates using the sol-gel process

The optimized conditions for the preparation of a new manganese porphyrinosilica-template material are reported. The manganese porphyrinosilica-template was prepared by the sol-gel process, by the reaction of -SO2Cl groups present in the phenyl rings of MnTDC(SO2Cl)PPCl with 3-aminopropyltriethoxysilane. The reaction produces a precursor porphyrinopropylsilyl species, which were then polymerized with tetraethoxysilane. The presence of manganese porphyrin on xerogel is confirmed by ultraviolet visible absorption spectroscopy and thermogravimetric analysis (TGA). The prepared materials have surface areas between 19 and 674 m2 g-1. Electron spectroscopy imaging of the materials show that manganese distribution in the xerogel is uniform. Both manganese(III) porphyrinosilica-template and a similar iron(III) porphyrinosilica-template can catalyze the epoxidation of cyclooctene using iodozylbenzene as oxygen donor. The metalloporphyrinosilica-template presents catalytic activity similar to that of metaloporphyrin in solution. © 2000 Elsevier Science B.V. All rights reserved.

A surface modification for hydrogen storage intermetallic particles by sol-gel method

A new process for the surface modification of hydrogen storage intermetallic particles used as anode material in secondary batteries is proposed in this article. The copper oxide particles coverage obtained by the sol-gel method is proposed to produce, under operational conditions of a Ni-MH battery, a metallic framework that tolerates the volume changes in charge/discharge cycles and does not inhibit the hydrogen absorption. Furthermore it was noticed an enhancement on the discharge capacity of the electrode material that can be related to a new hydrogen storage phase or to an inhibition of the surface oxidation promoted by the film coverage.

Caracterização textural e estrutural de V 2O 5/TiO 2 obtidos via sol-gel: Comparação entre secagem convencional e supercrítica

This work describes a modified sol-gel method for the preparation of V 2O 5/TiO 2 catalysts. The samples have been characterized by N 2 adsorption at 77K, x-ray diffractometry (XRD) and Fourier Transform Infrared (FT-IR). The surface area increases with the vanadia loading from 24 m 2 g -1, for pure TiO 2, to 87 m 2 g -1 for 9wt.% of V 2O 5. The rutile form is predominant for pure TiO 2 but became enriched with anatase phase when vanadia loading is increased. No crystalline V 2O 5 phase was observed in the catalysts diffractograms. Two species of surface vanadium observed by FT-IR spectroscopy a monomeric vanadyl and polymeric vanadates, the vanadyl/vanadate ratio remains practically constant.

Contribution of oxygen related defects to the electronic transport in SnO2 sol-gel films

SnO2 deposited by sol-gel is a polycrystalline film with small grain size. Oxygen present at a less grain boundary traps electrons and then the depletion layer around the potential barrier of the grain boundary becomes wider, comparable to the grain size. We have modeled the conductivity taking into account the trapped charge at the depletion layer of the grain boundary and other scattering mechanisms such as ionized impurity and polar optical. Experimental data of photoconductivity of SnO2 sol-gel films are simulated considering the dominant scattering at grain boundary and crystallite bulk. The fraction of trapped charge at the grain boundary depends on temperature and wavelength of irradiating light, being as high as 50% for illumination in the range 500-600 nm for SnO2-2%Nb as grown sample annealed in air to 550°C. This fraction can be quite reduced depending on exposure to light and annealing under different oxygen partial pressure conditions.

Effects of bleaching with carbamide peroxide gels on microhardness of restoration materials

The objective of this in vitro study was to quantitatively assess the effects of bleaching with 10 and 15% carbamide peroxide (CP) on restoration materials by performing superficial microhardness analysis. Acrylic cylindrical containers (4 x 2 mm) were filled with the following restoration products: Charisma (Heraues Kulzer, Vila Santa Catarina, São Paulo, Brazil), Durafill VS (Heraeus Kulzer), Vitremer (3M, Sumaré, São Paulo, Brazil), Dyract (Dentsply, Petrópolis, Rio de Janeiro, Brazil), and Permite C (SDI, São Pauio, São Paulo, Brazil). Sixty samples were prepared of each restoration material. Twenty samples received bleaching treatment with 10% CP, 20 samples received bleaching treatment with 15% CP, and 20 samples were kept submerged in artificial saliva, which was replaced daily. The treatment consisted of immersion of the specimens in 1 cm3 of CP at 10 and 15% for 6 hours per day during 3 weeks, whereupon the test specimens were washed, dried, and kept immersed in artificial saliva for 18 hours. Then the test and control specimens were analyzed using a microhardness gauge. The Knoop Hardness Number (KHN) was taken for each test and control specimen at five different locations by applying a 25 g force for 20 seconds. The values obtained were transformed into KHNs and the mean was calculated. The data were submitted to statistical analysis by analysis of variance and Tukey test, p < .05. The means/standard deviations were as follows: Charisma: CP 10% 38.52/4.08, CP 15% 34.31/6.13, saliva 37.36/4.48; Durafill VS: CP 10% 18.65/1.65, CP 15% 19.38/2.23, saliva 18.27/1.43; Dyract AP: CP 10% 30.26/2.81, CP 15% 28.64/5.44, saliva 33.88/3.46; Vitremer: CP 10% 28.15/3.04, CP 15% 17.40/3.11, saliva 40.93/4.18; and Permite C: CP 10% 183.50/27.09, CP 15% 159.45/5.78, saliva 215.80/26.15. A decrease in microhardness was observed for the materials Dyract AP, Vitremer, and Permite C after treatment with CP at 10 and 15%, whereas no effect on either of the two composites (Charisma and Durafill) was verified. CLINICAL SIGNIFICANCE: The application of the carbamide peroxide gels at 10 and 15% did not alter the microhardness of the composite resins Charisma and Durafill. In situ and clinical studies are necessary to enable one to conclude that the reduction in microhardness of the materials effectively results in clinical harm to the restorations.