Numerical simulation of the liquid phase in SnO2 thin film deposition by sol-gel-dip-coating

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Raman and photoluminescence of Er3+-doped SnO2 obtained via the sol-gel technique from solutions with distinct pH

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of cassava starch content and sintering temperature on the alumina consolidation technique

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Silver nanoparticles: influence of stabilizing agent and diameter on antifungal activity against Candida albicans and Candida glabrata biofilms

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Nanopore size growth and ultrafiltration performance of SnO2 ceramic membranes prepared by sol-gel route

Supported ceramic membranes have been produced by the sol-casting procedure from aqueous colloidal suspensions prepared by the sol-gel route. Coatings on a tubular alumina support have been successfully performed leading to crack free layers. Samples have been sintered at 400, 500 and 600 degreesC, and the effect of heating treatment on the nanostructure and on the ultrafiltration properties are analyzed. The characterization has been done by high resolution scanning electron microscopy, nitrogen adsorption-desorption isotherms, water permeation and cut-off determination using polyethylene glycol standard solutions. The micrographs have revealed that grains and pore size increase with the temperature, whereas their shape remains invariant. This results is in agreements with N-2 adsorption-desorption analyses, which have revealed that the mean pore size diameter increases from 4 to 10 nm as the sintering temperature increases from 400 to 600 degreesC, while the total porosity remains constant. Furthermore, the tortuosity, calculated from water permeability, is essentially invariant with the sintering temperatures. The membranes cut-off, determined with a retention rate equal to 95%, are 3500, 6500 and 9000 g . mol(-1) for 400, 500 and 600 degreesC, respectively, showing that the permeation properties of SnO2 ultrafiltration membranes can easily be controlled by sintering condition.

Vidros recobertos com camadas delgadas transparentes de SnO2

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

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.

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.

Small angle X-ray scattering study of surface modified tin oxide nanoparticles prepared by sol-gel route

The surface properties of SnO2 nanoparticles were modified by grafting ionic (Tiron (R). (OH)(2)C6H2(SO3Na)(2)(H2O)-H-.) or non-ionic (Catechol (R). C6H4-1,2-(OH)(2)) capping Molecules during aqueous sol-gel processing to improve the redispersibility of powdered xerogel. The effect of the amount of grafted organic molecules on the redispersibility of powders in aqueous solution at several basic pH values was Studied. The nanostructural features of the colloidal suspensions were analyzed by small angle X-ray scattering (SAXS) measurements. Irrespective of the nature and amount of grafted molecules, complete redispersion was obtained in aqueous solution at pH = 13. The redispersion at pH = 11 results in a mixture of dispersed primary particles and aggregates. The proportion of well dispersed nanoparticles and aggregates (and their average size) can be tuned by the quantity of grafted ionic molecules.

Formation of SnO2 supported porous membranes

In this work, the effect of the substrate microstructure on the formation of SnO2 membranes and of the sintering conditions on their porosity have been analysed. Samples have been prepared by colloidal suspensions cast on alumina or kaolin substrates. Supported membranes have been characterized by Hg porosimetry, MEV, XRD and N-2 adsorption-desorption isotherms. The results show that the narrower pore size distribution of alumina substrate allowed to prepare membranes more homogeneous and free of cracks than that supported on kaolin. The crystallite and pore sizes of the membranes could be controlled by adjusting the temperature of sintering, allowing materials with adequate microstructure with application for ultrafiltration process.

Electrical characterization of SnO2 : Sb ultrathin films obtained by controlled thickness deposition

A representative study is reported on the electrical properties of SnO2: Sb. ultrathin films (thickness of 40-70 nm) produced by a deposition method based on aqueous colloidal suspensions of 3-5 nm crystalline oxides. The results revealed the films' electrical behavior in a range of 10-300 K, showing a strong dependence on dopant incorporation, with minimum resistivity values in 10 mol % of Sb content. All the samples displayed semiconductor behavior, but the transport mechanism showed a strong dependence on thickness, making it difficult to fit it to well-known models. In thicker films, the mechanism proved to be an intermediary system, with thermally activated and hopping features. Electron hopping was estimated in the range of 0.4-1.9 nm, i.e., in the same order as the particle size. (c) 2007 American Institute of Physics.

Structure of SnO2 alcosols and films prepared by sol-gel dip coating

To obtain SnO2 films to be used for surface protection of fluoride glasses, a non-aqueous sol-gel route for the preparation was developed. An ethanolic SnO2 colloidal suspension was prepared by thermohydrolysis of SnCl4 solution at 70 degreesC. By using this procedure, redispersable powders with nanometer sized particles were obtained. Films were obtained by dip coating on glass and mica substrates. The structures of the ethanolic precursor suspension and films were compared to those of similar samples prepared by the classical aqueous sol-gel route. Comparative analyses performed by photon correlation spectroscopy demonstrated that the powders obtained by freeze-drying are fully redispersable either in aqueous or in alcoholic solutions at pH greater than or equal to 8. As prepared sols and redispersed colloidal suspensions have hydrodynamic radius distribution (2-14 nm) with an average size close to 7 nm. The variations in film structures with firing temperature were investigated by small-angle X-ray scattering and X-ray reflectometry. The experimental results show that the films have a two level porous structure composed of agglomerates of primary colloidal particles. The sintering of the primary particles leads to the densification of agglomerates and to the formation of inter-agglomerate spatially correlated pores. The volume fraction of intra-agglomerate pores is reduced from approximate to 50% to approximate to 30% by the precipitation of precursor salts partially hydrolyzed in ethanolic solution. (C) 2001 Elsevier B.V. B.V. All rights reserved.

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.

Optical characteristics of Er3+-Yb3+ doped SnO2 xerogels

Er3+ doped SnO2 xerogels have been obtained from aqueous colloidal suspensions. Emission and excitation spectra were obtained and allowed the identification of two main families of sites for Er3+. In the first one Er3+ substitutes for Sn4+ in the SnO2 cassiterite structure. In the second Er3+ are found adsorbed at the SnO2 particle surface. For the first family of sites the technological important infrared Er3+ emission about 1.5 mum is efficiently excited through absorption at the SnO2 conduction band at 3.8 eV. on the other hand the emission due to adsorbed ions appears inhomogeneously broadened by the statistical distribution of sites available for Er3+ ions at the surface of the particles. Moreover it is not excited by the host. The emission of this second family of sites could be also excited by an energy transfer mechanism involving Yb3+ ions also adsorbed a posteriori at particles surface. Results are compared with spectra obtained for Eu3+ doped samples. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Photoluminescence in quantum-confined SnO2 nanocrystals: Evidence of free exciton decay

Nanocrystalline SnO2 quantum dots were synthesized at room temperature by hydrolysis reaction of SnCl2. The addition of tetrabutyl ammonium hydroxide and the use of hydrothermal treatment enabled one to obtain tin dioxide colloidal suspensions with mean particle radii ranging from 1.5 to 4.3 nm. The photoluminescent properties of the suspensions were studied. The particle size distribution was estimated by transmission electron microscopy. Assuming that the maximum intensity photon energy of the photoluminescence spectra is related to the band gap energy of the system, the size dependence of the band gap energies of the quantum-confined SnO2 particles was studied. This dependence was observed to agree very well with the weak confinement regime predicted by the effective mass model. This might be an indication that photoluminescence occurs as a result of a free exciton decay process. (C) 2004 American Institute of Physics.