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.

Preparation of composite retentive areas for removable partial denture retainers

A method is presented in which light-polymerized composite material is used to obtain retention for a removable partial denture when usable natural tooth undercuts are unavailable. The desired contour is waxed on a diagnostic cast with the use of a surveyor, captured in a light-polymerizing temporary restorative material, and reproduced in composite resin on the abutment teeth.

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.

Preparation of zinc sodium polyphosphates glasses from coacervates precursors. Characterisation of the obtained glasses, and their applications

A soft chemistry route is described to obtain glasses in the P2O5-Na2O-ZnO-H2O. It is based on the addition of zinc salts to coacervates prepared from sodium polyphosphate. The processing of these coacervates leads to polyphosphate glasses with the same properties as those of glasses prepared in the classical way. So far, little work has been implemented in this system using 'coacervate route'. However, it makes an attractive method for coating and joining processes on the industrial scale. As the anion associated to zinc may take part in the adhesion mechanism, coacervate formation has been studied using zinc chloride, nitrate and sulphate as starting materials. The physical properties of the glasses obtained by this method are reported and potential applications of zinc and silver coacervate are described. (C) 2002 Academie des sciences / Editions scientifiques et medicales Elsevier SAS.

Preparation of Pb(Zr,Ti)O-3 thin films by soft chemical route

Lead zirconate titanate, Pb(Zr0.3Ti0.7)O-3 (PZT) thin films were prepared with success by the polymeric precursor method. Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), Micro-Raman spectroscopy and X-ray diffraction (XRD) were used to investigate the formation of the PZT perovskite phase. X-ray diffraction revealed that the film showed good crystallinity and no presence of secondary phases was identified. This indicates that the PZT thin films were crystallized in a single phase. PZT thin films showed a well-developed dense grain structure with uniform distribution, without the presence of rosette structure. The Raman spectra undoubtedly revealed these thin films in the tetragonal phase. For the thin films annealed at the 500-700 degreesC range, the vibration modes of the oxygen sublattice of the PZT perovskite phase were confirmed by FT-IR. The room temperature dielectric constant and dielectric loss of the PZT films, measured at 1 kHz were 646 and 0.090, respectively, for thin film with 365 nm thickness annealed at 700 degreesC for 2 h. A typical P-E hysteresis loop was observed and the measured values of P-s, P-r and E-c were 68 muC/cm(2), 44 muC/cm(2) and 123 kV/cm, respectively. The leakage current density was about 4.8 x 10(-7) A/cm(2) at 1.5 V. (C) 2003 Elsevier Ltd. All rights reserved.

Preparation of ZnO nanoparticles: Structural study of the molecular precursor

The structure of zinc acetate derived precursor currently used in the sol-gel synthesis of ZnO nanoparticles is described. The reaction products obtained before and after reflux of ethanolic zinc acetate solution have been studied by UV-Vis, photoluminescence, FTIR and EXAFS at the Zn K edge. EXAFS results evidence for both precursor solutions a change from the octahedral coordination sphere of oxygen atoms characteristic of the solid zinc acetate dihydrate compound into a four-fold environment. The EXAFS spectra of precursor solutions can be satisfactorily reproduced using the molecular structure reported for Zn4O(Ac)(6) (Ac = COOCH3). UV-Vis and FTIR measurements are also in agreement with the formation of this oligomeric precursor. The structural modification is more pronounced after reflux at 80degreesC, because the increase of the Zn4O(Ac)(6) amount and the formation of nearly 3.0 nm sized ZnO nanoparticle.

Preparation of SrBi2Ta2O9 ferroelectric thick films by electrophoretic deposition using aqueous suspensions

SrBi2Ta2O9 ferroelectric thick films were prepared by electrophoretic deposition (EPD). For that, ceramic powders were prepared by chemical method in order to obtain compounds with chemical homogeneity. The polymeric precursor method was used for the synthesis of the SrBi2Ta2O9 powder. The crystallographic structure of the powder was examined by X-ray diffraction, and the surface area was determined by single point BET adsorption. The 0.03 vol% suspension was formed by dispersing the powder in water using two different polymers as dispersants: an ester polyphosphate (C213) and an ammonium polyacrilate (Darvan 821-A). The influence of the different dispersants on the powder surface properties were investigated by zeta potential measurements. The films were deposited on platinum-coated alumina and Pt/Ti/SiO2/Si substrates by electrophoretic deposition using a 4 mA constant current, for 10 min, with two parallel electrodes placed at a separation distance of 3 min in the suspension. Several cycles of deposition-drying of the deposit was carried out until the desired thickness was obtained. After thermal treatment at temperatures ranging from 700 to 1000degreesC, the films were characterized by X-ray diffraction and scanning electron microscopy.

Preparation of new glass systems by the polymeric precursor method for dental applications

Glass ionomer cements (GICs) are largely employed in Dentistry for several applications, such as luting cements for the attachment of crowns, bridges, and orthodontic brackets as well as restorative materials. The development of new glass systems is very important in Dentistry to improve of the mechanical properties and chemical stability. The aim of this study is the preparation of two glass systems containing niobium in their compositions for use as GICs. Glass systems based on the composition SiO2,Al2O3-Nb2O5-CaO were prepared by chemical route at 700degreesC. The XRD and DTA results confirmed that the prepared materials are glasses. The structures of the obtained glasses were compared to commercial material using FTIR, Al-27 and Si-29 MAS-NMR. The analysis of FTIR and MAS-NMR spectra indicated that the systems developed and commercial material are formed by SiO4 and AlO4 linked tetrahedra. These structures are essential to get the set time control and to have cements. These results encourage further applications of the experimental glasses in the formation of GICs. (C) 2004 Elsevier B.V. All rights reserved.

Preparation of 9/65/35 PLZT thin films deposited by a dip-coating process

Crack-free polycrystalline PLZT (Pb,a)(Zr,Ti)O-3 thin films with the perovskite structure were prepared by dir-coating using the Pechinis process. Lead acetate, hydrated lanthanum carbonate, zirconium n-propoxide and titanium isopropoxide were used as raw materials. The viscosity of the solution was adjusted in the range of 20 to 56 cP and the films were deposited by a dip-coating process on silicon (100) as substrate. Solutions with ionic concentration of 0.1 and 0.2 M were used. Thin film deposition was accomplished by dipping the substrates in the solution with control of withdrawal speed from 5 to 20 mm/min. The thin films were thermally treated in two steps: at 300 degreesC amid 650 degreesC. The influence of withdrawal speed. viscosity, heating rate and ionic concentration on the morphology of PLZT thin film was discussed. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Preparation of Fe-Cr-P-Co amorphous alloys by electrodeposition

The effects of bath composition and electroplating conditions on structure, morphology, and composition of amorphous Fe-Cr-P-Co deposits on AISI 1020 steel substrate, priorly plated with a thin Cu deposit, were investigated. The increase of charge density activates the inclusion of Cr in the deposit. However, above specific values of the charge density, which depend on the deposition current density, the Cr content in the deposit decreases. This Cr content decreasing is probably due to the significant hydrogen evolution with the increasing of deposition cur-rent and charge density. The effect of charge density on the content of Fe and Co is not clear. However, there is a tendency of increasing of Fe content and decreasing of Co content with the raising of current density. The Co is more easily deposited than the P, and its presence results in a more intense inhibition effect on the Cr deposition than the inhibition effect caused by P presence. Scanning electron microscope (SEM) analysis showed that Co increasing in the Fe-Cr-P-Co alloys analyzed does not promote the susceptibility to microcracks, which led to a good quality deposit. The passive film of the Fe-Cr-P-Co alloy shows a high ability formation and high protective capacity, and the results obtained by current density of corrosion, j(cor), show that the deposit with addition of Co, Fe31Cr11P28Co30, presents a higher corrosion resistance than the deposit with addition of Ni, Fe54Cr21P20Ni5. (C) 2004 Published by Elsevier B.V.

Preparation of CuO/SiO2 and photocatalytic activity by degradation of methylene blue

A photocatalyst based on CuO/SiO2 was prepared, and evaluated for the degradation of methylene blue in aqueous medium. The photocatalyst was obtained by calcination method of copper salt, in the presence of silica. The characterization by XRD, FTIR, and TPR techniques confirmed the formation of CuO as active phase. SEM studies showed CuO deposited on the surface of SiO2. By ESI-MS, it was demonstrated that the degradation of methylene blue occurs through successive hydroxylations. Photodegradation assays showed that CuO/SiO2 was efficient for degradation, and that the material worked better in the presence of UV light.

New strategies in the preparation of exfoliated thermoplastic starch-montmorillonite nanocomposites

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

Preparation of CeO2 by a simple microwave-hydrothermal method

Cerium carbonate hydroxide (orthorhombic Ce(OH)CO3) hexagonal-shaped microplates were synthesized by a simple and fast microwave-hydrothermal method at 150 degrees C for 30 min. Cerium nitrate, urea and cetyltrimethylammonium bromide were used as precursors. Ceria (cubic CeO2) rhombus-shape was obtained by a thermal decomposition oxidation process at 500 degrees C for 1 h using as- synthesized Ce(OH)CO3. The products were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, thermogravimetric analysis and Fourier transformed infrared spectroscopy. The use of microwave-hydrothermal method allowed to obtain cerium compounds at low temperature and shorter time compared to other synthesis methods. (C) 2008 Elsevier B.V. All rights reserved.

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.

Preparation of N2, N2,7-trimethylguanosine affinity columns

2,2,7-trimethylguanosine (TMG) binding proteins from human cells were purified through TMG-affinity columns. TMG synthesis was improved and the TMG obtained was shown to be similar to the TMG in the 5' cap of the UsnRNAs. The eluates obtained with TMG-affinity chromatographies were very different from those isolated with m7G-affinity columns, thus suggesting that specific TMG- binding proteins were obtained. The fraction may be enriched with factors associated with import and/or hypermethylation of UsnRNPs.