Sintering and crystallite growth of nanocrystalline copper doped tin oxide

The effect of Cu2+ contents and of firing temperature on sintering and crystallite growth of nanocrystalline SnO2 xerogels was analyzed by thermoanalysis (mass loss (TG), linear shrinkage, and differential thermal analysis (DTA)), X-ray powder diffraction (XRPD), and EXAFS (extended X-ray absorption fine structures) measurements. Samples were prepared by two methods: (a) coprecipitation of a colloidal suspension from aqueous solution containing both Sn(IV) and Cu(II) ions and (b) grafting copper(II) species on the surface of tin pride gel. The thermoanalysis has shown that the shrinkage associated with the mass loss decreases by increasing the amount of copper. The EXAFS measurements carried out at the Cu K edge have evidenced the presence of copper in substitutional solid solution for the dried xerogel prepared with 0.7 mol % of copper, while for higher concentration of doping, copper has been observed also at the external surface of crystallites. The solid solution is metastable and copper migrates toward the surface during firing. The XRPD and DTA results have shown a recrystallization process near 320 degrees C, which leads to crystallite growth. The presence of copper segregated near the crystallite surface controls its growth.

SAXS study of formation and growth of tin oxide nanoparticles in the presence of complexing ligands

The effect of acetylacetone (acac) complexing ligand on the formation and growth of tin oxide-based nanoparticles during thermohydrolysis at 70 degreesC of a tin precursor SnCl4-n(acac)(n) (0 less than or equal to n less than or equal to 2) solution was analyzed by in situ small-angle X-ray scattering. A. transparent and stable sol was obtained after 2 h of thermohydrolysis at 70 degreesC, allowing the quantitative determination of the particle volume distribution function and its variation with the reaction time. The number of colloidal particles for equivalent thermohydrolysis temperature and time decreases as the [acac]/[Sn] ratio in initial solution increases from 0.5 to 6. Instead, the amount of soluble species remaining in solution increases for increasing [acac]/[Sn] ratio within the same range. This indicates that increasing amounts of Sn-acetylacetone complexes partially prevent the hydrolysis and consequent formation of colloidal particles. The N-2 adsorption isotherm characterization of freeze-dried powders demonstrates that the average pore size is approximately equal to the average size (approximate to9 Angstrom) of the colloidal primary particles in the sol, and that the porosity and surface area (approximate to200 m(2) g(-1)) are independent of the acac content in the initial solution.

An infection control protocol: effectiveness of immersion solutions to reduce the microbial growth on dental prostheses

This investigation evaluated the effectiveness of an infection control protocol for cleansing and disinfecting removable dental prostheses. Sixty-four dentures were rubbed with sterile cotton swab immediately after they had been taken from patients' mouths. Samples were individually placed in the culture medium and immediately incubated at 37 +/- 2 degreesC. The dentures were scrubbed for 1 min with 4% chlorhexidine, rinsed for 1 min in sterile water and placed for 10 min in one of the following immersion solutions: 4% chlorhexidine gluconate, 1% sodium hypochlorite, Biocide (iodophors) and Amosan (alkaline peroxide). After the disinfection procedures, the dentures were immersed in sterile water for 3 min, reswabbed and the samples were incubated. All samples obtained in the initial culture were contaminated with micro-organisms. All the lower dentures immersed in Biocide showed positive growth, and the upper dentures were positive for growth in six of eight dentures. The 4% chlorhexidine gluconate, 1% sodium hypochlorite and Amosan solutions have been proved effective to reduce the growth of the micro-organisms in the 10 min immersion period. The protocol evaluated in this study seems to be a viable method to prevent cross-contamination between dental personnel and patients.

Mesoproterozoic rapakivi granites of the Rondonia Tin Province, southwestern border of the Amazonian craton, Brazil - I. Reconnaissance U-Pb geochronology and regional implications

Rapakivi granites and associated mafic and ultramafic rocks in the Rondonia Tin Province, southwestern Amazonian craton, Brazil were emplaced during six discrete episodes of magmatism between ca 1600 and 970 Ma. The seven rapakivi granite suites emplaced at this time were the Serra da Providencia Intrusive Suite (U-Pb ages between 1606 and 1532 Ma); Santo Antonio Intrusive Suite(U-Pb age 1406 Ma), Teotonio Intrusive Suite (U-Pb age 1387 Ma); Alto Candeias Intrusive Suite (U-Pb ages between 1346 and 1338 Ma); Sao Lourenco-Caripunas Intrusive Suite (U-Pb ages between 1314 and 1309 Ma); Santa Clara Intrusive Suite (U-Pb ages between 1082 and 1074 Ma); and Younger Granites of Rondonia (U-Pb ages between 998 and 974 Ma). The Serra da Providencia Intrusive Suite intruded the Paleoproterozoic (1.80 to 1.70 Ga) Rio Negro-Juruena crust whereas the other suites were emplaced into the 1.50 to 1.30 Ga Rondonia-San Ignacio crust. Their intrusion was contemporaneous with orogenic activity in other parts of the southwestern Amazonian craton, except for the oldest, Serra da Providencia Intrusive Suite. Orogenic events coeval with emplacement of the Serra da Providencia Intrusive Suite are not clearly recognized in the region. The Santo Antonio, Teotonio, Alto Candeias and Sao Lourenco-Caripunas Intrusive Suites are interpreted to represent extensional anorogenic magmatism associated with the terminal stages of the Rondonian-San Ignacio orogeny. At least the Sao Lourenco-Caripunas rapakivi granites and coeval intra-continental rift sedimentary rocks may, in contrast, represent the products of extensional tectonics and rifting preceding the Sunsas/Aguapei orogeny (1.25 to 1.0 Ga). The two youngest rapakivi suites, the Santa Clara Intrusive Suite and Younger Granites of Rondonia, seemingly represent inboard magmatism in the Rondonian-San Ignacio Province during a younger episode of reworking in the Rio Negro-Juruena Province during the waning stages of the collisional 1.1 to 1.0 Ga Sunsas/Aguapei orogeny. The six intra-plate rapakivi granite episodes in the southwestern part of the Amazonian craton form three broad periods of anorogenic magmatism that have age-correlative events composed of similar rocks and geologic environments in eastern Laurentia and Baltica, although the exact timing of magmatism appears slightly different. Recognition of lithologic and chronological correlations between various cratons provide important constraints to models explaining the interplay between rapakivi granite magmatism and deep crustal evolution of an early Mesoproterozoic supercontinent. They are, furthermore, important to plate tectonic models for the assembly, dispersal and reassembly of Amazonia, Laurentia and Baltica in the Mesoproterozoic and Neoproterozoic. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Influence of the oxygen adsorbed on tin varistors doped with Co, Mn and Cr oxides

The non-ohmic properties of the 98.90% SnO2+(1-x)%CoO+0.05% Cr2O3+0.05% Nb2O5+x% MnO2 varistor system (all of them in mol %), as well as the influence of the oxidizing and reducing atmosphere on this system were studied in this work. Experimental evidence indicates that the electrical properties of the varistor depend on the defects that occur at the grain boundary and on the adsorbed oxygen species such as O''(2), O'(2), O in this region. Thermal treatments at 900 degreesC in oxygen and nitrogen atmospheres indicated such a dependence with the values of the non-linearity coefficient (alpha) increasing under oxygen atmosphere, being reduced in nitrogen atmosphere and restored after a new treatment in oxygen atmosphere, presenting a reversibility in the process. EDS analysis accomplished by SEM showed the distribution of the oxides in the varistor matrix. (C) 2002 Kluwer Academic Publishers.

Hydrophilization of PVC surfaces by argon plasma immersion ion implantation

Commercial polyvinylchloride (PVC) sheets were treated by plasma immersion ion implantation, PIII. Samples were immersed in argon glow discharges and biased with 25 kV negative pulses. Exposure time to the bombardment plasma changed from 900 to 10,800 s. Through contact angle measurements, the effect of the exposure time on the PVC wettability was investigated. Independent of t, all samples presented contact angles, theta, equal to zero after the treatment. However, in some cases, surface hydrophilization was not stable, as revealed by the temporal evolution of theta. Samples bombarded for shorter periods recovered partially or totally the hydrophobic character while the one exposed for the longest time stayed highly hydrophilic. These modifications are ascribed to the Cl loss and O incorporation as shown by XPS measurements. Furthermore, the mobility of surface polar groups and the variation in the cross-linking degree can also affect the PVC wettability.

Electrochemical study of perchlorate reduction at tin electrodes

The electrochemical behaviour of tin in de-aerated sodium perchlorate was studied using potentiodynamic and potentiostatic techniques. Tin behaviour in sodium perchlorate has been complicated unexpectedly by the reduction of the perchlorate anion. It is shown that the reduction process takes place within a potential region comprising the negative side of the double layer region and the positive side of the hydrogen region (-0.7 less than or equal to E less than or equal to -1.3 V). The presence of oxide on the electrode surface favours the reduction reaction, which may occur in two steps: the formation of basic tin(II) chloride followed by its reduction, producing chloride.

Thermal behaviour of Tin(II) complex with 8-hydroxyquinolinate in the solid state

Tin(II) complexes with 8-hydroxyquinolinate in solid state have been obtained by adding aqueous ammonium to a solution containing stannous chloride and 8-hydroxiquinoline in medium of HCl and acetone up to pH 5 and 9, respectively. The products obtained show the same composition, Sn(C9H6ON)(2); however there are some differences regarding both the thermal behaviour in an oxidant atmosphere and morphology. These products were characterised by elemental and complexometric analysis, TG and DTA curves, infrared and X-ray diffractometry. TG curves show, above 448 K, the partial oxidation on air atmosphere of Sn(II) complexes to Sn(IV) complexes, SnO(C9H6ON)(2). This behaviour does not depend only on pH in which the compounds were obtained but also on the heating rate in TG curves. Sn(II) complexes volatilise almost completely on nitrogen atmosphere and partially on air atmosphere depending on the oxidation degree of the compound.

Geological evolution of the basement rocks in the east-central part of the Rondonia Tin Province, SW Amazonian craton, Brazil: U-Pb and Sm-Nd isotopic constraints

On the basis of geologic, petrologic, and U-Pb geochronologic data the basement rocks in the east-central part of the Rondonia Tin Province (RTP, southwestern Amazonian craton) are grouped into five lithologic associations: (1) tonalitic gneiss (1.75 Ga); (2) enderbitic granulite (1.73 Ga); (3) paragneiss; (4) granitic and charnockitic augen gneisses (1.57-1.53 Ga); and (5) fine-grained granitic gneiss and charnockitic granulite (1.43-1.42 Ga). The first three are related to development of the Paleoproterozoic Rio Negro-Juruena Province and represent the oldest crust in the region. The tonalitic gneisses and enderbitic granulites show calc-alkaline affinities and Nd isotopic compositions (initial epsilon(Nd) = +0-1 to -1.5; T-DM of 2.2-2.1 Ga) that suggest a continental arc margin setting for the original magmas. The paragneisses yield T-DM values of 2.2-2.1 Ga suggesting that source material was primarily derived from the Ventuari-Tapajos and Rio Negro-Juruena crusts, but detrital zircon ages and an intrusive granitoid bracket deposition between 1.67 and 1.57 Ga. The granitic and charnockitic augen gneisses show predominantly A-type and within-plate granite affinities, but also some volcanic arc granite characteristics. The initial epsilon(Nd) values (+0.6 to +2.0) indicate mixing of magmas derived from depleted mantle and older crustal sources. These rocks are correlated to the 1.60-1.53 Ga Serra da Providencia intrusive suite that reflects inboard magmatism coeval with the Cachoeirinha orogen located to the southeast. The fine-grained granitic gneiss and charnockitic granulites represent the first record of widespread magmatism at 1.43-1.42 Ga in northern Rondonia. Their geochemical signatures and the slightly positive initial epsilon(Nd) values (+0.7 to +1.2) are very similar to those of the most evolved granites of the calc-alkaline Santa Helena batholith farther southeast. U-Pb monazite and Sm-Nd whole-rock-garnet ages demonstrate that a high-grade tectonometa-morphic episode occurred in this region at 1.33-1.30 Ga. This episode attained upper-amphibolite conditions and is interpreted as the peak of the Rondonian-San Ignacio orogeny. The U-Pb and Sm-Nd data presented here and data published on rapakivi granites elsewhere indicate that the east-central part of the RTP is a poly-orogenic region characterized by successive episodes of magmatism, metamorphism, and deformation between 1.75 and 0.97 Ga. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Hardness and compressive strength of indirect composite resins: effects of immersion in distilled water

The aim of this study was to evaluate the effect of ageing in distilled water on the hardness and compressive strength of a direct composite resin Z100, a feldspatic porcelain (Noritake) and three indirect composites (Artglass, Solidex and Targis). For the Vickers hardness tests, five disk-shaped specimens (2 x 4 mm) of each material were prepared according to the manufacturers' instructions. The hardness tests were conducted using a Vickers diamond indentor. Compressive strength measurements were recorded on cylindrical specimens with a diameter of 6 mm and a length of 12 mm. The compression tests were carried out with a constant cross-head speed of 0.5 mm min(-1) on a mechanical test machine. For each material, 10 specimens were tested after 7 days of dry storage at 37 +/- 1 degreesC and 10 specimens were tested after water storage at 37 +/- 1 degreesC for 180 days. Noritake porcelain specimens showed higher hardness values than the composites. Among the composite materials, Z100 promoted the highest VHN values, regardless of the ageing periods. The results showed that Solidex and Z100 had the highest compressive strength values. Ageing in water reduced the hardness for all composites, but had no long-term effect on the compressive strength.

Solid-state and solution structural study of acetylacetone-modified tin(IV) chloride used as a precursor of SnO2 nanoparticles prepared by a sol-gel route

The effect of addition of different amounts of acetylacetone (acacH) on the species formed at room temperature and after thermohydrolysis at 70 degreesC for 30 and 120 min of ethanolic SnCl4.5H(2)O solutions is followed by EXAFS spectroscopy at the Sn K-edge. We show that thermohydrolyzed solutions are a mixture of SnO2 nanoparticles and soluble tin polynuclear species. The complexation of the tin molecular precursors by acetylacetonate ligands is evidenced by H-1, C-13, and Sn-119 NMR spectroscopy and EXAFS for a acacH/Sn ratio higher than 2. Single crystals are isolated from solution and the structure, determined by X-ray diffraction, is built up from monomeric Cl-3(H2O)Sn(acac)-H2O units bridged together by hydrogen bonding. The acacH/Sn ratio in solution controls the polycondensation of the hydrolyzed species but not the crystallite size of the SnO2 nanoparticles (similar to2 nm). Because of the major presence of chelated tin mono- and dimeric complexes in solution for acacH/Sn > 2, the condensation is almost inhibited, meanwhile the decrease of amount of chelated complexes for the acacH/Sn < 2 gives rise to an increase of the number of nanoparticles.

Transport and sensors properties of nanostructured antimony-doped tin oxide films

Tin oxide thin films doped with 7 mol% antimony oxide multilayer were prepared by the polymeric precursor method. Morphological characterization revealed films with round-shaped grains, nanometric size (similar to 13 nm), and low roughness. These films display high transmittance (similar to 80%) in the visible range of transmittance spectra, which is desirable for transparent conductive oxide films. Analysis on electrical resistivity versus temperature data showed two different conduction mechanisms toward the temperature range. The gas sensor properties measurement of the thicker thin film revealed good sensibility for the NOx. (c) 2006 Elsevier B.V. All rights reserved.

Influence of ambient gas on the growth and properties of porous tin-doped indium oxide thin films made by pulsed laser deposition

The laser ablation method was used for depositing porous nanocrystalline indium-tin oxide thin films for gas sensing applications. Samples were prepared at different pressures using three gases (O-2, 0.8N(2):0.2O(2), N-2) and heat-treated in the same atmosphere used for the ablation process. X-ray diffraction results show that the films are not oriented and the grain sizes are in the range between 15 and 40 nm. The grains are round shaped for all samples and the porosity of the films increases with the deposition pressure. The degree of sintering after heat treatment increases for lower oxygen concentrations, generating fractures on the surface of the samples. Film thicknesses are in the range of I pm for all gases as determined from scanning electron microscopy cross-sections. Electrical resistance varies between 36.3 ohm for the film made at 10 Pa pressure in N-2 until 9.35 x 10(7) ohm for the film made at 100 Pa in O-2. (C) 2007 Elsevier 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.