Efficiency and purity control in the preparation of pure and/or aluminum-doped barium ferrites by hydrothermal methods using ferrous ions as reactants

The synthesis of hexagonal barium ferrite (BaFe12O19) was studied under hydrothermal conditions by a method in which a significant amount of ferrous chloride was introduced along side ferric chloride among the starting materials. Though all of the Fe2+ ions in the starting material were converted to Fe3+ ions in the final product, Fe2+ was confirmed to participate differently from the Fe3+ used in the conventional method in the mechanism of forming barium ferrite. Indeed the efficiency of the synthesis and the quality of the product and the lack of impurities such as Fe2O3 and BaFe2O4 were improved when Fe2+ was included. However, the amount of ferrous ions that could be included to obtain the desired product was limited with an optimum ratio of 2:8 for FeCl2/FeCl3 when only 2h of reaction time were needed. It was also found that the role of trivalent Fe3+ could be successfully replaced by Al3+. Up to 50% of their on could be replaced by Al3+ in the reactants to produce Al- doped products. It was also found that the ratio of Fe2+/M3+ could be increased in the presence of Al3+ to produce high quality barium ferrite.

Investigation by Combined Solid-State NMR and SAXS Methods of the Morphology and Domain Size in Polystyrene-b-Polyethylene Oxide-b-Polystyrene Triblock Copolymers

The microphase structure of a series of polystyrene-b-polyethylene oxide-b-polystyrene (SEOS) triblock copolymers with different compositions and molecular weights has been studied by solid-state NMR, DSC, wide and small angle X-ray scattering (WAXS and SAXS). WAXS and DSC measurements were used to detect the presence of crystalline domains of polyethyleneoxide (PEO) blocks at room temperature as a function of the copolymer chemical composition. Furthermore, DSC experiments allowed the determination of the melting temperatures of the crystalline part of the PEO blocks. SAXS measurements, performed above and below the melting temperature of the PEO blocks, revealed the formation of periodic structures, but the absence or the weakness of high order reflections peaks did not allow a clear assessment of the morphological structure of the copolymers. This information was inferred by combining the results obtained by SAXS and (1)H NMR spin diffusion experiments, which also provided an estimation of the size of the dispersed phases of the nanostructured copolymers. (C) 2009 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48:55-64,2010

Chromic oxide as a digestibility marker for dogs - A comparison of methods of analysis

The study reported compared coefficients of apparent digestibility (CAD) obtained by total collection (TC) and by chromic oxide (Cr2O3) determined by visible absorption spectrometry (VIS) and flame atomic absorption spectrophotometry (FAAS). These quantification methods were also investigated to assess their precision. Nineteen adult dogs housed in individual digestibility cages were fed three commercial diets, each test including five or seven animals. The experiment was carried out in a completely randomized design with three among-subjects factors (foods) and three within-subject factors (methods), and the dogs were the experimental unit. Estimated CAD for all dietary components in the three diets by either chromium quantification methods did not differ and showed fair agreement with TC results (P > 0.05). Coefficients of chromic oxide recoveries in feces were 1.06 +/- 0.044 and 1.01 +/- 0.045 for VIS and FAAS, respectively, values significantly different (P < 0.05), indicating better recovery for FAAS. Significant differences (P<0.05) were found in the mean concentration of Cr2O3 for diets and feces (17 +/- 0.6 and 19 +/- 0.8g/kg for VIS and FAAS, respectively). Coefficient of variation for FAAS was 1.69% and 1.77% for VIS, which did not differ significantly (P > 0.05). Pearson's correlation coefficient (r=0.99; P < 0.01) indicated positive and significant association among the results for VIS and FASS, indicating reasonable precision and agreement of chromic oxide contents determined by these methods. Therefore, FAAS and VIS can be used successfully to determine Cr2O3 in dog foods and feces. (c) 2006 Elsevier B.V. All rights reserved.

Preparation and characterization of cellulose/hydrous niobium oxide hybrid

A composite of cellulose extracted from bagasse with Nb2O5 center dot nH(2)O in three different proportions (16.67, 37.5 and 50.0 wt%) was prepared using the co-precipitation method. The materials were characterized by X-ray diffractometry (XRD), Fourier transform infra-red spectroscopy (FTIR), thermogravimetric analysis (TG/DTG), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). TG data obtained show that the presence of inorganic material influenced slightly the stability of the hybrid material. The precipitation of 16.67 wt.% of oxide was sufficient to inhibit the combustion peaks present in the DSC curve of cellulose. This work will help find new applications for these materials. Published by Elsevier Ltd.

Effect of temperature on the interaction between the nonionic surfactant C(12)E(5) and poly(ethylene oxide) investigated by dynamic light scattering and fluorescence methods

The interaction between the nonionic surfactant C(12)E(5) and a high molar mass (M = 5.94 x 10(5)) poly(ethylene oxide) (PEG) in aqueous solution has been examined as a function of temperature by dynamic light scattering and fluorescence methods over a broad concentration range. Clusters of small surfactant micelles form within the PEO coil, leading to its extension. The hydrodynamic radius of the complex increases strongly with temperature as well as with the concentrations of surfactant and polymer. At high concentrations of the surfactant, the coil/micellar cluster complex coexists with free C(12)E(5) micelles in the solution. Fluorescence quenching measurements show a moderate micellar growth from 155 to 203 monomers in PEO-free solutions of C(12)E(5) over a wide concentration range (0.02-2.5%) at 8 degrees C. Below 0.25% C(12)E(5), the average aggregation number (N) of the micelles is smaller in the presence of PEO than in its absence. However, N increases with increasing surfactant concentration up to a plateau value of about 270 at about 1.2% (ca. 30 mM) C(12)E(5). At high surfactant concentrations, N is larger in the presence of polymer than in its absence, a finding which is connected to a significant lowering of the clouding temperature due to the PEO at these compositions. Similar results of increasing aggregation number followed by a plateau were also found at a fixed concentration of surfactant (2.5%) and varied PEO.

Electroluminescence of zinc oxide thin-films prepared via polymeric precursor and via sol-gel methods

Zinc oxide (ZnO) is an electroluminescent (EL) material that can emit light in different regions of electromagnetic spectrum when electrically excited. Since ZnO is chemically stable, inexpensive and environmentally friendly material, its EL property can be useful to construct solid-state lamps for illumination or as UV emitter. We present here two wet chemical methods to prepare ZnO thin-films: the Pechini method and the sol-gel method, with both methods resulting in crystalline and transparent films with transmittance > 85% at 550 nm. These films were used to make thin-film electroluminescent devices (TFELD) using two different insulator layers: lithium fluoride (LiF) or silica (SiO2). All the devices exhibit at least two wide emission bands in the visible range centered at 420 nm and at 380 nm attributed to the electronic defects in the ZnO optical band gap. Besides these two bands, the device using SiO2 and ZnO film obtained via sol-gel exhibits an additional band in the UV range centered at 350 nm which can be attributed to excitonic emission. These emission bands of ZnO can transfer their energy when a proper dopant is present. For the devices produced the voltage-current characteristics were measured in a specific range of applied voltage. (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.

PREPARATION AND CHARACTERIZATION OF TI(IV) OXIDE GRAFTED ONTO SILICA ON A SILICA-GEL SURFACE

Silica gel with a surface area of 500 m2g-1 and an average pore diameter of 60 angstrom was chemically modified with Ti(IV) oxide using the grafting method. The amount of metal oxide attached to the surface was 1.8.10(-3) mol g-1. The X-ray photoelectron spectra showed that the metal ion species on the surface are Ti(IV) in TiO2 and MTiO3 (M = Ca2+, Sr2+, Ba2+ and Pb2+), i.e. they have the binding energy of Ti2p3/2 = 458.7 eV. The dehydration of the solid at higher temperature increased the O(II)/Ti (O(II) = oxygen bound to titanium atom) ratio, presumably due to a reticulation of the hydrous Ti(IV) oxide on the silica surface at higher temperatures. Migration of Ti(IV) into the silica gel matrix was observed but the specific surface area was not significantly changed.

SrTiO3 preparation through coprecipitation methods

Precursor powders to obtain SrTiO3 were prepared by using 8-hydroxyquinoline precipitant agent. The residues from the thermal decomposition, followed by TG/DTG/DTA, were characterized by XRD and it could be verified that the mixed oxides could be obtained varying the thermal decomposition conditions like atmosphere and heating rate. However, the morphology and crystallinity of these residues is highly affected by such variations. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Development of metal oxide nanoparticles by soft chemical method

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

Preparation and characterization of ceria nanospheres by microwave-hydrothermal method

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.

Interaction of the nonionic surfactant C12E8 with high molar mass poly(ethylene oxide) studied by dynamic light scattering and fluorescence quenching methods

Dynamic light scattering has been used to investigate ternary aqueous solutions of n-dodecyl octaoxyethylene glycol monoetber (C12E8) with high molar mass poly(ethylene oxide) (PEO). The measurements were made at 20 °C, always below the cloud point temperature (Tc) of the mixed solutions. The relaxation time distributions are bimodal at higher PEO and surfactant concentrations, owing to the preacute of free surfactant micelles, which coexist with the slower component, representing the polymer coil/micellar cluster comptex. As the surfactant concentration is increased, the apparent hydrodynamic radius (RH) of the coil becomes progressively larger. It is suggested that the complex structure consists of clusters of micelles sited within the polymer coil, as previously concluded for the PEO-C12E8-water system. However. C12E8 interacts less strongly than C12E8 with PEO; at low concentrations of surfactant the complex does not contribute significantly to the total scattered intensity. The perturbation of the PEO coil radius with C12E8 is also smaller than that in the C12E8 system. The addition of PEO strongly decreases the clouding temperature of the system, as previously observed for C12E8/PEO mixtures in solution Addition of PEO up to 0.2% to C12E8 (10 wt %) solutions doss not alter the aggregation number (Nagg) of the micelles probably because the surfactant monomers are equally partitioned as bound and unbound micelles. The critical micelle concentration (cmc), obtained from the I1/I3 ratio (a measure of the dependence of the vibronic band intensities on the pyrene probe environment), does not change when PEO is added, suggesting that for neutral polymer/surfactant systems the trends in Nagg and the cmc do not unambiguously reflect the strength of interaction.

Use of nicarbazin, salinomycin and zinc oxide as alternative molting methods for commercial laying hens

An experiment was carried out to evaluate the performance, egg quality and morphometry of the reproductive tract, liver, pancreas and tongue of laying hens submitted to different molting methods. Two hundred and eighty eight 72-week-old Isa brown layers were distributed according to a completely randomized design with six treatments (molting methods) and six replicates of eight birds each. Layers were fed diets containing 3000 ppm zinc oxide, 60 ppm or 120 ppm nicarbazin, 30 ppm or 60 ppm salinomycin, or were submitted to feed fasting. Data were submitted to analysis of variance and means were compared by the test of Tukey at 5% probability level. Molting methods alternative to feed fasting were effective to induce molting in layer and provided good performance results in the second laying cycle.