In situ and simultaneous nanostructural and spectroscopic studies of ZnO nanoparticle and Zn-HDS formations from hydrolysis of ethanolic zinc acetate solutions induced by water

The simultaneous formation of nanometer sized zinc oxide (ZnO), and acetate zinc hydroxide double salt (Zn-HDS) is described. These phases, obtained using the sol-gel synthesis route based on zinc acetate salt in alcoholic media, were identified by direct characterization of the reaction products in solution using complementary techniques: nephelometry, in situ Small-Angle X-ray Scattering (SAXS), UV-Vis spectroscopy and Extended X-ray Absorption Fine Structures (EXAFS). In particular, the hydrolytic pathway of ethanolic zinc acetate precursor solutions promoted by addition of water with the molar ratio N = [H2O]/[Zn2+] = 0.05 was investigated in this paper. The aim was to understand the formation mechanism of ZnO colloidal suspension and to reveal the factors responsible for the formation of Zn-HDS in the final precipitates. The growth mechanism of ZnO nanoparticles is based on primary particle (radius approximate to 1.5 nm) rotation inside the primary aggregate (radius < 3.5 nm) giving rise to an epitaxial attachment of particles and then subsequent coalescence. The growth of second ZnO aggregates is not associated with the Otswald ripening, and could be associated with changes in equilibrium between solute species induced by the superficial etching of Zn-HDS particles at the advanced stage of kinetic.

Influência dos dopantes potássio e lítio na cerâmica relaxora niobato de chumbo e magnésio (PMN)

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

Estudo da distribuição de tamanho e composição iônica de aerossóis e seus efeitos na capacidade de nuclear gotas de nuvens

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influence of seed particle frequency on the phase formation and on the microstructure of 0.88 PZN-0.07 BT-0.05 PT ceramic

The Pechini method as well as the simultaneous addition of seeds particles and dopant solutions of BaTiO3 (BT) and PbTiO3 (PT) were used to prepare the perovskite phase 0.88 PZN-0.07 BT-0.05 PT. To study the influence of seed particle frequency on the synthesis of the PZN ceramic, two ranges of seed particle size were used: the range from 30 to 100 nm, termed small seed particles (frequency of 10(15) particles/cm(3)); and the range from 100 to 900 nm, termed large seed particles (frequency of 10(13) particles/cm(3)). The crystalline nuclei size influenced the calcining process, the sintering process and the microstructure. Samples prepared with lower seed frequency displayed more amount of pyroclore phase, need higher temperatures for sintering and showed a more heterogeneous microstructure with poor dielectric properties. (C) 2000 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

Photoluminescence of SrTiO3: Influence of Particle Size and Morphology

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

SPH simulations of clumps formation by dissipative collisions of molecular clouds - II. Magnetic case

We performed computer simulations of interstellar cloud-cloud collisions using the three-dimensional smoothed particle magnetohydrodynamics method. In order to study the role of the magnetic field on the process of collision-triggered fragmentation, we focused our attention on head-on supersonic collisions between two identical spherical molecular-clouds. Two extreme configurations of the magnetic field were adopted: parallel and perpendicular to the initial clouds motion. The initial magnetic field strength was approximately 12.0 muG. In the parallel case, much more of the collision debris were retained in the shocking region than in the non-magnetic case where gas escaped freely throughout the symmetry plane. Differently from the non-magnetic case, eddy-like vortices were formed. The regions of highest vorticity and the the regions of highest density are offset. We found clumps formation only in the parallel case, however, they were larger, hotter and less dense than in the analogous non-magnetic case. In the perpendicular case, the compressed field works as a magnetic wall, preventing a stronger compression of the colliding clouds. This last effect inhibits direct contact of the two clouds. In both cases, we found that the field lines show a chaotic aspect in large scales. Also, the field magnitude is considerably amplified in the shock layer. However, the field distribution is almost coherent in the higher density regions.

SPH simulations of clumps formation by dissipative collision of molecular clouds - I. Non magnetic case

Computer experiments of interstellar cloud collisions were performed with a new smoothed-particle-hydrodynamics (SPH) code. The SPH quantities were calculated by using spatially adaptive smoothing lengths and the SPH fluid equations of motion were solved by means of a hierarchical multiple time-scale leapfrog. Such a combination of methods allows the code to deal with a large range of hydrodynamic quantities. A careful treatment of gas cooling by H, H(2), CO and H II, as well as a heating mechanism by cosmic rays and by H(2) production on grains surface, were also included in the code. The gas model reproduces approximately the typical environment of dark molecular clouds. The experiments were performed by impinging two dynamically identical spherical clouds onto each other with a relative velocity of 10 km s(-1) but with a different impact parameter for each case. Each object has an initial density profile obeying an r(-1)-law with a cutoff radius of 10 pc and with an initial temperature of 20 K. As a main result, cloud-cloud collision triggers fragmentation but in expense of a large amount of energy dissipated, which occurred in the head-on case only. Off-center collision did not allow remnants to fragment along the considered time (similar to 6 Myr). However, it dissipated a considerable amount of orbital energy. Structures as small as 0.1 pc, with densities of similar to 10(4) cm(-3), were observed in the more energetic collision.

Formation Mechanism via a Heterocoagulation Approach of FePt Nanoparticles Using the Modified Polyol Process

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

Mechanically activating formation of layered structured bismuth titanate

Bismuth titanatc-Bi(4)Ti(3)O(12) (BIT) with wide application in the electronic industry as capacitors, memory devices and sensors is the simplest compound in the Aurivillius family, which consists of (Bi(2)O(2))(2+) sheets alternating with (Bi(2)T(i)3O(10))(2-) perovskite-like layers. The synthesis of more resistive BIT ceramics would be preferable advance in obtaining of well-densified ceramic with small grains randomly oriented to limit the conductivity along the (Bi(2)O(2))(2+) layers. Having in mind that the conventional ceramic route for the synthesis can lead to non-stoichiometry in composition, in consequence of the undesirable loss in bismuth content through volatilization of Bi(2)O(3) at elevated temperature, our efforts were addressed to preparation of BIT by mechanical activation the constituent oxides. The nucleation and phase formation of BIT, crystal structure, microstructure, powder particle size and specific surface area were followed by XRD, Rietveld refinement analysis, thermal analysis, scanning electron microscopy (SEM) and the BET specific surface area measurements. (c) 2005 Elsevier B.V. All rights reserved.

Study of potassium additive on the phase formation and ferroelectric properties of 0.9PMN-0.1PT ceramics

A recent and innovative method to include Ti into the columbite precursor has permitted to synthesize 0.9PMN-0.1PT powders with high homogeneity. The present work describes this methodology, named modified columbite method, showing that the reaction between MN(T)and PbO at 800 degrees C for 2 h results in perovskite single-phase. The crystal structure alterations in the columbite and perovskite phases obtained by this methodology and the effects of potassium doping were investigated by the Rietveld method. Changes in the powder morphology, density and weight loss during the sintering process were also studied. Conclusively, potassium does not affect significantly the perovskite amount, but reduces the particle and grain sizes. This dopant also changes the relaxor behavior of 0.9PMN-0.1 PT ceramic, reducing the dielectric loss and enhancing the diffuseness of the phase transition. (C) 2005 Published by Elsevier Ltd and Techna Gronp S.r.l.

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.

Tin oxide nanoparticle formation using a surface modifying agent

This work presents results concerning the preparation of redispersible tin oxide nanoparticles achieved by using Tiron molecule ((OH)(2)C(6)H(2) (SO(3)Na)(2)) as surface modifying agent. The adsorption isotherm measurements show that an amount of 10 wt.% of Tiron is need to recover the SnO(2) nanoparticles surface with a monolayer. These nanoparticles can be easily redispersed in tetramethyl ammonium hydroxide at pH greater than or equal to11 until a powder concentration of 12 vol.% of tin. Under these conditions, hydrodynamic particle size is about 7 nm and increases until 52 nm at pH 6 due to the aggregation phenomenon. The time evolution of the viscoelastic properties indicates that the suspensions at pH 12.5, containing 12 vol.% tin oxide and 10 wt.% of surface modifier are kinetically stable. After thermal treatment at different temperature the powder characterisation evidences that the presence of Tiron monolayer at the nanoparticles surface increases the thermal stability of the porous texture and prevent the micropore size growth. This set of results contributes to satisfy the demand for more controlled synthesis of nanoparticles with high thermal stability as required for fabrication of ultrafiltration ceramic membranes. (C) 2004 Elsevier Ltd. All rights reserved.

Jarosite pseudomorph formation from arsenopyrite oxidation using Acidithiobacillus ferrooxidans

In this work, the oxidizing action of a native strain type A. ferrooxidans on a sulphide containing a predominance of arsenopyrite and pyrite has been evaluated. Incubation of the A. ferrooxidans strain in flasks containing 200 mL of T&K medium with the ore (particle size of 106 mu m) at pulp density 8% (w/v) at 35 degrees C on a rotary shaker at 200 rpm resulted in preferential oxidation of the arsenopyrite and the mobilization of 88% of the arsenic in 25 days. Mineralogical characterization of the residue after biooxidation was carried out with FTIR. XRD and SEM/XEDS techniques. An in situ oxidation of the arsenopyrite is suggested on the basis of the frequent appearance of jarosite pseudomorph replacing arsenopyrite, in which the transformations Fe(2+) -> Fe(3+), S(-2) -> S(+6) and As(-1) -> As(+3) -> As(+5) occur for the most part without formation of soluble intermediates, resulting in a type of jarosite that typically contains high concentrations of arsenic (type A-jarosite). However, during pyrite oxidation, dissolution of the constituent Fe and S predominates, which is evidenced by corrosion of pyrite particles with formation of pits, generating a type of jarosite with high quantities of K (type B-jarosite). Lastly, a third type of jarosite (type C-jarosite) also precipitated forming a thin film that covered the grains of pyrite principally. (C) 2010 Elsevier B.V. All rights reserved.

Formation of beta-nickel hydroxide plate-like structures under mild conditions and their optical properties

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Formation of colloidal particles of hydrous iron oxide by forced hydrolysis

The mechanism of formation and growth of hydrous iron oxide (FeOOH) during the initial stages of forced hydrolyses of ferric chloride aqueous solution was studied by small angle X-ray scattering (SAXS). The effect of the hydrolysis temperature (60°C, 70°C and 80°C) and of the addition of urea on the formation of colloidal particles under isothermal conditions were investigated. Based on the experimental scattering functions in the Guinier range, we suggest the presence of elongated colloidal particles. The particle diameter and length, and their variation with time, were determined by fitting the form factor of prolate ellipsoids to the experimental scattering functions. We have assumed that our solutions are in a dilute state and that all colloidal particles are approximately of the same size. The colloidal particles have geometrical shapes similar to those of the subcrystals that build up the superstructure of β-FeOOH crystals, indicating that the formation of this hydrous iron oxide is governed by an aggregation process. Otherwise, the addition of urea hinders the growth and yields smaller particles, with a reduction in size greater than 50%. © 2000 Elsevier Science B.V. All rights reserved.