Synthesis of KNbO3 nanostructures by a microwave assisted hydrothermal method

One-dimensional nanostructures of KNbO3 have attracted a great interest in the scientific community, mainly because of their promising application as nanoelectromechanical systems (NEMS). However, the synthesis of KNbO3 structures becomes complex due to the natural tendency to form non-stoichiometric potassium niobates. In this context, we report on the crystallization of one-dimensional KNbO3 nanostructures through the reaction between Nb2O5 and KOH under microwave-assisted hydrothermal synthesis (M-H). The use of this synthesis method made possible a very fast synthesis of singlecrystalline powders. Based on SEM, TEM and XRD characterizations, the influence of the synthesis time and the reactants concentration in the structure and morphology of the resultant KNbO3 was established. The conditions that favor the crystallization of nanofingers were determined to be small amounts of Nb2O5 and short reaction times. (C) 2008 Elsevier B.V. All rights reserved.

Structural characterization of phase transition of Al2O3 nanopowders obtained by polymeric precursor method

Nanocrystalline Al(2)O(3)powders have been synthesized by the polymeric precursor method. A study of the evolution of crystalline phases of obtained powders was accomplished through X-ray diffraction, micro-Raman spectroscopy and refinement of the structures through the Rietveld method. The results obtained allow the identification of three steps on the gamma-Al2O3 to alpha-Al2O3 phase transition. The single-phase alpha-Al2O3 Powder was obtained after heat-treatment at 1050 degrees C for 2 h. A study of the morphology of the particles was accomplished through measures of crystallite size, specific surface area and transmission electronic microscopy. The particle size is closely related to gamma-Al2O3 to alpha-Al2O3 phase transition. (c) 2007 Elsevier B.V. All rights reserved.

Structural changes of biocompatible neutral microemulsions stabilized by mixed surfactant containing soya phosphatidylcholine and their relationship with doxorubicin release

Depending on the composition, the mixture of surfactant, oil and water, may form supramolecular aggregates with different structures which can significantly influence the drug release. In this work several microemulsion (ME) systems containing soya phosphatidylcholine (SPC) and eumulgin HRE40 (TM) (EU) as surfactant, cholesterol (O) as oil phase, and ultra-pure water as an aqueous phase were studied. MEs with and without the antitumoral drug doxorubicin (DOX) were prepared. The microstructures of the systems were characterized by photon correlation spectroscopy, rheological behavior, polarized light microscopy, small-angle X-ray scattering (SAXS) and X-ray diffraction (XRD). The results reveal that the diameter of the oil droplets was dependent on the surfactant (S) amount added to formulations. The apparent viscosity was dependent on the O/S ratio. High O/S ratio leads to the crystallization of cholesterol polymorphs phases which restricts the mobility of the DOX molecules into the ME structure. Droplets with short-range spatial correlation were formed from the ME with the low O/S ratio. The increase of the cholesterol fraction in the O/S mixture leads to the formation of ordered structures with lamellar arrangements. These different structural organizations directly influenced the drug release profiles. The in vitro release assay showed that the increase of the O/S ratio in the formulations inhibited the constant rate of DOX release. Since the DOX release ratio was directly dependent on the ratio of O/S following an exponential decay profile, this feature can be used to control the DOX release from the ME formulations. (C) 2008 Elsevier B.V. All rights reserved.

Taxonomy of Ophiuroidea (Echinonermata) from the continental shelf and slope of the southern and southeastern Brazilian coast

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

Metanotal gland of the genus Eidmanacris (Grylloidea, Phalangopsidae): taxonomic importance

O presente trabalho compara a glândula metanotal de cinco espécies do gênero Eidmanacris por meio de microscopia eletrônica de varredura: E. corumbatai Garcia, 1998, E. alboannulata (Piza, 1960), E. dissimilis Desutter-Grandcolas, 1995, E. larvaeformis (Chopard, 1938) e Eidmanacris sp. A configuração externa da glândula foi determinada pela presença de duas projeções medianas que apresentam abertura em seu ápice e um grupo de cerdas abaixo destas projeções. Apesar de haver um padrão geral semelhante, a configuração da glândula é espécie-específica, que pode ser definida principalmente pela organização de cerdas e pela posição das projeções medianas. Nossos resultados sugerem a importância taxonômica desta estrutura, que deveria ser melhor analisada na descrição de espécies do gênero Eidmanacris. Pela observação do comportamento reprodutivo destas espécies, nós concluímos que a liberação da secreção desta glândula é importante para o sucesso reprodutivo.

A- and B-modes echobiometry in cataractous and noncataractous eyes of English Cocker Spaniel dogs

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

Antennal malformations in light ocelli drones of Apis mellifera (Hymenoptera, Apidae)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Multi-method Study on Aquatic Humic Substances from the Rio Negro - Amazonas State/Brazil: Emphasis on Molecular-Size Classification of their Metal Contents

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

Development and applications of three-dimensional gamma ray tomography system using ray casting volume rendering techniques

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

Phase-locking of superimposed diffractive gratings in photoresists

The superposition of optical interference patterns in a photoresist film can produce a rich variety of diffractive structures. In particular, a periodic non-sinusoidal surface relief profile can be synthesized by adding the Fourier components (sinusoidal gratings) of the desired profile. In order to control the shape of the grooves it is very important an accurate adjustment of the relative spatial shift between the recorded sinusoidal components. We describe the implementation of an opto-electronic feedback loop to select and lock such spatial shift at any desired position, thus allowing the synthesis of structures varying from symmetrical to asymmetrical relief profiles in a continuous range. To demonstrate the feasibility of the technique, the Fourier synthesis of two spatial harmonics is accomplished. The superposed sinusoidal gratings were recorded in positive photoresist films using a holographic setup operating at the line lambda = 457.9 run of an argon-ion laser. A detailed description of the procedure as well as the resulting profiles recorded in the photoresist is presented. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Evolution of rheological properties and local structure during gelation of siloxane-polymethylmethacrylate hybrid materials

Hybrid siloxane-polymethylmethacrylate (PMMA) nanocomposites with covalent bonds between the inorganic (siloxane) and organic (polymer) phases were prepared by the sot gel process through hydrolysis and polycondensation of 3-(trimethoxysilyl)propylmethacrylate (TMSM) and polymerization of methylmethacrylate (MMA) using benzoyl peroxide (BPO) as initiator. The effect of MMA, BPO and water contents on the viscoelastic behaviour of these materials was analysed during gelation by dynamic rheological measurements. The changes in storage (G') and loss moduli (G), complex viscosity (eta*) and phase angle (6) were measured as a function of the reaction time showing the viscous character of the sot in the initial step of gelation and its progressive transformation to an elastic gel. This study was complemented by Si-29 and C-13 solid-state nuclear magnetic resonance (NMR/MAS) measurements of dried gel. The analysis of the experimental results shows that linear chains are formed in the initial step of the gelation followed by a growth of branched structures and formation of a three-dimensional network. Near the gel point this hybrid material demonstrates the typical scaling behaviour expected from percolation theory.

Crystallographic studies on the binding of isonicotinyl-NAD adduct to wild-type and isoniazid resistant 2-trans-enoyl-ACP (CoA) reductase from Mycobacterium tuberculosis

The resumption of tuberculosis led to an increased need to understand the molecular mechanisms of drug action and drug resistance, which should provide significant insight into the development of newer compounds. Isoniazid (INH), the most prescribed drug to treat TB, inhibits an NADH-dependent enoyl-acyl carrier protein reductase (InhA) that provides precursors of mycolic acids, which are components of the mycobacterial cell wall. InhA is the major target of the mode of action of isoniazid. INH is a pro-drug that needs activation to form the inhibitory INH-NAD adduct. Missense mutations in the inhA structural gene have been identified in clinical isolates of Mycobacterium tuberculosis resistant to INH. To understand the mechanism of resistance to INH, we have solved the structure of two InhA mutants (121V and S94A), identified in INH-resistant clinical isolates, and compare them to INH-sensitive WT InhA structure in complex with the INH-NAD adduct. We also solved the structure of unliganded INH-resistant S94A protein, which is the first report on apo form of InhA. The salient features of these structures are discussed and should provide structural information to improve our understanding of the mechanism of action of, and resistance to, INH in M. tuberculosis. The unliganded structure of InhA allows identification of conformational changes upon ligand binding and should help structure-based drug design of more potent antimycobacterial agents. (c) 2007 Elsevier B.V. All rights reserved.

Computational studies of the reversible domain swapping of p13suc1

A minimalist representation of protein structures using a Go- like potential for interactions is implemented to investigate the mechanisms of the domain swapping of p13suc1, a protein that exists in two native conformations: a monomer and a domain- swapped dimer formed by the exchange of a beta- strand. Inspired by experimental studies which showed a similarity of the transition states for folding of the monomer and the dimer, in this study we justify this similarity in molecular descriptions. When intermediates are populated in the simulations, formation of a domain- swapped dimer initiates from the ensemble of unfolded monomers, given by the fact that the dimer formation occurs at the folding/ unfolding temperature of the monomer ( T-f). It is also shown that transitions, leading to a dimer, involve the presence of two intermediates, one of them has a dimeric form and the other is monomeric; the latter is much more populated than the former. However, at temperatures lower than T-f, the population of intermediates decreases. It is argued that the two folded forms may coexist in absence of intermediates at a temperature much lower than T-f. Computational simulations enable us to find a mechanism, `` lock- and- dock'', for domain swapping of p13suc1. To explore the route toward dimer formation, the folding of unstructured monomers must be retarded by first locking one of the free ends of each chain. Then, the other free termini could follow and dock at particular regions, where most intrachain contacts are formed, and thus de. ne the transition states of the dimer. The simulations also showed that a decrease in the maximum distance between monomers increased their stability, which is explained based on confinement arguments. Although the simulations are based on models extracted from the native structure of the monomer and the dimer of p13suc1, the mechanism of the domain- swapping process could be general, not only for p13suc1.

Quantitative structural analysis of the transition from LT-LixCoO2 to HT-LixCoO2 using the rietveld method: correlation between structure and electrochemical performance

A quantitative phase analysis was made of LiXCoO2 powders obtained by two distinct chemical methodologies at different temperatures (from 400 to 700degreesC). A phase analysis was made using Rietveld refinements based on X-ray diffraction data, considering the LiXCoO2 powders as a multiphase system that simultaneously contained two main phases with distinct, layered and spinel-type structures. The sults showed the coexistence of both structures in LiXCoO2 obtained at low temperature (400 and 500degreesC), although only the layered structure was detected at higher temperatures (600 and 700degreesC, regardless of the chemical powder process employed. The electrochemical performance, evaluated mainly by the cycling reversibility of LiXCoO2 in the form of cathode insertion electrodes, revealed that there is a close correlation between structural features and the electrochemical response, with one of the redox processes (3.3 v/3.9 v) associated only with the presence of the spinel-type structure. (C) 2003 Elsevier B.V. All rights reserved.

Role of the oriented attachment mechanism in the phase transformation of oxide nanocrystals

Bottom-up methods to obtain nanocrystals usually result in metastable phases, even in processes carried out at room temperature or under soft annealing conditions. However, stable phases, often associated with anisotropic shapes, are obtained in only a few special cases. In this paper we report on the synthesis of two well-studied oxides-titanium and zirconium oxide-in the nanometric range, by a novel route based on the decomposition of peroxide complexes of the two metals under hydrothermal soft conditions, obtaining metastable and stable phases in both cases through transformation. High-resolution transmission electron microscopy analysis reveals the existence of typical defects relating to growth by the oriented attachment mechanism in the stable crystals. The results suggest that the mechanism is associated to the phase transformation of these structures.