950 resultados para Micro-structural characterization


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A polymeric complex [Eu(α-tpc)3(α-Htpc) 2]n and its characterization by single crystal X-ray and thermal analysis, infrared and photoluminescence spectroscopies are described. The compound crystallizes in the monoclinic Cc space group. The asymmetric unit is formed from a europium ion bonded to one carboxyl oxygen of five different thiophene carboxylic moieties. Three of these moieties are deprotonated and bridge between neighboring europium ions giving rise to an infinite polymer along the c axis. Besides the europium characteristic emission lines, the emission spectra show unambiguously the crystal size effect on the 5D0 → 7F0 transition. The complex thermal decomposition at 220 C leads to a stable luminescent complex in which the 5D0 → 7F4 transition reveals a monomeric characteristic. The Judd-Ofelt intensity parameters to the polymeric and the monomeric compound with the same ligand and coordination number were compared. © 2013 Published by Elsevier Ltd.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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In this study, the physicochemical characteristics of calcium phosphate based bioactive ceramics of different compositions and blends presenting similar micro/nanoporosity and micrometer scale surface texture were characterized and evaluated in an in vivo model. Prior to the animal experiment, the porosity, surface area, particle size distribution, phase quantification, and dissolution of the materials tested were evaluated. The bone regenerative properties of the materials were evaluated using a rabbit calvaria model. After 2, 4, and 8 weeks, the animals were sacrificed and all samples were subjected to histologic observation and histomorphometric analysis. The material characterization showed that all materials tested presented variation in particle size, porosity and composition with different degrees of HA/TCP/lower stoichiometry phase ratios. Histologically, the calvarial defects presented temporal bone filling suggesting that all material groups were biocompatible and osteoconductive. Among the different materials tested, there were significant differences found in the amount of bone formation as a function of time. At 8 weeks, the micro/nanoporous material presenting similar to 55,TCP:45%,HA composition ratio presented higher amounts of new bone regeneration relative to other blends and a decrease in the amount of soft tissue infiltration. (C) 2014 Elsevier B.V. All rights reserved.

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In this paper, we report a detailed structural and electronic characterization of PbMoO4 crystals by using a conventional hydrothermal (CH) method. The samples were characterized by X-ray diffraction (XRD), Fourier transform Raman (FT-Raman), field-emission gun scanning electron microscopy (FEG-SEM) and photoluminescence (PL) measurements. In addition, first-principles quantum mechanical calculations based on the density functional theory were employed in order to understand the band structure and density of states for the PbMoO4. Analysis of both theoretical and experimental results allows to rationalize the role of order-disorder effects in the observed green PL emissions in these ordered powders.

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

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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Regeneration microsites are characterized by diverse combinations of attributes which assure the best conditions for seed germination and seedling establishment. By understanding these attributes, we can contribute to determining better management methodologies for reestablishing ecological process in sites under restoration. Thus, we sought to characterize and differentiate the micro-site conditions of restoration plantings to indentify likely physical-chemical limitations for the establishment of native tree species in the forest understory. This study was carried out in reforestation plantings with different ages (10, 22 and 55 years). The physical-chemical characterization of the micro-site of regeneration of the study areas was carried out by evaluating the soil compression level, porosity, humidity, organic matter and nutrients content and granulometry, as well as litter dry mass and canopy cover. An increase on the canopy cover and soil porosity, humidity, clay and organic matter content were observed in the oldest restored areas, as well as a decrease in soil compression. Thus, these findings demonstrated that the evaluated microsite properties are in process of restoration. Therefore, microsite conditions for seedling establishment become even more similar to reference ecosystems as restoration planting evolve.

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In this paper, we present a method to order low temperature (LT) self-assembled ferromagnetic In1-xMnxAs quantum dots (QDs) grown by molecular beam epitaxy (MBE). The ordered In1-xMnxAs QDs were grown on top of a non-magnetic In0.4Ga0.6As/GaAs(100) QDs multi-layered structure. The modulation of the chemical potential, due to the stacking, provides a nucleation center for the LT In1-xMnxAs QDs. For particular conditions, such as surface morphology and growth conditions, the In1-xMnxAs QDs align along lines like chains. This work also reports the characterization of QDs grown on plain GaAs(100) substrates, as well as of the ordered structures, as function of Mn content and growth temperature. The substitutional Mn incorporation in the InAs lattice and the conditions for obtaining coherent and incoherent structures are discussed from comparison between Raman spectroscopy and x-ray analysis. Ferromagnetic behavior was observed for all structures at 2K. We found that the magnetic moment axis changes from [110] in In1-xMnxAs over GaAs to [1-10] for the ordered In1-xMnxAs grown over GaAs template. (C) 2012 American Institute of Physics. [http://dx.doi.org/10.1063/1.4745904]

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Formation of oriented or aligned micro- and nanofibers using biocompatible materials opens the possibility to obtain engineered tissues that can be used in medicine, environmental engineering, security and defense, among other applications. Pectin, a heteropolysaccharide, is a promising material to be incorporated into the fibers because, besides being biocompatible, this material is also biodegradable and bioactive. In this work, the formation of oriented fibers using solutions containing pectin and polyethylene oxide (biocompatible polymers), and chloroform (as the solvent) is investigated. The injection of solution into an intense electric field defined between two parallel electrodes was used to obtain oriented fibers. This novel approach is a modification of the conventional electrospinning process. The presence of pectin in the fibers was confirmed by FTIR analysis. Fibers with diameters of hundreds of nanometers and several centimeters long can be collected. The incorporation of pectin leads to a higher variation of the diameter of the fibers, and a trend to larger fiber diameters. This behavior can be related to the presence of pectin clusters in the fibers. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.057203jes] All rights reserved.

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This paper reports on the synthesis (chemical co-precipitation reaction) and characterization (X-ray diffraction, magnetization, and electron paramagnetic resonance) of nanosized Cd1-xMnxS particles with manganese concentration up to x = 0.73. Though the literature reports that nanosized (bulk) CdS can incorporate as much as 30% (50%) of manganese ion within its crystal structure we found manganese segregation at the nanoparticle surface at doping levels as low as 14%. We found that both XRD and magnetization data support the presence of the Mn3O4 phase (observed spin-glass transition around 43 K) at the high manganese doping levels whereas the EPR data strongly suggest preferential incorporation of manganese at the nanoparticle's surface, even at low manganese doping levels. Analyses of the experimental data strongly suggest the preparation of well-defined core/shell (Cd1-xMnxS/Mn3O4) structures at higher levels of manganese doping.

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Six new lanthanide complexes of stoichiometric formula (C)(2)[Ln(Pic)(5)]-where (C) is a imidazolium cation coming from the ionic liquids 1-butyl-3-methylimidazolium picrate (BMIm-Pic), 1-butyl-3-ethylimidazolium picrate (BEIm-Pic), and 1,3-dibutylimidazolium picrate (BBIm-Pic), and Ln is Eu(III) or Gd(III) ions-have been prepared and characterized. To the best of our knowledge, these are the first cases of Ln(III) pentakis(picrate) complexes. The crystal structures of (BEIm)(2)[Eu(Pic)(5)] and (BBIm)(2)[Eu(Pic)(5)] compounds were determined by single-crystal X-ray diffraction. The [Eu(Pic)(5)](2-) polyhedra have nine oxygen atoms coordinated to the Eu(III) ion, four oxygen atoms from bidentate picrate, and one oxygen atom from monodentate picrate. The structures of the Eu complexes were also calculated using the sparkle model for lanthanide complexes, allowing an analysis of intramolecular energy transfer processes in the coordination compounds. The photoluminescence properties of the Eu(III) complexes were then studied experimentally and theoretically, leading to a rationalization of their emission quantum yields.

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An octahedral Zn complex with o-phenanthroline (o-phen) and cyanoguanidine (cnge) has been synthesized and characterized. The crystal structural data show the formation of a ZnN5O core where the metal coordinates to two mutually perpendicular o-phenanthrolines as bidentate ligands [Zn-N bond lengths in the 2.124(2)-2.193(2) angstrom range], the cyanide nitrogen of a cnge [d(Zn-N) = 2.092(2) angstrom, angle(Zn-N-C) = 161.1(2)degrees], and a water molecule [d(Zn-Ow) = 2.112(2) angstrom]. Spectral data (FT-IR, Raman, and fluorescence) and speciation studies are in agreement with the structure found in the solid state and the one proposed to exist in the solution. To evaluate the changes in the microbiological activity of Zn, antibacterial studies were carried out by observing the changes in minimum inhibitory concentration of the complex, the ligands, and the metal against five different bacterial strains. The antibacterial activity of Zn improved upon complexation in three of the tested strains.

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In this work, CaTiO3:Sm (CT:Sm) were prepared by a soft chemical processing at different annealing temperatures starting with a disordered structure and reaching an ordered one, with the propose to understand the relationship between structural order-disorder and photoluminescence emission. The samples were characterized by titanium K-edge, Titanium L-II and L-III-edge XANES, electron paramagnetic resonance (EPR) and photoluminescence (PL) measurements. XANES results clearly point the presence of local distortion in [TiO6] octahedral clusters until the crystallization was completed. The interactions of the network clusters that form the CT:Sm structures provides favorable structural and electronic conditions for the appearance of PL phenomena. (C) 2012 Published by Elsevier B.V.