935 resultados para Metal complexes. Characterization. Synthesis
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In this work Ba0.99Eu0.01MoO4 (BEMO) powders were prepared by the first time by the Complex Polymerization Method. The structural and optical properties of the BEMO powders were characterized by Fourier Transform Infra-Red (FTIR), X-ray Diffraction (XRD), Raman Spectra, High-Resolution Scanning Electron Microscopy (HR-SEM) and Photoluminescent Measurements. XRD show a crystalline scheelite-type phase after the heat treatment at temperatures greater than 400 degrees C. The ionic radius of Eu3+ (0.109 nm) is lower than the Ba2+ (0.149 nm) one. This difference is responsible for the decrease in the lattice parameters of the BEMO compared to the pure BaMoO4 matrix. This little difference in the lattice parameters show that Eu3+ is expected to occupy the Ba2+ site at different temperatures, stayed the tetragonal (S-4) symmetry characteristic of scheelite-type crystalline structures of BaMoO4. The emission spectra of the samples, when excited at 394 nm, presented the D-5(1)-> F-7(0, 1 and 2) and D-5(0)-> F-7(0, 1, 2, 3 and 4) Eu3+ transitions at 523, 533, 554, 578, 589, 614, 652 and 699 nm, respectively. The emission spectra of the powders heat-treated at 800 and 900 degrees C showed a marked increase in its intensities compared to the materials heat-treated from 400 to 700 C. The decay times for the sample were evaluated and all of them presented the average value of 0.61 ms. Eu3+ luminescence decay time follows one exponential curve indicating the presence of only one type of Eu3+ symmetry site.
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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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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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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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In this study, microcrystalline cellulose (MCC) was prepared from the acid hydrolysis of bacterial cellulose (BC) produced in culture medium of static Acetobacter xylinum. The MCC-BC produced an average particle size between 70 and 90 mu m and a degree of polymerization (DP) of 250. The characterization of samples was performed by thermogravimetric analysis, X-ray diffraction, and scanning electron microscopy (SEM). The MCC shows a lower thermal stability than the pristine cellulose, which was expected due to the decrease in the DP during the hydrolysis process. In addition, from X-ray diffractograms, we observed a change in the crystalline structure. The images of SEM for the BC and MCC show clear differences with modifications of BC fiber structure and production of particles with characteristics similar to commercial MCC.
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Palladium(II) coordination compounds of general formula trans-[PdX(2)(isn)(2)], X = Cl(-) (1), N(3) (-) (2), SCN(-) (3), NCO(-) (4), isn = isonicotinamide; were synthesized and characterized in solid state by elemental analysis, infrared spectroscopy, and simultaneous TG-DTA. TG experiments reveal that the compounds 1-4 undergo thermal decomposition in three or four stages, yielding Pd(0) as final residue, according to calculus and identification by X-ray powder diffraction.
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The synthesis and thermal behavior of the new [Pd(fum)(bipy)] (n) center dot 2nH(2)O (1), [Pd(fum)(bpe)] (n) center dot nH(2)O (2) and [Pd(fum)(pz)] (n) center dot 3nH(2)O (3) {bipy = 4,4'-bipyridine, bpe = 1,2-bis(4-pyridyl)ethene and pz = pyrazine} fumarate complexes are described in this work as well their characterization by IR and (13)C CPMAS NMR spectroscopies. TG curves showed that the compounds released organic ligands and lattice water molecules in the temperature range of 46-491 A degrees C. In all the cases, metallic palladium was identified as the final residue.
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The synthesis and characterization of a new organic ligand monooctyldiphenylphosphinate (L) is described, as well as a new Eu(3+) diketonate complex [Eu(tta)(3)(L)(2)] (tta = thenoyltrifluoracetone). The ligand (L) was formed by substitution reaction (80% yield) and characterized by uni- and bidimensional (1)H, (13)C and (31)P NMR experiments, to confirm its molecular structure. The coordination of (L) to Eu(3+) in the complex [Eu(tta)(3)(L)(2)] was confirmed by FT-IR spectra. The emission spectra present the same profile when excited in Eu(3+) or in the ligands, suggesting an energy transfer from ligands to Eu(3+) ions. The emission spectra of the precursor [Eu(tta)(3)(H(2)O)(2)], and [Eu(tta)(3)(L(2))] present bands arising from f-f intra-configurational transitions. The only (5)D(0)-(7)F(0) transition shows the presence of at least one site without symmetry center. The FWHM of such transition is 7 cm(-1) and 57 cm(-1) for [Eu(tta)(3)(H(2)O)(2)] and [Eu(tta)(3)(L)(2)] complexes, respectively. This widening is provided by the presence of large groups around Eu(3+) ion. The calculated intensity parameters Omega(2) and Omega(4) show that the interaction features between center-ion and ligand are different; the small value of Omega(4) is related to long range effects of alkyl chain. The Langmuir isotherms of this ligand and complex have been investigated although their hydrolysis in water subphase does not allow stable monolayers. (C) 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Highly crystalline ZnO and Ga-modified zinc oxide (ZnO:Ga) nanoparticles containing 1, 3 and 5 atom% of Ga3+ were prepared by precipitation method at low temperature. The films were characterized by XRD, BET, XPS and SEM. No evidence of zinc gallate formation (ZnGa2O4), even in the samples containing 5 atom% of gallium, was detected by XRD. XPS data revealed that Ga is present into the ZnO matrix as Ga3+, according to the characteristic binding energies. The particle size decreased as the gallium level was increased as observed by SEM, which might be related to a faster hydrolysis reaction rate. The smaller particle size provided films with higher porosity and surface area, enabling a higher dye loading. When these films were applied to dye-sensitized solar cells (DSSCs) as photoelectrodes, the device based on ZnO: Ga 5 atom% presented an overall conversion efficiency of 6% (at 10 mW cm(-2)), a three-fold increase compared to the ZnO-based DSSCs under the same conditions. To our knowledge, this is one of the highest efficiencies reported so far for ZnO-based DSSCs. Transient absorption (TAS) study of the photoinduced dynamics of dye-sensitized ZnO:Ga films showed that the higher the gallium content, the higher the amount of dye cation formed, while no significant change on the recombination dynamics was observed. The study indicates that Ga-modification of nanocrystalline ZnO leads to an improvement of photocurrent and overall efficiency in the corresponding device.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)