943 resultados para Pechini method and chromium


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Molybdenum trioxide nanobelts and prism-like particles with good crystallinity and high surface areas have been prepared by a facile hydrothermal method, and the morphology could be controlled by using different inorganic salts, such as KNO3, Ca(NO3)(2), La(NO3)(3), etc. The possible growth mechanism of molybdenum trioxide prism-like particles is discussed on the basis of the presence of HI and the modification of metal cations. The as-prepared nanomaterials are characterized by means of powder X-ray diffraction (PXRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transformation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and ultraviolet and visible spectroscopy (UV-vis). TEM and HRTEM micrographs show that the molybdenum trioxide nanobelts and prism-like particles have a relatively high degree of crystallinity and uniformity. BET specific surface areas of the as-prepared molybdenum trioxide nanocrystals are 67-79 m(2)g(-1). XPS analysis indicates that the hexavalent molybdenum is predominant in the nanocrystals. UV-vis spectra reveal that the direct band gap energy of the annealed molybdenum trioxide prism-like particles shows a pronounced blue shift compared to that of bulk MoO3 powder.

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An effective electrogenerated chemiluminescence (ECL) sensor was developed by coimmobilization of the Ru(bpy)(2)(3+)-doped silica (RuDS) nanoparticles and carbon nanotubes (CNTs) on glassy carbon electrode through hydrophobic interaction. The uniform RuDS nanoparticles were prepared by a water-in-oil (W/O) microemulsion method and Ru(bpy)(3)(2+) doped inside could still maintain its high ECL efficiency. With such unique immobilization method, a great deal of Ru(bpy)(3)(2+) was immobilized three-dimensionally on the electrode , which could greatly enhance the ECL response and result in the increased sensitivity. On the other hand, CNTs played dual roles as matrix to immobilize RuDS nanoparticles and promoter to accelerate the electron transfer between Ru(bpy)(3)(2+) and the electrode. The as-prepared ECL sensor displayed good sensitivity and stability.

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Mercaptoethane sulfonate protected, water-soluble gold and silver nanoparticles (Au-MES and Ag-MES) are synthesized by one-phase method and characterized by TEM, TGA and XPS techniques, UV-vis and FTIR spectra. Both Au-MES and Ag-MES nanoparticles are soluble in the water up to 2.0 mg/ml and the stability of AU-MES is much better than that of Ag-MES. When dissolved in the water. they behave like a polyanion and can be used to build multilayer films with polyaniline (PANI) by way of layer-by-layer. A new approach is presented to fabricate the Multilayer films of Au-MES/PANI and Ag-MES/PAN]. The assembly mechanism of these multilayer films is also discussed. We anticipate highly conducting PANI films can be obtained by doping with these nanoparticles.

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Mg-8Gd-0.6Zr-xNd-yY (mass%) alloys which containing different Nd:Y mass ratio of 3:0, 2:1, 1:2 and 0:3 with a constant x + y = 3 were prepared by metal mould casting method, and the microstructure, aging behaviour and tensile properties have been investigated. The fibrous eutectic areas along the boundaries enlarge clearly in the as-cast alloys containing Y element, and the fine grain boundaries and dispersed precipitation are observed in the aged alloys. The Mg-8Gd-0.6Zr-2Nd-Y alloy exhibits notably age-hardening behaviour and the highest mechanical property. The ultimate tensile strength and yield strength of Mg-8Gd-0.6Zr-2Nd-Y alloy in the peak aged hardness are 293 and 221 MPa at room temperature, 248 and 191 MPa at 230 degrees C. The improvement of age-hardening response and tensile properties is mainly attributed to the quadrate-like stable Mg5RE precipitate, which forms readily and orderly in aged Mg-8Gd-0.6Zr-2Nd-Y alloy.

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Nanocrystals and powders of KMgF3 doped with Eu2+ were synthesized by the microemulsion method and the solvothermal process, respectively. The emission and excitation spectra of KMgF3:Eu2+ phosphors were measured and compared with those of the samples synthesized through a solid. state reaction, Bridgman-Stockbarger method, and mild hydrothermal technique. The KMgF3: Eu2+ samples synthesized by means of the microemulsion method and the solvothermal process show only a sharp emission peak located at 360 nm, in the emission spectra, which arises from the f -> f(P-6(1/2)-> S-8(1/2)) transition of Eu2+. The broad emission bands appear at 420 nm,,which arises from Eu2+ <- O2- cannot be observed(in the mild hydrothermal and single crystal samples, the emission peak at 420 nm besides the emission of Eu2+ at 360 nm is observed). In the excitation spectrum of the KMgF3: Eu2+ samples synthesized by the microemulsion method and the solvothermal process, the excitation peaks show an intensive blue shift. The blue shift can he attributed to the lower oxygenic content in the KMgF3: Eu2+ samples synthesized by the microemulsion method and the solvothermal process.

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The organic-inorganic hybrid materials vanadium oxide [(VO2)-O-IV(phen)(2)](.)6H(2)O (1) and [(2,2'-bipy)(2)(VO2)-O-V](H2BO3)(.)3H(2)O (2) have been conventional and hydrothermal synthesized and characterized by single crystal X-ray diffraction, elemental analyses, respectively. Although the method and the ligand had been used in the syntheses of the compounds (1) and (2) are different, they almost possess similar structure. They all exhibit the distorted octahedral [VO2N4] unit with organonitrogen donors of the phen and 2,2'-bipy ligands, respectively, which coordinated directly to the vanadium oxide framework. And they are both non-mixed-valence complexes. But the compound (1) is isolated, and the compound (2) consists of a cation of [(2,2'-bipy)(2)(VO2)-O-V](+) and an anion of (H2BO3)(-). So the valence of vanadium of (1) and (2) are tetravalence and pentavalence, respectively. Meanwhile it is noteworthy that pi-pi stacking interaction between adjacent phen and 2,2'-bipy groups in compounds I and 2 also play a significant role in stabilization of the structure. Thus, the structure Of [(VO2)-O-IV(phen)(2)](.)6H(2)O and [(2,2'-bipy)(2)(VO2)-O-V](H2BO3)(.)3H(2)O are both further extended into interesting three-dimensional supramolecular.

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Novel soluble rare earth aromatic carboxylates were prepared. The triplet energy level of organic ligand was measured. The photoluminescence properties of the Tb3+ and EU3+ aromatic carboxylates and lifetimes were investigated, which indicated that these rare earth complexes have high quantum efficiency. Because of their excellent solubility, polymer-doping rare earth carboxylates were fabricated as thin Films by spin-coating method and their luminescence properties were studied. Some rare earth organic light-emitting diodes were successfully fabricated which performed high pure color. The maximum luminance of the device of ITO/PVK/PVK :Th (AS)(3)Phen: PBD/PBD/Al is 32 cd(.)m(-2) at 28 V.

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Ru(bpy)(3)(2+) electrochemiluminescence (ECL) method and electrocatalysis method were first used to study the ion-gate behavior of supported lipid bilayer membrane (sBLM). We found that sBLM, made of dimethyldioctadecylammonium bromide (a kind of synthetic lipid), showed ion-gate behavior for the permeation of Ru(bpy)(3)(2+) in the presence of perchlorate anion. There existed a threshold concentration (0.1 muM) of perchlorate anion for ion-gate opening. Below the threshold the ion-gate was closed. Above the threshold, the number of opened ion-gate sites increased with the increase of perchlorate anion concentration and leveled off at concentrations higher than 1200 muM. Based on it, a new sensor for perchlorate was developed. Furthermore, the opening and closing of the ion-gate behavior was reversible, which means the sensor can repeatedly be used.

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A novel compound [Ni(phen)(3)](2)[(SiMo10V1/2O40)-O-V((VO)-O-IV)(2)] . 2H(2)O has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the triclinic, system, space group P-1, a = 12.378(4) Angstrom, b = 14.148(5) Angstrom, c = 14.316(2) Angstrom, alpha = 105.91(2)degrees, beta = 95.31(2)degrees, gamma = 96.89(3)degrees, V = 2373.0(12) Angstrom(3), Z = 1, (lambdaMo(Kalpha)) = 0.71073 Angstrom, R1 (wR2) = 0.0869(0.2174). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.51 < theta < 22.50degrees using the omega-scan technique. Empirical absorption correction (psi scan) was applied. The structure was solved by the direct method and refined by the Full-matrix least-squares on F-2 using the SHELXL-97 software. X-ray crystallographic study showed that the title compound contained a bi-capped alpha-Kegin-type [(SiMo10V2O40)-O-IV((VO)-O-IV)(2)](4-) polyoxoanion.

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A novel compound [Cu(en)(2)](4)[(SiMo8V4O40)-O-v(V-IV O)(2)] [MoO4](2) . 5H(2)O has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. Black crystals crystallize in the tetragonal. system, space group 14/m, a = b = 14.019(2) Angstrom, c = 20.341(4) Angstrom, V = 3997.9(11) Angstrom(3), Z = 2, lambda(MoKalpha) = 0.71073 Angstrom (R(F) = 0.0443 for 1819 reflections). Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range of 1.76 < theta < 24.98degrees using the omega-scan technique. The structure was solved by the direct method and refined by the full-matrix least squares on F-2 method using the SHELXL-97 software. X-ray crystallographic study showed that the title compound contained a bicapped alpha-Keggin fragment [SiMo8 (V4O40)-O-v((VO)-O-IV)(2)](4-) polyoxoanion.

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The different poly (methyl methacrylate) (PMMA) /SiO2 hybrids were prepared through sol-gel method involving PMMA emulsion (emulsion method) and PMMA/THF solution (solution method). The samples were characterized by differential scanning calorimetry(DSC), thermogravimetry analysis(TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results showed that PMMA/SiO2 composites in nanoscale were prepared by emulsion method, and its size of phase heterogeneity was less than that of solution method. Meanwhile, the polymer emulsion as the reactive medium was more suitable for the formation of SiO2 network.

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Single crystals of PrMnO3 and TbMnO3 were grown by floating zone method and the crystal structure was determined by single crystal X-ray diffractometry. The structure of these compounds belongs to the orthorhombic system (space group is Pnma, No. 62) with the lattice parameters alpha approximate to root (.) - a(p), b approximate to 2 (.) a(p) , c approximate to root 2.a(p) and Z = 4, where a(p) is ideal cubic perovskite cell parameter.

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A conductive carbon ceramic composite electrode (CCE) comprised of cc-type 1:12 phosphomolybdic acid (PMo12) and carbon powder in an organically modified silicate matrix was fabricated using a sol-gel method and characterized by scanning electron microscopy, cyclic voltammetry, and Osteryoung square-wave voltammetry. Osteryoung square-wave voltammograms of the modified electrode immersed in different acidic aqueous solutions present the dependence of current and redox potential on pH. The PMo12-doped CCE shows more reversible reaction kinetics, good stability and reproducibility, especially the renewal repeatability by simple polishing in the event of surface fouling or dopant leaching. Moreover, the modified electrode shows good catalytic activity for the electrochemical reduction of bromate.

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CaY1-xBO4: xEu was synthesied by solid state reaction method, and the displacement and luminescence of the Eu3+ in CaYBO4 host were studied. Two luminescent centers could be observed at certain Eu3+-concentration, indicating that the Eu3+ occupies two different crystallographic sites. This result shows that the Eu3+ occupies two different Y3+ sites in CaYBO4. The investigation on Eu-O charge transfer bands indicates that the larger distortion or the lower symmetry of Eu3+ site is,the shorter wavelength of the Eu-O charge transfer band is. When the Eu3+-concentration is high (x > 0.10), Eu3+ occupies the sites of Ca2+ and is reduced to Eu2+.

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The effects of rubber content and temperature on dynamic fracture toughness of ABS materials have been investigated based on the J-integral and crack opening displacement (COD, delta) concepts by an instrumented Charpy impact test. A multiple specimens R-curve method and stop block technique are used. It is shown that the materials exhibit a different toughness behavior, depending on rubber content and temperature. The resistance against stable crack initiation (J(0.2) or delta(0.2)) increases with increasing rubber content. However, J(0.2) first increased with increasing temperature until reaching the maximum value; after that, it decreases with further increasing the temperature. (C) 2000 John Wiley & Sons, Inc.