966 resultados para synthesis and integrative research


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In this article, we firstly reported on the synthesis and characterization of ultratine CeF3 nanoparticles (NPs) modified by catanionic surfactant via a reverse micelles-based route. The catanionic surfactant PN was prepared by mixing the di(2-ethylhexyl) phosphoric acid (DEHPA) and primary amine (N1923) with 1:1 molar ratio. It exhibited a high surface activity and formed much small reverse micelles in comparison with its individual component (DEHPA or N1923). The PN reverse micelles were then used as templates to prepare ultrafine CeF3 NPs. The narrow distributed nanoparticles have an average diameter 1.8 nm. FTIR spectra indicated that there existed strong chemical interactions between nanoparticles and the adsorbed surfactants. The modification resulted in the FFIR peak position of P=O shifting to lower energy. Due to the effect of modification and small size, the CeF3 NPs showed a remarkable red shift of 54 mn in the fluorescence emission in comparison with that of bulk material and a red shift of 18 nm in contrast with that of the normal CeF3 NPs with an average diameter of 16 nm.

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Y2O3:RE3+ (RE = Eu, Tb, Dy) porous nanotubes were first synthesized using carbon nanotubes as template. The morphology of the coated precursors and porous Y2O3:Eu3+ nanotubes was determined by scanning electron Microscopy (SEM) and transmission electron microscopy (TEM). It was found that the coating of precursors on carbon nanotubes (CNTs) is continuous and the thickness is about 15 nm, after calcinated, the Y2O3:Eu3+ nanotubes are porous with the diameter size in the range of 50-80 nm and the length in micrometer scale. X-ray diffraction (XRD) patterns confirmed that the samples are cubic phase Y2O3 and the photoluminescence studies showed that the porous rare earth ions doped nanotubes possess characteristic emission of Eu3+, Tb3+, and Dy3+. This method may also provide a novel approach to produce other inorganic porous nanotubes used in catalyst and sensors.

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A blue emitting Sr2CeO4 phosphor with a one-dimensional structure has been prepared by a two-step spray pyrolysis (SP) method, starting from the aqueous solutions of metal nitrates with citric acid and polyethylene glycol (PEG) as additives. The material is ultimately designed for field emission displays (FEDs). X-ray diffraction (XRD), thermogravimetric and differential thermal analysis (TG-DTA), field emission scanning electron microscope pictures (FE-SEM) as well as photoluminescence (PL) and cathodoluminescence (CL) spectroscopy and lifetime measurements have been employed to characterize the samples. The morphology, PL and low voltage CL properties of Sr2CeO4 phosphors as-prepared using the SP method have been investigated by changing the concentration of the precursor solution, concentration of PEG, annealing temperature, acceleration voltage and filament current. The obtained Sr2CeO4 phosphor particles are spherical and of submicron size, 0.5-2 mu m. The emission spectrum of the phosphors shows a broad band with maximum at 467 nm (lifetime = 37.4 mu s; CIE chromaticity coordinates: x = 0.15 and y = 0.21), presumably due to a ligand-to-metal charge-transfer transition.

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Polyelectrolytes have been widely used as building blocks for the creation of thickness-controllable multilayer thin films in a layer-by-layer fashion, and also been used as flocculants or stabilizer of colloids. This paper reports novel finding that a kind of polyelectrolyte, polyamines, can facilely induce HAuCl4 to spontaneously form well-stabilized gold nanoparticles without the additional step of introducing a reducing reagent during the elevation of temperature, even at room temperature in some cases. The polymer chain-confined microenvironment and the acid-induced evolution of amide of such kind of polyelectrolyte solution play an important role in the nucleation and growth of gold nanoparticles. This method would not only be helpful to gain an insight into the formation of gold nanoparticles in polyelectrolyte systems, but also provide a novel and facile one-step polyelectrolyte-based synthetic route to polyelectrolyte protected gold nanoparticles in aqueous media for potential applications. More importantly, this strategy will be general to the preparation of other nanoparticles.

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Thiophene copolymers and their derivatives with poly(ethylene oxide) side chains were synthesized. The starting monomers were 3-hexylthiophene and 2-(3-thienyl) ethanol with poly(ethylene oxide) grafted to the side chains. New functionalized polythiophenes were prepared by both chemical oxidation with FeCl3 and electropolymerization. The conjugating polymers were characterized. The structures of the polythiophene derivatives agreed with the design.

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Dispersion copolymerization of acrylamide with acrylic acid in an aqueous solution of ammonium sulfate using poly(2-acrylamido-2-methylpropanesulfonic acid sodium) as the stabilizer and ammonium persulfate (APS) as the initiator was investigated. The influence of initiator concentration, stabilizer concentration, ammonium sulfate concentration, chain-transfer agent concentration, and polymerization temperature on the copolymerization was discussed. The results showed that varying the ammonium sulfate concentration could affect the particle size and the intrinsic viscosity of the copolymer significantly. With increasing the stabilizer concentration, the particle size of the copolymer decreased first, and then increased, meanwhile the intrinsic viscosity of the copolymer decreased. The increase of initiator concentration, chain-transfer agent concentration, and polymerization temperature resulted in the increase in the particle size. Polydisperse spherical particles were formed in the system, and the kinetics for the dispersion copolymerization were discussed.

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The quasiliving characteristics of the ringopening polymerization of epsilon-caprolactone (CL) catalyzed by an organic amino calcium were demonstrated. Taking advantage of this feature, we synthesized a series of poly (F-caprolactone) (PCL)-poly(L-lactide) (PLA) cliblock copolymers with the sequential addition of the monomers CL and L-lactide. The block structure was confirmed by H-1-NMR, C-13-NMR, and gel permeation chromatography analysis. The crystalline structure of the copolymers was investigated by differential scanning calorimetry and wide-angle X-ray diffraction analysis. When the molecular weight of the PLA block was high enough, phase separation took place in the block copolymer to form PCL and PLA domains, respectively.

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A novel mimic TeHA was synthesized by modifying hyaluronic acid (HA) with tellurium, whose function is similar to that of glutathione peroxidase (GPX). The structure of TeHA was characterized by means of infrared spectroscopy and nuclear magnetic resonance spectroscopy, showing that the target Te is located at -CH2OH of the N-acetyl-D-glucosamine of HA. The activity of TeHA is 163.6 U/mu mol according to Wilson's method. In contrast to other mimics, TeHA displays a high activity. Moreover, TeHA can use many hydroperoxides as substrates, such as H2O2, cumenyl hydroperoxide, and tert-butyl hydroperoxide, and cumenyl hydroperoxide is the optimal substrate. A ping-pong mechanism was deduced for the reduction reactions catalyzed by TeHA according to the steady-state kinetic studies.

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Three new cyclometalated iridium(III) complexes based on ligands of diphenylquinoline with fluorinated substituents were prepared, and characterized by elemental analysis (EA), H-1 NMR, and mass spectroscopy (MS). The photophysical and electrophosphorescent properties of the complexes were briefly discussed.

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A novel mimic was synthesized by modifying hyaluronic acid (HA) with tellurium, whose function is similar to that of glutathione peroxidase (GPX). The structure of TeHA was characterized by means of IR and NMR, the target-Te was located at -CH2OH of the N-acetyl-D-glucosamine of HA. The H2O2 reducing activity of TeHA, by glutathione (GSH), was 163.6 U/mu mol according to Wilson's method. In contrast to other mimics, TeHA displayed the highest activity. Moreover, TeHA accepted many hydroperoxides as its substrates, such as H2O2, cumenyl hydroperoxide (CuOOH) and tert-butyl hydroperoxide (t-BuOOH), and CuOOH was the optimal substrate of TeHA. A ping-pong mechanism was observed in the steady-state kinetic studies of the reactions catalyzed by TeHA.

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The four AB(2) monomers, N-[3- or 4-bis(4-hydroxyphenyl)toluoyl]-4-chlorophthalimide and N-{3- or 4-[1,1-bis(4-hydroxyphenyl)]ethylphenyl}-4-chlorophthalimides, were prepared and used for synthesis of hyperbranched poly(ether imide)s bearing hydroxyl end groups. These hyperbranched poly(ether imide)s had moderate molecular weights with broad distributions and showed glass-transition temperatures (Tgs) between 177 and 230 degreesC. The thermogravimetric analytic measurement revealed the decomposition temperature at 5% weight-loss temperatures (T-d(5%)) ranging from 240 to 281 degreesC. Analysis using H-1 NMR spectroscopy revealed the four types of hyperbranched poly(ether imide)s to have similar degrees of branching (ca. 60%). These polymers were modified by acylation or nucleophilic substitution reaction at the hydroxyl end groups. The conversion effectiveness depended on the type of modification reaction, modifier, and reaction conditions. The thermal stability and solubility of hyperbranched poly(ether imide)s were improved by the modification of the end groups.

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The synthesis and characterization of hyperbranched aromatic poly(ester-imide)s are described. A variety of AB(2) monomers, N-[3- or 4-bis(4-acetoxyphenyl)toluoyl]-4-carboxyl-phthalimide and N-{3- or 4-[1,1-bis(4-acetooxyphenyl)]ethylphenyl}-4-carboxy phthalimides were prepared starting from condensation of nitrobenzaldehydes or nitroacetophenones with phenol and used for synthesis of hyperbranched poly(ester-imide)s containing terminal acetyl groups by transesterification reaction. These hyperbranched poly(ester-imide)s were produced with weight-average molecular weight of up to 6.87 g/mol. Analysis of H-1 NMR and C-13 NMR spectroscopy revealed the structure of the four hyperbranched poly(ester-imide)s. These hyperbranched poly(ester-imide)s exhibited excellent solubility in a variety of solvents such as N,N-dimethylacetamide, dimethyl sulfoxide, and tetrahydrofuran and showed glass-transition temperatures between 217 and 255 degreesC. The thermogravimetric analytic measurement revealed the decomposition temperature at 10% weight-loss temperature (T-d(10)) ranging from 365 to 416 degreesC in nitrogen.

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Graft copolymerization of maleic anhydride (MA) onto poly(3-hydroxybutyrate) (PHB) was carried out by use of benzoyl peroxide as initiator. The effects of various polymerization conditions on graft degree were investigated, including solvents, monomer and initiator concentrations, reaction temperature, and time. The monomer and initiator concentrations played an important role in graft copolymerization, and graft degree could be controlled in the range from 0.2 to 0.85% by changing the reaction conditions. The crystallization behavior and the thermal stability of PHB and maleated PHB were studied by DSC, WAXD, optical microscopy, and TGA. The results showed that, after grafting MA, the crystallization behavior of PHB was obviously changed. The cold crystallization temperature from the glass state increased, the crystallization temperature from the melted state decreased, and the growth rate of spherulite decreased. With the increase in graft degree, the banding texture of spherulites became more distinct and orderly. Moreover, the thermal stability of maleated PHB was obviously improved, compared with that of pure PHB.

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Novel soluble alternating conjugated copolymers (PFSP and PFSR) comprised of phenothiazine unit are synthesized by palladium-catalyzed Suzuki coupling reactions. Their thermal stability, photoluminescence, electroluminescence, hole injection and transport properties are investigated. The resulting copolymers exhibit good thermal stability and excellent hole-injection ability (about -5.2eV), which are closely matched to the work function of ITO. Double-layer devices demonstrate that PFSP is a promising hole-transporting material for electroluminescent devices.