987 resultados para one-pass tableau
Resumo:
A one-step method has been developed for synthesizing gold-polyaniline (Au@PANI) core-shell particles by using chlorauric acid (HAuCl4) to oxidize aniline in the presence of acetic acid and Tween 40 at room temperature. SEM images indicated that the resulting core-shell particles were composed of submicrometre-scale Au particles and PANI shells with an average thickness of 25 nm. Furthermore, a possible mechanism concerning the growth of Au@PANI particles was also proposed based on the results of control experiments.
Resumo:
A new setup to couple capillary electrophoresis (CE) with electrochemiluminescence (ECL) detection is described in which the electrical connection of CE is achieved through a porous section at a distance of 7 mm from the CE capillary outlet. Because the porous capillary wall allowed the CE current to pass through and there was no electric field gradient beyond that section, the influence of CE high-voltage field on the ECL procedure was eliminated. The porous section formed by etching the capillary with hydrofluoric acid after only one side of the circumference of 2-3 mm of polyimide coating of the capillary was removed, while keeping the polyimide coating on the other part to protect the capillary from HF etching makes the capillary joint much more robust since only a part of the circumference of it is etched. A standard three-electrode configuration was used in experiments with Pt wire as a counter electrode, Ag/AgCl as a reference electrode, and a 300-mum diameter Pt disk as a working electrode. Compared with CE-ECL conventional decoupler designs, the present setup with a porous joint has no added dead volume created.
Resumo:
Highly stable silver nanoclusters with narrow size distribution have been prepared by heating a third-generation poly(propyleneimine) dendrimer/AgNO3 aqueous solution without the additional step of introducing other reducing agents and protect agents. UV-vis absorption, transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), and X-ray diffraction (XRD) have been used to characterize the resulting products. The as-obtained sample was in coexistence of Ag and Ag2O. It also suggested that increasing temperature resulted in both the decrease in number of small particles and the increase in size of large particles.
Resumo:
Polyelectrolyte-protected gold nanoparticles have been facilely obtained by heating an amine-containing polyelectrolyte/HAuCl4 aqueous solution without the additional step of introducing other reducing agents. All experimental data indicate that different initial molar ratio of polyelectrolyte to gold can lead to the formation of dispersed nanoparticles, quasi one-dimensional aggregates of nanoparticles or bulk metal deposits. More importantly, the growth kinetics of gold particles thus formed can be tuned by changing the initial molar ratio of polyelectrolyte to gold.
Resumo:
A new class of organic-inorganic hybrid porous clay heterostructures (HPCHs) have been prepared through the surfactant-directed assembly of organosilica in the galleries of montmorillonite. The reaction involved hydrolysis and condensation of phenyltriethoxysilane and tetraethoxysilane in the presence of intragallery surfactant templates (dodecylame and cetyltrimethylammonium ion). The surfactant templates were removed from the pores by solvent-extraction. The products were characterized by X-ray diffraction (XRD), N-2 adsorption, solid-state Si-29 and C-13 NMR, and FTIR. XRD patterns indicated a regular interstratification of the clay layers for HPCHs. Depending on loading of phenyl groups, HPCHs had BET surface areas of 390-771 m(2) g(-1), pore volumes of 0.3-0.59 cm(3) g(-1), and the framework pore sizes in the supermicropore to small mesopore range (1.2-2.6 nm). HPCHs were hydrophobic and acidic.
Resumo:
Self-immobilized nickel and iron diimine catalysts bearing one or two allyl groups of [ArN=C](2)(C10H6)NiBr2 [Ar = 4-allyl-2,6-(i-Pr)(2)C6H2] (1), [ArN=C(Me)[Ar'N=C(Me)]C5H3NFeCl2 [Ar = Ar' = 4-allyl-2,6-(i-Pr)(2)C6H3, Ar = 2,6-(i-Pr)(2)C6H3, and Ar' = 4-allyl-2,6-(i-Pr)(2)C6H3] were synthesized and characterized. All three catalysts were investigated for olefin polymerization. As a result, these catalysts not only showed high activities as the catalyst free from the allyl group, such as [ArN=C](2)C10H6,NiBr2 (Ar = 2,6-(i-Pr)(2)C6H2)], but also greatly improved the morphology of polymer particles to afford micron-granula polyolefin. The self-immobilization of catalysts, the formation mechanism of microspherical. polymer, and the influence on the size of the particles are discussed. The molecular structure of self-immobilized nickel catalyst 1 was also characterized by crystallographic analysis.
Resumo:
The self-assembly of oligo(o-phenylenediamine) (OPD) into 1-D nanostructures on a macroscopic length scale was found when they were transferred from N-methyl pyrrolidone to deionized water. Field emission scanning electron microscopy and confocal fluorescence microscopy were used to investigate the morphology of the precipitates. Results showed that large amounts of OPD 1-D supertructures could be obtained through the simple reprecipitation route, and the length of the fibers could be tuned from microscale to macroscale by adjusting the ratio of two solvents. X-ray diffraction patterns and UV-vis spectra revealed that pi-pi interactions between OPD molecules that facilitated the formation of 1-D structures became predominant when they were transferred from a good solvent to a bad one. Accordingly, a possible formation mechanism was proposed.
Resumo:
Novel spherical three-dimensional (3D) dendritic gold-polypyrrole nanocomposites were successfully prepared in the presence of an amphiphilic p-toluene sulfonic acid (TSA) as dopant and surfactant via a self-assembly process which is based on the oxidation of pyrrole (Py) and the reduction of the chloroaurate ions, yielding PPy and Au(0) simultaneously. It was found that the probability of obtaining dendritic Au@PPy/TSA nanostructures depended on the concentration of TSA and the rate of addition of the oxidant (HAuCl4), It was also proposed that the supramolecular micelles formed by Py and TSA play the role of a 'soft template' to produce the dendritic Au@PPy/TSA nanocomposites.
Resumo:
Poly(diallyl dimethylammonium) chloride (PDDA), an ordinary and watersoluble, cationic polyelectrolyte, was investigated for its ability to generate and stabilize gold colloids from a chloroauric acid precursor. In this reaction, PDDA acted as both reducing and stabilizing agents for gold nanoparticles (AuNPs). More importantly, PDDA is a quaternary ammonium polyelectrolyte, which shows that the scope of the reducing and stabilizing agents for metal nanoparticles can be extended from the amine-containing molecules to quaternary ammonium polyelectrolytes or salts. UV-vis spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS) and Fourier transform infrared (FTIR) were used to characterize the synthetic AuNPs. The PDDA-protected AuNPs obtained are very stable and have relative narrow size distribution.
Resumo:
In this work, we have developed a one-pot, morphology controlled epitaxial growth method to synthesize novel cactus-like ZnO in solution. Utilizing zinc acetate and hexamethylenetetramine as the precursors, ZnO nanorods synthesized in the first step remained in the solution, without any separation, served directly as the matrix for the epitaxial growth in the second step. Control experiments revealed that a proper mass of precursors added in the second step was crucial to form cactus-like ZnO. The as-synthesized ZnO was single crystalline and possessed three photoluminescence emissions centered at 390, 425 and 490 run. Finally, a possible mechanism for the epitaxial growth ZnO was proposed and discussed.
Resumo:
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.
Resumo:
Polyetherimides and copolymers have been synthesized in one pot from bis(chlorophthalimide), dichlorodiphenylsulfone, and bisphenolate using diphenylsulfone as the solvent. The inherent viscosities of the obtained polyimides are in the range of 0.32-0.72 dL/g, and the structures of polyimides were confirmed by IR and elemental analyses. All of the polyimides have good solubility in common organic solvents. The 5% weight-loss temperatures of the polyimides were 429-507 C in air. The glass transition temperatures (T3) of 4,4'-(9-fluorenylidene) diphenol-based polyimides are in the range of 253-268 degrees C. The Tg of bisphenol A-based polyimides is in the range of 198204 degrees C, while the T-g change inconspicuously when the ratios of diphenylsulfone increase. The wide-angle X-ray diffraction showed that all polyimides prepared are amorphous.
Resumo:
One-pot preparation of shell-type silver-gold bimetallic nanostructures with hollow interiors and bearing nanospikes, based on colloid seed-engaged replacement reaction and colloid-mediated deposition reactions, has been reported. Heating-induced evolution of Ag-Au bimetallic nanoshells can lead to spontaneous production of nanospikes on the colloid surface. The hollow interior structure and bimetallic nature of the as-prepared colloids are characterized by transmission electron microscopy (TEM), UV-vis spectroscopy, and X-ray photoelectron spectroscopy (XPS).
Resumo:
Two novel organic-inorganic hybrid complexes [(CuX)(2)(o-phen)](infinity) (X = Br (1), Cl (2); o-phen = o-phenanthroline) have been synthesized hydrothermally and characterized structurally by elemental analyses, IR, ESR, XPS spectrum, TG analyses and single-crystal X-ray diffraction. Both title compounds exhibit novel one-dimensional chainlike copper halide scaffolding constructed by the unusual [Cu3X3] hexagon motifs by sharing opposite edges, where a single Cu site of each [Cu3X3] hexagon is chelated with N donors of o-phen group. To our knowledge, such basic o-phen-copper halide skeleton has not been reported hitherto. Moreover, TG analyses indicate that both title compounds possess high thermal stability.