Microwave-assisted hydrothermal synthesis of hydroxy-sodalite zeolite membrane

A high quality pure hydroxy-sodalite zeolite membrane was successfully synthesized on an alpha-Al2O3 support by a novel microwave-assisted hydrothermal synthesis (MARS) method. Influence of synthesis conditions, such as synthesis time, synthesis procedure, etc., on the formation of hydroxy-sodalite zeolite membrane by MAHS method was studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and gas permeation measurements. The synthesis of hydroxy-sodalite zeolite membrane by MAHS method only needed 45 min and synthesis was more than 8 times faster than by the conventional hydrothermal synthesis (CHS) method. A pure hydroxy-sodalite zeolite membrane was easily synthesized by MAHS method, while a zeolite membrane, which consisted of NaX zeolite, NaA zeolite and hydroxy-sodalite zeolite, was usually synthesized by CHS method. The effect of preparation procedures had a dramatic impact on the formation of hydroxy-sodalite zeolite membrane and a single-stage synthesis procedure produced a pure hydroxy-sodalite zeolite membrane. The pure hydroxy-sodalite zeolite membrane synthesized by MARS method was found to be well inter-grown and the thickness of the membrane was 6-7 mum. Gas permeation results showed that the hydrogen/n-butane permselectivity of the hydroxy-sodalite zeolite membrane was larger than 1000. (C) 2004 Elsevier Inc. All rights reserved.

Synthesis and characterization of Eu-doped hydroxyapatite through a microwave assisted microemulsion process

Europium doped hydroxyapatite (Eu:HAp) nanosized particles with multiform morphologies have been successfully prepared via a simple microemulsion-mediated process assisted with microwave heating. The physicochemical properties of the samples were well characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), Fourier transform infrared spectroscopy (FT-IR), photoluminescence (PL) spectra, and the kinetic decays, respectively. The results reveal that the obtained Eu:HAp particles are well assigned to the hexagonal lattice structure of the hydroxyapatite phase. Additionally, it is found that samples exhibit uniform morphologies which can be controlled by altering the pH values. Furthermore, the samples show the characteristic D-5(0)-F-7(1-4) emission lines of Eu3+ excited by UV radiation.

Microwave-assisted preparation of 2-methallyloxyphenol

Catechol reacted with beta-methallyl chloride in the presence of base and phase transfer catalyst under microwave irradiation and gave 2-methallyloxyphenol within 1 similar to 2 minutes. The yield of 2-methallyloxyphenol varied from 64%similar to 68%.

Hyperbranched polymer-assisted hydrothermal in situ synthesis of submicrometer silver tubes

We produced silver tubes with an outer diameter of 1 mu m, wall thickness of 200 nm, and length of hundreds of micrometers by hydrothermal treatment of aqueous solutions of AgNO3 and hyperbranched polyglycidol (HPG) at 165 degrees C. The surfaces of the silver tubes were chemically modified by HPG, which was confirmed by FTIR of the silver tubes.

Microwave-assisted synthesis of high-molecular-weight poly(ether imide)s by phase-transfer catalysis

A facile and rapid polycondensation reaction of disodium bisphenol A with bis(chlorophthalimide)s was preformed with a domestic microwave oven in o-dichlorobenzene by phase-transfer catalysis. The polymerization reactions, in comparison with conventional heating polycondensation, proceeded rapidly and were completed within 25 min. The polymerizations gave the corresponding poly(ether imide)s with inherent viscosities of 0.55-0.92 dL g(-1). The effects of various factors on the polymerization, such as the amount of the catalyst, the reaction time, and the microwave power were studied. The properties of the polymers were briefly characterized.

Engineering white light-emitting Eu-doped ZnO urchins by biopolymer-assisted hydrothermal method

With the presence of biopolymer-sodium alginate as additive, Eu-doped ZnO (zinc oxide) urchins consisting of nanorods were synthesized through a hydrothermal route. X-ray diffraction pattern makes evident the absence of phase other than wurtzite ZnO. Upon excited by 325 nm xenon laser, such nanostructured Eu-doped ZnO urchins emit white light, which originates from the luminescence of ZnO and the intra-4f transitions of Eu3+ ions. Besides acting as stabilizing agent, sodium alginate may also sensitize the Eu3+ ions in the nanostructures and facilitate the energy transfer from the host to Eu3+ ions. (c) 2006 American Institute of Physics.

3D Fe3S4 flower-like microspheres: high-yield synthesis via a biomolecule-assisted solution approach, their electrical, magnetic and electrochemical hydrogen storage properties

Well-defined 3D Fe3S4 flower-like microspheres were synthesized via a simple biomolecule-assisted hydrothermal process for the first time. On the basis of a series of contrast experiments, the probable growth mechanism and fabrication process of the products were proposed. The electrical conductivity property of the as-synthesized Fe3S4 sample exhibited a rectifying characteristic when a forward bias was applied for the bottom-contacted device. The magnetic properties of the products were studied as well and the results demonstrated that the products presented ferromagnetic properties related to the corresponding microstructure. In addition, we first verified that the Fe3S4 flower-like microspheres could store hydrogen electrochemically, and a discharge capacity of 214 mA h g(-1) was measured without any activation under normal atmospheric conditions at room temperature.

辅助水热法制备不同形貌的柱状ZnO微晶(英文)

本文采用乙醇辅助水热法制备得到了柱状ZnO微晶。得到的微晶形貌多样，有单脚、三脚、四脚、五脚、六脚以及多脚状，并以“骨架＋支架”模型进行解释。X射线衍射分析结果表明产物为纯的六方相纤锌矿结构，扫描电子显微镜（SEM）观察表明产物具有单晶属性。本文还研究了ZnO的室温光谱性能。

Effects of ammonia and cetyltrimethylammonium bromide (CTAB) on morphologies of ZnO nano- and micromaterials under solvothermal process

Submicrometer zinc oxide (ZnO) with different morphologies including spindle-like, pencil-like, branch rod-like and frizzy flower-like shapes, have been hydrothermally synthesized in mixed solvents of ethanol and water at 140 degrees C. It was found that the volumes of added ammonia, surfactant (cetyltrimethylammonium bromide, CTAB), and mixed solvent play crucial roles in morphological control of ZnO nanostructures. Increasing the volume of ammonia added to the reaction system, the shape of ZnO evolves from spindle into branch rod-like. Synergetic influence between CTAB and ammonia can only be observed at high concentration of ammonia.

Salt-assisted microwave demulsification

Experimental data are presented to show the influence of a very small amount of inorganic salt on the demulsification of water-in-oil emulsions. It was found that some inorganic salts could effectively enhance the demulsification efficiency and increase the light transmittance of the water separated from the emulsions. The demulsification efficiency may reach 100% in a very short time under microwave radiation.

Shape and Phase-Controlled Synthesis of KMgF3 Colloidal Nanocrystals via Microwave Irradiation

In this paper, we present a facile one-step route to controlled synthesis of colloidal KMgF3 nanocrystals via the thermolysis of metal trifluoroacetate precursors in combined solvents (OA/OM) using microwave irradiation. X-ray diffraction (XRD), transmission electron microscopy (TEM), thermogravimetric and differential thermal analysis (TG-DTA), Fourier transform infrared (FT-IR) spectra, and photoluminescence (PL) spectra were employed to characterize the samples. Only through the variation of the OA/OM ratio, can the phase and shape of nanocrystals be readily controlled, resulting in the formation of well-defined near-spherical nanoparticles, and nanoplates of cubic-phased KMgF3, as well as nanorods of tetragonal-phased MgF2, and a possible mechanism has been proposed to elucidate this effect. Furthermore, all these samples in this system can be well dispersed in nonpolar solvents such as cyclohexane to form stable and clear colloidal solutions, due to the successful coating of organic surfactants (OA/OM) on the nanocrystal surface.

Salt-assisted acid hydrolysis of chitosan to oligomers under microwave irradiation

The effect of inorganic salts such as sodium chloride on the hydrolysis of chitosan in a microwave field was investigated. While it is known that microwave heating is a convenient way to obtain a wide range of products of different molecular weights only by changing the reaction time and/or the radiation power, the addition of some inorganic salts was shown to effectively accelerate the degradation of chitosan under microwave irradiation. The molecular weight of the degraded chitosan obtained by microwave irradiation was considerably lower than that obtained by traditional heating. Moreover, the molecular weight of degraded chitosan obtained by microwave irradiation assisted under the conditions of added salt was considerably lower than that obtained by microwave irradiation without added salt. Furthermore, the effect of ionic strength of the added salts was not linked with the change of molecular weight. FTIR spectral analyses demonstrated that a significantly shorter time was required to obtain a satisfactory molecular weight by the microwave irradiation-assisted inorganic salt method than by microwave irradiation without inorganic salts and conventional technology. (C) 2005 Elsevier Ltd. All rights reserved.