Effects of polyethyleneimine-functionalized MCM-41 on flame retardancy and thermal stability of polyvinyl alcohol

Hyperbranched polyethylenimine（PEI）-functionalized mesoporous silica（MCM@PEI） was synthesized and used to produce poly（vinyl alcohol）（PVA） nanocomposites.The modified nanofiller was characterized with infrared spectroscopy,thermogravimetric analysis,X-ray diffraction,scanning electron microscopy,transmission electron microscopy,and N₂ adsorption.When compared with pure mesoporous silica（MCM）,the MCM@PEI nanoparticles exhibited better dispersion in the PVA matrix.The effects of MCM@PEI on the thermal and flame properties of PVA nanocomposites were also studied.Improvement in the thermal properties was confirmed by enhanced thermal stability and char yield.Incorporation of MCM@PEI in PVA led to a significant drop in the heat release rate and the total heat release.     

SYNTHESIS AND COATING OF ORDERED MESOPOROUS SILICA

1,3,5-trimethyl benzene (TMB) was used as organic swelling agent in O/W emulsions to template ultra-large mesoporous materials using the hydrothermal method. The silicas with well-defined mesopores and hydrothermally robust framework were characterized by X-ray diffraction, transmission electron microscopy and BET surface area analysis. The influence of the quantity of TMB during preparation was studied. It has been found that the TMB/CTAB ratio must be controlled for producing high pore volume materials. Polysulfone (PSU), as the usual extraction agent, was coated on the silicas with the solvent evaporation method to produce a solid separation medium. The adsorptivity and the surface area of the coated MCM were determined: 10% PSU coated MCM adsorbed twice as much phenol as the uncoated material, reaching 0.5 mg/g silica. It was found that the surface area of the coated material decreased rapidly with an increase of the PSU Ioadina.     

Preparation and Li^＋ storage properties of hierarchical hollow porous carbon spheres

Hollow ordered porous carbon spheres （HOPCS） with a hierarchical structure were prepared by templating with hollow ordered mesoporous silica spheres （HOMSS）. Scanning electron microscopy （SEM） and transmission electron microscopy （TEM） showed that HOPCS exhibited a spherical hollow morphology. High-resolution TEM, small angle X-ray diffraction （SAXRD） and N2 sorption measurements confirmed that HOPCS inversely replicated the unconnected hexagonal-stacked pore structure of HOMSS, and possessed ordered porosity. HOPCS exhibited a higher storage capacity for Li^＋ ion battery （LIB） of 527.6 mA h/g, and good cycling performance. A large capacity loss during the first discharge-charge cycle was found attributed to the high content of micropores. The cycling performance was derived from the hierarchical structure.     

SYNTHESIS OF MESOPOROUS TiO_2 MATERIALS WITH HIGH SPECIFIC AREA USING INORGANIC ACIDS AS CATALYSTS

This paper presents a synthesis process for preparing mesoporous titanium dioxide materials in the absence of any templates and using inorganic acids as catalysts. Tetrabutyl titanate was used as the precursor at ambient temperature, and four different inorganic acids, i.e., hydrochloric, nitric, sulfuric and phosphoric, were used as catalysts. The as-prepared mesoporous TiO2 materials were characterized by SEM, XRD and nitrogen adsorption/desorption measurements. The influences of different inorganic acids on the properties of TiO2 were discussed and compared in details. Experiments showed that the inorganic acids have significant effects on the surface area, pore volume, pore size, and pore size distribution of the products. The mesoporous TiO2 materials catalyzed by phosphoric acid exhibited the largest specific surface area and largest pore volume with narrow pore size distribution. Vacuum and infrared drying methods tested in the process were found to have subtle impact on the structure of the TiO2 materials prepared.     

EFFECTS OF FINELY DISPERSED METALLIC PALLADIUM ON MICROSTRUCTURE AND PROPERTIES OF NANOCOMPOSITES PRODUCED BY SOL-GEL TECHNIQUE

Nanosized palladium particles were incorporated into mesoporous silica matrix to obtain nanocomposites using the sol-gel technique. Effects of the finely dispersed metallic palladium on the microstructure and properties of the nanocomposites were investigated. By means of X-ray diffraction and optical absorption, it was found that palladium particles were 5-9 nm in diameter and their uniform dispersion in the mesoporous silica depended on both the content of the palladium and the structural features of the silica matrix. The results showed that the mixing method of preparation led to wider size distribution of the nanosized particles as compared to the immersion method, but dispersed degree was reduced. Although the incorporation of nanosized palladium particles could not substantially induce significant structural changes of the matrix, the apparent red-shifted optical absorptions for the nanocomposites were observed as compared to the parent monolithic silica, particularly with increase in palladium loading and calcination temperature.     

SYNTHESIS OF MESOPOROUS TiOz MATERIALS WITH HIGH SPECIFIC AREA USING INORGANIC ACIDS AS CATALYSTS

This paper presents a synthesis process for preparing mesoporous titanium dioxide materials in the absence of any templates and using inorganic acids as catalysts. Tetrabutyl titanate was used as the precursor at ambient temperature, and four different inorganic acids, i.e., hydrochloric, nitric, sulfuric and phosphoric, were used as catalysts.The as-prepared mesoporous TiO2 materials were characterized by SEM, XRD and nitrogen adsorption/desorption measurements, The influences of different inorganic acids on the properties of TiO2 were discussed and compared in details. Experiments showed that the inorganic acids have significant effects on the surface area, pore volume, pore size,and pore size distribution of the products. The mesoporous TiO2 materials catalyzed by phosphoric acid exhibited the largest specific surface area and largest pore volume with narrow pore size distribution. Vacuum and infrared drying methods tested in the process were found to have subtle impact on the structure of the TiO2 materials prepared,     

Preparation and functionalization of mesoporous silica spheres as packing materials for HPLC

This paper presents the integrated results of a series of new methods for preparing mesoporous silica spheres as high-performance liquid chromatography （HPLC） packing materials. The separation performance of the mesoporous spheres materials has also been determined. Micrometer- sized silica spheres with uniform spherical morphologies and ordered mesostructures were first successfully synthesized by the method employing a water-soluble polymer-assisted assembly. Then the templates for getting ordered mesoporous materials with high-density silanol groups were removed by using hydrothermal oxidation. Finally the silica spheres were functionalized with C8 alkyl groups by surface modification under hydrothermal conditions. The resultant functionalized silica spheres were demonstrated to be excellent oacking materials for HPLC.     

Improving photoelectrochemical activity of dye sensitized solar cell by a bilayered electrode with an overlayer of mesoporous anatase TiO_2

For better performance of dye sensitized solar cells(DSSCs) ,a bilayer structured electrode was constructed by employing a mesoporous anatase TiO2 overlayer above a commercial P25 TiO2 nanoparticles underlayer. The mesoporous anatase TiO2,prepared through a facile surfactant-assisted sol-gel process,possessed large pore size and well inter-connected network structure,both beneficial for dye adsorption and electron transfer. The dye adsorption capability of the mesoporous TiO2 was nearly twice that of the P2...     

Synthesis of Ag/AgCl-mesoporous silica nanocomposites using a simple aqueous solution-based chemical method and a study of their antibacterial activity on E. coli

Simple aqueous solution-based chemical methods have been developed for the synthesis of Ag/AgCl nanoparticle-mesoporous silica nanocomposites. Ag loading in the mesoporous silica was accomplished using a wet-impregnation method. The AgCl-mesoporous silica nanocomposite material(AgCl-mSi) was synthesized by using a 'one pot' method. Synthesized materials were characterized using X-ray diffraction,N2 adsorption-desorption analysis and high-resolution transmission electron microscopy. Antibacterial activity of...     

PREPARATION AND MICROSTRUCTURE CHARACTERIZATION OF Ni／TiO2 NANOCOMPOSITE

Homogeneous Ni^2 -doped titania gel was synthesized by a sol-gel process,and the xerogel was then obtained through aging and drying,leading to the formation of Ni/TiO2 nanocomposite after heat treatment under a suitable reducing atmosphere.The resulting nanocomposite was characterized by TGA-DSC,TEM,XRD and BET methods.The results show that the structure and grain size of the nanocomposites could be manipulated by altering the heat-treatment conditions,and that the nanocomposite possesses a mesoporous structure with a pore radius of ca.28nm and a specific surface area of 49.1 m^2.g^-1.It is demonstrated that the nanosized Ni dispersion in the titania matrix significantly affects the anatase-rutile phase transformation.     

Fabrication of magnetic nanosized γ-FeNi-coated ceramic core-shell microspheres by heterogeneous precipitation and thermal reduction

Precursors with NiCO3·2Ni(OH)2·2H2O-and Fe2O3·nH2O-coated alumina,graphite and cenosphere were synthesized by precipitation using ferrous sulfate,nickel sulfate,ammonium bicarbonate,alumina,graphite and cenosphere as the main starting materials.Magnetic γ-FeNi-coated alumina,graphite and cenosphere core-shell structural microspheres were subsequently prepared by thermal reduction of the as-prepared precursors at 600℃ for 2h.Precipitation parameters,e.g.concentration of ceramic micropowders(10g/L),sulfate solution(0.2mol/L),rate of adding reactants(3mL/min)and pH value were optimized by a trial-and-error method.Powders of the precursors and the resulting coating of γ-FeNi with grain size below 40nm on alumina,graphite and cenosphere microspheres were characterized by scanning electron microscopy(SEM),energy dispersive spectroscopy(EDS)and X-ray diffraction(XRD).The magnetic properties of the nanosize γ-FeNi-coated alumina,graphite and cenosphere microspheres were measured by vibrating sample magnetometer(VSM).The results show that the core-shell structuralγ-FeNi-coated ceramic microspheres exhibited higher coercivity than pure γ-FeNi powders,indicating that these materials can be used for high-performance functional materials and devices.     

Controllable hydrothermal synthesis of star-shaped Sr3Fe2(OH)12 assemblies and their thermal decomposition and magnetic properties

Pure phase star-shaped hydrogarnet Sr₃Fe₂(OH)₁₂ assemblies were synthesized by a mild hydrothermal method (210 °C, 12 h), and the effects of the preparation conditions on the phase composition of the product were investigated. It was found that the impurity phases could be decreased or eliminated by increasing the molar ratio of Sr²⁺ to Fe³⁺, and that high temperatures favored the formation of Sr₃Fe₂(OH)₁₂ and reduced the concentration of CO₃^2–-containing byproducts. The thermal decomposition of the star-shaped Sr₃Fe₂(OH)₁₂ assemblies was examined, and the results showed that the dehydration process at higher temperatures is accompanied by the formation of SrFeO_3–δ. Above 655 °C, a solid state reaction between the SrFeO_3–δ and Sr(OH)₂ or SrCO₃ results in the formation of Sr₄Fe₃O_10–δ.The magnetic properties of the as-synthesized Sr₃Fe₂(OH)₁₂ and of samples calcined at different temperatures were assessed. A sample calcined at 575 °C exhibited greatly enhanced ferromagnetic properties, with a remanent magnetization of 1.28 emu/g and a coercivity of 4522.1 Oe at room temperature.     

Controlled synthesis of hollow magnetic Fe3O4 nanospheres: Effect of the cooling rate

The controlled synthesis of hollow magnetite (Fe₃O₄) nanospheres of varying sizes and structures was successfully obtained via a facile solvothermal process and varying cooling processes. The Fe₃O₄ nanospheres were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and superconducting quantum interference device magnetometry. The diameters of the as-synthesized nanospheres were controlled at around 500–700 nm by simply changing the cooling rate, which had an obvious influence on the morphology and magnetic properties of these Fe₃O₄ nanospheres. While a low cooling rate triggered the formation and extension of the cracks present in the Fe₃O₄ nanospheres, a sudden drop of temperature tended to favor multi-site nucleation of the crystals as well as the formation of compact and smooth hollow nanospheres with superior crystallinity and high saturation magnetization. The growth mechanism of hollow magnetite oxide nanospheres was proposed and the correlation between the structure and the magnetic properties of the hollow nanospheres was discussed, which promises the potential of the hollow nanospheres in various applications such as drug delivery and cell separation.     

Magnetically modified microbial cells： A new type of magnetic adsorbents

Microbial cells, either in free or immobilized form, can be used for the preconcentration or removal of metal ions, organic and inorganic xenobiotics or biologically active compounds. Magnetic modification of these cells enables to prepare magnetic adsorbents that can be easily manipulated in difficult-to-handle samples, such as suspensions, in the presence of external magnetic field. In this review, typical examples of magnetic modifications of microbial cells are presented, as well as their possible applications for the separation of organic xenobiotics and heavy metal ions.     

On the Cox-Merz rule for magnetic dispersions

The Cox-Merz rule can be a useful, empirical tool for relating steady and oscillatory shear flow property measurements. Here we test its applicability for magnetic dispersions. Neither the rule nor a previously published modification of it applies for the dispersions, but we demonstrate that the steady shear viscosity and the magnitude of the complex viscosity are nonetheless related. Received: 30 August 2000 Accepted: 21 December 2000     

Sedimentation acceleration of remanent iron oxide by magnetic flocculation

Sedimentation based processes are widely used in industry to separate particles from a liquid phase. Since the advent of the ＂Nanoworld＂ the demand for effective separation technologies has rapidly risen, calling for the development of new separation concepts, one of which lies in hybrid separation using the superposition of a magnetic field for magnetic particles. Possible product portfolio of such separation consists of pigment production, nanomagnetics production for electronics and bio separation, A promising step in that direction is magnetic field enhanced cake filtration, which has by now progressed from batch to continuous ooeration. In sedimentation processes in a mass force field the settling behaviour of particles strongly depends on physico-chemical properties, concentration and size distribution of the particles. By adjusting the pH, the interparticle forces, in particular the electrostatic repulsion, can be manipulated. For remanent magnetic particles such as magnetite, pre-treatment in a magnetic field could lead to a change of interparticle interactions. By magnetizing the particles apart from van der Waals attraction and electrostatic repulsion, an additional potential is induced, the magnetic attraction, which could easily dominate the other potentials and result in agglomeration in the primary minimum. By sedimentation analysis, a wide spectrum of parameters like pH, magnetic field strength and concentration have been investigated. The results show a strong increase of sedimentation velocity by magnetic flocculation of the raw suspension. This leads to a rise in throughput due to the acceleration of sedimentation kinetics by imparting a non-chemical interaction to the physico-chemical properties in the feed stream of the separation apparatus.     

Interaction forces between soft magnetic particles in uniform and non-uniform magnetic fields

The influence of the magnetization of a soft magnetic sphere on the surrounding magnetic field is measured and characterized.The interaction force between two soft magnetic particles is directly measured using an ultra precision load sensor in uniform and non-uniform magnetic fields. The interaction force largely follows an inverse fourth power law as a function of separation distance between particle centers. At small distances,the effect of magnetization of one particle on the magnetization of its adjacent particle causes the attractive（repulsive） force to be larger（smaller） than that predicted by the inverse fourth power law.The theoretical prediction based on a modified dipole model,that takes into account the coupling effect of the magnetization among soft magnetic particles,gives excellent agreement with the measured force in a uniform magnetic field.The interaction force under a non-uniform applied magnetic field can be reasonably predicted using the dipole-dipole interaction model when the local magnetic field is used to determine the magnetization.     

Magnetic modification of diamagnetic agglomerate forming powder materials

A simple method for the magnetic modification of various types of powdered agglomerate forming diamagnetic materials was developed. Magnetic iron oxide particles were prepared from ferrous sulfate by microwave assisted synthesis. A suspension of the magnetic particles in water soluble organic solvent (methanol, ethanol, propanol, isopropyl alcohol, or acetone) was mixed with the material to be modified and then completely dried at elevated temperature. The magnetically modified materials were found to be stable in water suspension at least for 2 months.     

Rapid determination of iron oxide content in magnetically modified particulate materials

Magnetically responsive composite materials have been used in interesting applications in various areas of bioscience, biotechnology, and environmental technology. In this work, a simple method to determine the amount of magnetic iron oxide nano- and microparticles attached to magnetically-modified particulate diamagnetic materials has been developed using a commercially available magnetic permeability meter. The procedure is fast and enables dry particulate magnetically modified materials to be analysed without any modification or pretreatment. We show that the magnetic permeability can be measured for materials containing up to 20% magnetic iron oxide. The magnetic permeability measurements are highly reproducible.     

Effects of magnetic field on fluidization properties of magnetic pearls

An experimental study of the influence of external magnetic field on the fluidization behavior of magnetic pearls was carried out. Magnetic pearls are a magnetic form of iron oxide that mainly consists of Fe2O3 which are recovered from a high-volume power plant fly ash from pulverized coal combustion. Due to its abundance, low price and particular physical and chemical properties, magnetic pearls can be used as a heavy medium for minerals or solid waste dry separation based on density difference. This paper introduces the properties of magnetic pearls and compares the performance of magnetic pearls fluidised bed operation with or without an external magnetic field. Experimental results show that an external magnetic field significantly improves the fluidization performance of magnetic pearls such as uniformity and stability.