A novel method to synthesize amorphous silica-alumina materials with mesoporous distribution without using templates and pore-regulating agents

In this study, a novel sol-gel method is used to synthesize amorphous silica-alumina materials with a narrow mesoporous distribution and various Si/Al molar ratios without using any templates and pore-regulating agents. During the preparation procedure, only inexpensive inorganic salts were used as raw materials, instead of expensive and harmful alkoxides. The precursor sol was dried at room temperature in a vacuum box kept at 60 mmHg until it began to form the gel. The results of a nitrogen sorption experiment indicate that the synthesized materials with different Si/Al molar ratios have similar mesoporous distributions (within 2-12 nm). Moreover, it was found that the material's pore size distribution remains at a similar value during the heat treatment from room temperature to 550 degreesC. On the basis of the nitrogen sorption, TEM, and AFM characterization results, a formation mechanism of mesopores which accounts for the experimental data is also suggested. This suggested mechanism involves rearrangement of the primary particles during the drying process to form the precursors of the similarly sized mesopores. The synthesized materials were characterized by XRD, thermal analysis (TG/DTA), Al-27 and Si-29 MAS NMR spectroscopy, SEM, TEM, and AFM. The results of Al-27 and 29Si MAS NMR indicate that the distribution of silicon and aluminum in the synthesized materials is more uniform and homogeneous than that in the mixed oxides prepared via the traditional sol-gel method even at high alumina contents. The type and density of the acid sites were studied using pyridine adsorption-desorption FTIR spectroscopy. It was shown that the acidity of the synthesized materials is higher than that of the silica-alumina materials prepared by conventional methods.

Acid catalyzed synthesis of ordered bifunctionalized mesoporous organosilicas with large pore

Thiol-functionalized mesoporous ethane-silicas with large pore were synthesized by co-condensation of 1,2-bis(trimethoxy-sily)ethane (BTME) with 3-mercaptopropyltrimethoxysilane (MPTMS) using nonionic oligomeric polymer C1H (OCH(2)-CH(2))(10)OH (Brij-76) or poly(alkylene oxide) block copolymer (P123) as surfactant in acidic medium. The results of powder X-ray diffraction (XRD), nitrogen gas adsorption, and transmission electron microscopy (TEM) show that the resultant materials have well-ordered hexagonal mesoscopic structure with uniform pore size distributions. (29)Si MAS NNR, (13)C CP-MAS NMR. FT-IR, and UV Raman spectroscopies confirm the attachment of thiol functionalities in the mesoporous ethane-sificas. The maximum content of the attached thiol group (-SH) in the mesoporous framework is 2.48mmol/g. The ordered mesoporous materials are efficient Hg(2+) adsorbents with almost every -SH site accessible to Hg(2+). In the presence of various kinds of heavy metal ions such as Hg(2+), Cd(2+), Zn(2+), Cu(2+) and Cr(3+), the materials synthesized using poly(alkylene oxide) block cooollxmier (Pluronic 123) g(2+), as surfactant show almost similar affinity to Hg(2+), Cd(2+), and Cr(3+), while the materials synthesized using ofigomeric polymer C(18)H(37)(OCH(2)CH(2))(10)OH (Brij-76) as surfactant exhibit high selectivity to Hg(2+). (C) 2004 Elsevier Inc. All rights reserved.

Permeability of Fractal Porous Media by Monte Carlo Simulations

The permeability of the fractal porous media is simulated by Monte Carlo technique in this work. Based oil the fractal character of pore size distribution in porous media, the probability models for pore diameter and for permeability are derived. Taking the bi-dispersed fractal porous media as examples, the permeability calculations are performed by the present Monte Carlo method. The results show that the present simulations present a good agreement compared with the existing fractal analytical solution in the general interested porosity range. The proposed simulation method may have the potential in prediction of other transport properties (such as thermal conductivity, dispersion conductivity and electrical conductivity) in fractal porous media, both saturated and unsaturated.

A porous bulk metallic glass with unidirectional opening pores

Porous Zr-based bulk metallic glass (PMG) with unidirectional opening pores is prepared by electrochemical etching of tungsten wires of the W/bulk metallic glass (BMG) composites. The porosity and pore size can be controlled by adjusting the tungsten wires. The PMG showed no measurable loss in thermal stability as compared to the monolithic Zr-based BMG by water quenching and is more ductile and softer than the pore-free counterpart. The specific surface area of the PMGs is calculated to be 0.65, 3.96, and 10.54 m(2)/kg for 20, 60, and 80 vol % porosity, respectively. (c) 2007 The Electrochemical Society.

Formation and characterization of tin oxide aerogel derived from sol-gel process based on tetra(n-butoxy)tin(IV)

Transparent and translucent SnO2 aerogels with high specific surface area (>300m(2)/g) have been prepared by sol-gel process using tetra(n-butoxy)tin(IV) as a starting compound, and supercritical drying technique for solvent extraction. Light scattering measurements reveal that the polymeric cluster size distribution in sol system is gradually broadened during sol-gel transition. SEM images show that the aerogels are made up of the cottonlike oxide agglomerates with a large number of Pores. TEM images show that these aerogels seem to be self-similar at different magnifications. Their pore size distribution is pretty wide ranging, from mesopore to macropore especially for that of translucent aerogel. (C) 2004 Elsevier B.V. All rights reserved.

Preparation and AFM characterization of self-ordered porous alumina films on semi-insulated gaas substrate

Self-ordered porous alumina films on a semi-insulated GaAs substrate were prepared in oxalic acid aqueous solutions by three-step anodization. The I-t curve of anodization process was recorded to observe time effects of anodization. Atomic force microscopy was used to investigate structure and morphology of alumina films. It was revealed that the case of oxalic acid resulted in a self-ordered porous structure, with the pore diameters of 60-70 nm, the pore density of the order of about 10(10) pore cm(-2), and interpore distances of 95-100nm. At the same time the pore size and shape change with the pore widening time. Field-enhanced dissolution model and theory of deformation relaxation combined were brought forward to be the cause of self-ordered pore structure according to I-t curve of anodization and structure characteristics of porous alumina films. (c) 2006 Elsevier Ltd. All rights reserved.

Porous ZnAl2O4 spinel nanorods doped with Eu3+: synthesis and photoluminescence

Eu3+-doped zinc aluminate (ZnAl2O4) nanorods with a spinel structure were successfully synthesized via an annealing transformation of layered precursors obtained by a homogeneous coprecipitation method combined with surfactant assembly. These spinel nanorods, which consist of much finer nanofibres together with large quantities of irregular mesopores and which possess a large surface area of 93.2 m(2) g(-1) and a relatively narrow pore size distribution in the range of 6 - 20 nm, are an ideal optical host for Eu3+ luminescent centres. In this nanostructure, rather disordered surroundings induce the typical electric-dipole emission (D-5(0) --> F-7(2)) of Eu3+ to predominate and broaden.

Preparation and AFM characterization of self-ordered porous alumina films on semi-insulated gaas substrate

Self-ordered porous alumina films on a semi-insulated GaAs substrate were prepared in oxalic acid aqueous solutions by three-step anodization. The I-t curve of anodization process was recorded to observe time effects of anodization. Atomic force microscopy was used to investigate structure and morphology of alumina films. It was revealed that the case of oxalic acid resulted in a self-ordered porous structure, with the pore diameters of 60-70 nm, the pore density of the order of about 10(10) pore cm(-2), and interpore distances of 95-100nm. At the same time the pore size and shape change with the pore widening time. Field-enhanced dissolution model and theory of deformation relaxation combined were brought forward to be the cause of self-ordered pore structure according to I-t curve of anodization and structure characteristics of porous alumina films. (c) 2006 Elsevier Ltd. All rights reserved.

Template-assisted syntheses of two novel porous zirconium methylphosphonates

Two porous zirconium methylphosphonates (designated as ZMPmi and ZMPme respectively) were synthesized by using dibutyl methylphosphonate (DBMP) as a template. Two efficient post-synthetic treatments were developed to remove the incorporated template without destroying the hybrid structures. The materials were characterized by SEM, EPMA, TG, DTA, FTIR, and NMR. Specific surface area and porosity were evaluated by BET, alpha(s)-plots and DFT methods based on N-2 adsorption-desorption isotherms. The specific surface areas of ZMPmi and ZMPme are determined to be 279 and 403 m(2) g(-1) and the maxima of pore size distributions are at 0.7 and 1.3 nm respectively. (c) 2005 Elsevier Inc. All rights reserved.

Effect of drying methods on the structure and catalytic combustion activity of Mn-substituted hexaaluminate catalysts

Conventional oven drying (COD) and supercritical drying (SCD) methods were applied to the preparation of Mn-substituted hexaaluminate (BaMnA(11)O(19-alpha)) catalysts. The effect of drying methods on phase composition, specific surface area, pore structure and combustion activity of the samples was investigated. The samples obtained by SCD have higher surface area, narrower pore size distribution, and higher combustion activity than those obtained by COD.