Porous Solids of Boron Phosphate, Aluminum Phosphate, and Silicon Phosphate

1994 ◽  
Vol 371 ◽  
Author(s):  
K. B. Babb ◽  
D. A. Lindquist ◽  
S. S. Rooke ◽  
W. E. Young ◽  
M. G. Kleve
Keyword(s):  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Total Pore Volume ◽  
Aluminum Phosphate ◽  
Porous Solids ◽  
Gel Point ◽  
Average Pore ◽  
Average Pore Radius ◽  
Surface Areas

AbstractAnhydrous sol-gel condensation of triethyl phosphate [(CH3CH2O)3PO] with boron trichioride (BCl3), triethyl aluminum [(CH3CH2)3Al] or silicon tetrachloride [SiCI4] in organic solvents led to rigid gels. The pore fluid of the gels was removed under supercritical conditions in a pressurized vessel to form porous solids. The condensation chemistry prior to the gel point was monitored by solution 1H, 13C, 31P, and 11B NMR. The materials were then calcined at progressively higher temperatures to produce high surface area phosphates. Nitrogen gasphysisorption was used to determine the surface areas, total pore volume, and average pore radius of the products. FT-IR was used to determine functional groups in the materials. The microstructure was also examined by scanning electron microscopy.

Pyrolysis of Organosilicon Gels to Silicon Carbide

1986 ◽  
Vol 73 ◽  
Author(s):  
Joseph R. Fox ◽  
Douglas A. White ◽  
Susan M. Oleff ◽  
Robert D. Boyer ◽  
Phyllis A. Budinger
Keyword(s):  
Silicon Carbide ◽  
Surface Area ◽  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Carbon Chain ◽  
Carbon Chain Length ◽  
Pyrolysis Products ◽  
Surface Areas ◽  
Physical Measurements

AbstractSol-gel precursors to silicon carbide have been prepared using trifunctional chloro and alkoxysilanes which contain both the silicon and carbon necessary for SiC formation. Crosslinked gels having the ideal formula [RSiO1 5].]n have been synthesized by a hydrolysis/condensation scheme for a series of saturated and unsaturated R groups. The starting gels have been characterized by a variety of elemental analysis, spectroscopic and physical measurements including IR. XRD. TGA.. surface area and pore volume. A particularly powerful method for characterizing these gels is the combination of 13C and 29 Si solid state NMR which can provide information about the degree of crosslinking as well as residual hydroxy/alkoxy content.The controlled pyrolysis of these gels has been used to prepare silicon carbide-containing ceramic products with surface areas in excess of 600m2/gm. The pyrolysis products are best described as a partially crystalline, partially amorphous mixture of β-SiC, silica and carbon. The effect of carbon chain length and the degree of unsaturation in the R group on the composition and surface area of the product has been determined. The origin of the high surface area of the pyrolysis products has been identified and its implications on potential uses of these materials is discussed.

Surfactant-Templated Synthesis of Modified Porous Clay Heterostructure (PCH)

2008 ◽  
Vol 55-57 ◽  
pp. 317-320 ◽  
Author(s):  
K. Srithammaraj ◽  
Rathanawan Magaraphan ◽  
H. Manuspiya
Keyword(s):  
Pore Volume ◽  
Pore Diameter ◽  
Condensation Reaction ◽  
High Surface ◽  
High Surface Area ◽  
Bentonite Clay ◽  
Directed Assembly ◽  
Average Pore Diameter ◽  
Average Pore ◽  
Surface Areas

Porous Clay Heterostructures (PCHs) have been prepared by the surfactant-directed assembly of mesostructured silica within the two-dimensional interlayer galleries of clays. The PCH is an interesting material to use as entrapping system such as ethylene scavenger, owing to its high surface area with uniform and specific pore size. In the present work, the PCH was synthesized within the galleries of Na-bentonite clay by the polymerization of tetraethoxysilane (TEOS) in the presence of surfactant micelles. In addition, a mesoporous clay with organic-inorganic hybrid (HPCH) is modified via co-condensation reaction of TEOS with methyltriethoxysilane (MTS) to enhance hydrophobicity of PCH material for entrapping system. According to pore characterization, PCHs have surface areas of 421-551 m2/g, an average pore diameter in the supermicropore to small mesopore range of 4.79-5.02 nm, and a pore volume of 0.57-0.66 cc/g while HPCHs have surface areas of 533-966 m2/g, an average pore diameter of 4.28-6.38 nm, and a pore volume of 0.42-0.77cc/g.

Imaging organic aerogels at the molecular level

1991 ◽  
Vol 49 ◽  
pp. 418-419
Author(s):  
G.C. Ruben ◽  
R.W. Pekala
Keyword(s):  
Pore Size ◽  
High Surface ◽  
Sol Gel ◽  
Acoustic Properties ◽  
Porous Solids ◽  
Dense Matrix ◽  
High Porosity ◽  
Microporous Material ◽  
Surface Areas ◽  
Organic Aerogels

The sol-gel polymerization of metal alkoxides or certain multifunctional organic monomers leads to the formation of highly crosslinked, transparent gels. If the solvent is simply evaporated from the pores of these gels, large capillary forces are exerted, and a collapsed structure known as a xerogel is formed. In order to preserve the gel skeleton, it is necessary to remove the the aforementioned solvent under supercritical conditions. The low density, microporous material that results from this operation is known as an aerogel. Aerogels have an ultrafine cell/pore size (< 500 Å), connected porosity, high surface areas (400-1000 m2/g), and an ultrastructure composed of interconnected colloidal-like particles or polymeric chains with characteristic dimensions of 100 Å. This ultrastructure is responsible for the unique optical, thermal, and acoustic properties of aerogels. For example, the ultrafine cell/pore size minimizes light scattering; and thus, aerogels are transparent porous solids. The high porosity of aerogels makes them excellent insulators with their thermal conductivity being approximately 100X lower than that of the fully dense matrix. Finally, the aerogel skeleton is responsible for the low sound velocities observed in these materials (i.e. 100-300 m/sec).

Inorganic and Organic Aerogels

MRS Bulletin ◽  
1990 ◽  
Vol 15 (12) ◽  
pp. 30-36
Keyword(s):  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Visible Spectrum ◽  
Supercritical Drying ◽  
Porous Solids ◽  
Metal Alkoxides ◽  
Open Cell Foams ◽  
Sol Gel Transition ◽  
Organic Aerogels

Aerogels are a special class of open-cell foams derived from the supercritical drying of highly cross-linked inorganic or organic gels. These materials have ultrafine cell/pore sizes (less than 1,000 Å), continuous porosity, high surface area (400–1000 m2/g), and a microstructure composed of interconnected colloidal-like particles or polymeric chains with characteristic diameters of 100 Å. This microstructure is responsible for the unusual optical, acoustic, thermal, and mechanical properties of aerogels. For example, aerogels can be prepared as transparent, porous solids because their ultrafine cell/pore size minimizes light scattering in the visible spectrum. Figure 4.1 shows the different aerogels that will be discussed in this article.The hydrolysis and condensation of metal alkoxides is the most common synthetic route for the formation of inorganic aerogels. Inorganic aerogels have been prepared from monomers such as tetraisopropoxy titanate, aluminum secbutylate, and zirconium isopropoxide. Nevertheless, the majority of scientific research has concentrated on the sol-gel polymerization of tetramethoxysilane (TMOS), or the less toxic tetraethoxysilane (TEOS). The resultant silica aerogels are being investigated for applications ranging from window insulation to the collection of hypervelocity partis cles in space.The sol-gel polymerization of a multifunctional monomer in solution, leading to the formation of an aerogel, is not unique to metal alkoxides. Organic reactions that proceed through a sol-gel transition have been discovered recently.

scholarly journals Synthesis of Functionalized Silica from Rice Husks Containing C-I End Group

2019 ◽  
Vol 16 (4) ◽  
pp. 0886 ◽  
Author(s):  
Sobh Et al.
Keyword(s):  
Sodium Silicate ◽  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Functionalized Silica ◽  
X Ray Diffraction ◽  
One Pot ◽  
Average Pore ◽  
Xps Spectra ◽  
Atomic Force

In this paper, we have extracted Silica from rice husk ash (RHA) by sodium hydroxide to produce sodium silicate. 3-(chloropropyl)triethoxysilane (CPTES) functionalized with sodium silicate via a sol-gel method in one pot synthesis to prepare RHACCl. Chloro group in compound RHACCl replacement in iodo group to prepere RHACI. The FT-IR clearly showed absorption band of C-I at 580 cm-1. Functionalized silica RHACI has high surface area (410 m2/g) and average pore diameter (3.8 nm) within mesoporous range. X-ray diffraction pattern showed that functionalized silica RHACI has amorphous phase .Thermogravemitric analysis (TGA) showed two decomposition stages and SEM morphology of RHACI showed that the particles have irregular shape. Atomic force microscope (AFM) technique was proved that the RHACI  has a nanostructure The XPS spectra of I 3d for all the studied surfaces are presented in the peak located at 618.5 eV binding energy was associated with C–I bond.

Preparation and Characterization of Aerogel-Based Carbon Nanocomposites

1994 ◽  
Vol 349 ◽  
Author(s):  
Wanqing Cao ◽  
Xian Yun Song ◽  
Arlon J. Hunt
Keyword(s):  
Elevated Temperatures ◽  
High Surface ◽  
Sol Gel ◽  
Average Particle Size ◽  
High Surface Area ◽  
Porous Solids ◽  
Average Particle ◽  
Infrared Transmission ◽  
Hydrocarbon Gases ◽  
Original Weight

ABSTRACTAerogels are highly porous solids prepared by sol-gel processing and supercritical evacuation. Because of their high surface area, aerogels can be used as an effective catalyst for the thermal decomposition of many gaseous compounds. A variety of hydrocarbon gases have been chosen to deposit carbon in the aerogel matrix, with the deposition temperature varying from 500° to 850°C depending on the hydrocarbon used. The amount of carbon that can be deposited in the aerogel is surprisingly large, reaching up to 10 times the original weight after extensive deposition using acetylene. Overall, the aerogel composites prepared have a uniform microstructure with the average particle size in the nanometer range. In addition, we have observed some interesting graphitic structures including carbon nanotubes and rings of various shapes. Carbon deposited in the aerogel can reduce infrared transmission of the material as well as volume shrinkage at elevated temperatures, thereby improving its thermal performance.

Spectroscopic Characterization of Mixed Titania-Silica Xerogel Catalysts

1999 ◽  
Vol 590 ◽  
Author(s):  
MA Holland ◽  
DM Pickup ◽  
G Mountjoy ◽  
SC Tsang ◽  
GW Wallidge ◽  
...  
Keyword(s):  
Catalytic Activity ◽  
Pore Structure ◽  
Surface Area ◽  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Silica Xerogel ◽  
Test Reaction ◽  
Saxs Data ◽  
Surface Areas

ABSTRACTThe synthesis of high surface area (TiO2)0.18(SiO2)0.82xerogels has been achieved using the sol-gel route. Heptane washing was used before the drying stage to minimise capillary pressure and hence preserve pore structure and maximise the surface area. The as-prepared xerogels were tested for their catalytic activity using the epoxidation of cyclohexene with tert-butyl hydrogen peroxide (TBHP) as a test reaction. Surface areas up to 450 m2g-1 were achieved with excellent selectivities and reasonable percent conversions. SAXS data has identified that heptane washing during drying, in general, results in a preservation of the pore structure, and produces more effective catalysts with higher surface areas and larger pore diameters. Fr-IR spectroscopy has revealed that the catalytic activity is dependant upon the number of Si-O-Ti linkages, inferring intimate mixing of the precursors at the atomic level. XANES data reveals the presence of reversible 4/6-fold Ti sites that are thought to be ‘active’ catalytic sites. The most effective catalyst was produced with a calcination temperature of 500°C, and a heating rate of 5 °Cmin-l

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