Characterization of the Surface Area and Porosity of Sol-Gel Films Using Saw Devices

1988 ◽  
Vol 121 ◽  
Author(s):  
Gregory C. Frye ◽  
Antonio J. Ricco ◽  
Stephen J. Martin ◽  
C. Jeffrey Brinker
Keyword(s):  
Pore Size ◽  
Surface Area ◽  
Adsorption Isotherms ◽  
Sol Gel ◽  
Film Surface ◽  
Nitrogen Adsorption ◽  
Porous Films ◽  
Pore Size Distributions ◽  
Test Film ◽  
Sol Gel Films

ABSTRACTA novel technique for accurately obtaining nitrogen adsorption isotherms on thin porous films has been developed. These isotherms are useful for characterizing the surface area and pore size distribution of porous samples. The sensitivity to adsorbed nitrogen is increased by several orders of magnitude over conventional techniques by forming the test film on the substrate of a surface acoustic wave (SAW) device. This device functions as a microbalance able to detect less than 100 pg/cm2 of film. Surface areas and pore size distributions calculated from adsorption isotherms obtained with this technique on silicate sol-gel films are compared to those for bulk samples prepared from similar sol-gel solutions.

scholarly journals Comparison of Nitrogen Adsorption and Mercury Penetration Results. Pore Size Distributions for a Series of Mo-A12O3 Catalysis with Increasing MoO3 Content

1987 ◽  
Vol 4 (1-2) ◽  
pp. 87-104 ◽  
Author(s):  
Bruce D Adkins ◽  
Jill B. Heink ◽  
Burtron H. Davis
Keyword(s):  
Pore Size ◽  
Surface Area ◽  
Three Dimensional ◽  
Nitrogen Adsorption ◽  
Bet Surface Area ◽  
Size Distributions ◽  
Electron Microscopic ◽  
Pore Size Distributions ◽  
Electron Microscopic Data ◽  
Penetration Data

Scanning electron microscopic data, X-ray diffraction patterns and porosity measurements are consistent with a structure for an Mo-A12O3 catalyst series containing a single surface layer of Mo up to the point where the Mo loadings exceed the amount required for a monolayer. For greater Mo loadings than required for a monolayer, three dimensional orthorhombic MoO3 is also present. The cumulative pore volume, on an alumina basis, does not appear to be significantly altered by MoO3 loadings up to about 15 wt.%. The BET surface area, on an alumina basis, remains constant with Mo loading. However, the apparent surface area calculated from mercury penetration data decreases with Mo loading. For these materials with cylindrical pores, the Broekhoff-deBoer model for the calculation of pore size distributions produced closer agreement to the mercury penetration pore size distribution. This is in contrast to materials composed of nonporous spheres where the Broekhoff-deBoer model provided poorer agreement to mercury penetration results than either the Cohan or a packed sphere model. The results show that, within a factor of two the pore size distributions calculated from nitrogen adsorption and mercury penetration data are comparable.

Article

1998 ◽  
Vol 76 (4) ◽  
pp. 382-388 ◽  
Author(s):  
Jack M Miller ◽  
David Wails ◽  
J Stephen Hartman ◽  
Karla Schebesh ◽  
Jennifer L Belelie
Keyword(s):  
Catalytic Activity ◽  
Pore Size ◽  
Zinc Chloride ◽  
Sol Gel ◽  
Nitrogen Adsorption ◽  
Potassium Fluoride ◽  
Physical Structure ◽  
Alkylation Reaction ◽  
Size Distributions ◽  
Pore Size Distributions

Novel mesoporous silicas have been prepared via a sol-gel route involving fluoride-catalyzed hydrolysis of tetraethylorthosilicate (TEOS). Incorporation of zinc chloride by sol-gel synthesis gives a range of mesoporous materials with significantly higher catalytic activity than the commercially available catalyst, Clayzic, in a model Friedel-Crafts alkylation reaction. The dependence of catalytic activity and physical structure on the amounts of solvent, water, zinc chloride, and potassium fluoride used in the preparation are explored, and the materials have been further characterized by nitrogen adsorption to determine surface areas, total pore volumes, and pore-size distributions and by 29Si and 19F MAS NMR spectroscopy. The most active catalysts generally have the highest total pore volumes, with pore-size distributions larger than 8 nm.Key words: sol-gel, Friedel-Crafts, Clayzic, silica.

The Influence of TiO2 Photoanode Morphology for Scattering Enhanced Properties of Dye-Sensitized Solar Cell

2013 ◽  
Vol 667 ◽  
pp. 425-434 ◽  
Author(s):  
Mohd Hanapiah Abdullah ◽  
Ismail Lyly Nyl ◽  
Mohamed Zahidi Musa ◽  
Mohamad Rusop Mahmood
Keyword(s):  
Pore Size ◽  
Surface Area ◽  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Tio2 Electrode ◽  
Pore Size Distributions ◽  
Tio2 Sol ◽  
Micron Size ◽  
Enhanced Properties

Effect of PEG on the TiO2 electrode morphology for scattering enhanced properties of the modified paste containing TiO2 sol-gel mixed with Degussa P-25 were investigated. The high surface area of the scattering centres in this study were formed by using nano size particles ascribed from TiO2 sol-gel while the sub-micron size particles were utilized from the reaction of PEG on the Degussa P-25 particles. The pore size distributions were tailored by varying the PEG content in the fabricated electrodes. Higher surface area with adequate pore size of P30 electrode has contributed to higher JSC and efficiency (η) of 11.35450 mA/cm2 and 2.479624 %, respectively. Photocurrent action spectra of IPCE of the DSSC exhibit the maximum of 42 % at 550 nm correspond to the P30 TiO2 electrode. Overall results suggest that the incorporation of TiO2 sol-gel component mixed with TiO2 paste derived from commercially available nanopowder could enhance surface area as well as serves for better light scattering effect, while PEG addition creates adequate pore size distribution to maximize the dye adsorbed on the TiO2 electrode.

Growth and characterization of semiconductor nanoparticles in porous sol-gel films

1997 ◽  
Vol 12 (11) ◽  
pp. 3115-3126 ◽  
Author(s):  
E. J. C. Dawnay ◽  
M. A. Fardad ◽  
Mino Green ◽  
E. M. Yeatman
Keyword(s):  
Heat Treatment ◽  
Aqueous Solution ◽  
Pore Size ◽  
Sol Gel ◽  
Passive Films ◽  
Silica Layer ◽  
Crystallite Growth ◽  
Porous Films ◽  
Sol Gel Films

Two methods for the preparation of semiconductor doped sol-gel films, for applications in nonlinear optics, have been studied and compared. In the first, porous films are spun from sols containing the cation precursor, and then reacted with H2S gas, and in the second, the cation is adsorbed onto the pore surfaces of passive films from aqueous solution before the gas reaction. Extensive results for CdS doping are given, and preliminary results are reported for other semiconductor species. It is shown that a sputtered silica layer can seal the structure to allow further heat treatment without loss of dopant. The effects of heat treatment of doped films are described, and the limitation of crystallite growth by pore size is shown.

Texture Evaluation of Sol-Gel Derived Mesoporous Bioactive Glass

2013 ◽  
Vol 284-287 ◽  
pp. 230-234
Author(s):  
Yu Jen Chou ◽  
Chi Jen Shih ◽  
Shao Ju Shih
Keyword(s):  
Surface Area ◽  
Calcination Temperature ◽  
High Surface ◽  
Sol Gel ◽  
High Surface Area ◽  
Nitrogen Adsorption ◽  
Bioactive Glasses ◽  
Transmission Electron ◽  
Sol Gel Process ◽  
Adsorption Desorption

Recent years mesoporous bioactive glasses (MBGs) have become important biomaterials because of their high surface area and the superior bioactivity. Various studies have reported that when MBGs implanted in a human body, hydroxyl apatite layers, constituting the main inorganic components of human bones, will form on the MBG surfaces to increase the bioactivity. Therefore, MBGs have been widely applied in the fields of tissue regeneration and drug delivery. The sol-gel process has replaced the conventional glasses process for MBG synthesis because of the advantages of low contamination, chemical flexibility and lower calcination temperature. In the sol-gel process, several types of surfactants were mixed with MBG precursor solutions to generate micelle structures. Afterwards, these micelles decompose to form porous structures after calcination. Although calcination is significant for contamination, crystalline and surface area in MBG, to the best of the authors’ knowledge, only few systematic studies related to calcination were reported. This study correlated the calcination parameters and the microstructure of MBGs. Microstructure evaluation was characterized by transmission electron microscopy and nitrogen adsorption/desorption. The experimental results show that the surface area and the pore size of MBGs decreased with the increasing of the calcination temperature, and decreased dramatically at 800°C due to the formation of crystalline phases.

scholarly journals Comparison of Nitrogen Adsorption and Mercury Penetration Results: II. Pore size Distributions Calculated from Type IV Isotherm Data

1988 ◽  
Vol 5 (3) ◽  
pp. 168-190 ◽  
Author(s):  
Bruce D. Adkins ◽  
Burtron H. Davis
Keyword(s):  
Pore Size Distribution ◽  
Pore Size ◽  
Size Distribution ◽  
Nitrogen Adsorption ◽  
Type Iv ◽  
Pore Size Distributions ◽  
Nitrogen Desorption ◽  
The Difference ◽  
Penetration Data ◽  
Packed Sphere

The pore distributions calculated from nitrogen desorption and from mercury penetration data are similar for the four materials utilized in this study. While there are small differences in the distributions calculated using different models (Cohan. Foster or Broekhoff-deBoer) with nitrogen adsorption or desorption isotherm data, all three show reasonable agreement with distributions calculated from mercury penetration data. Frequently practical catalysts have such a broad pore size distribution that neither method alone is adequate to measure the total pore size range. The present results suggest a direct comparison, without recourse to a scaling factor, is appropriate when comparing results from the two methods even though the pore size distribution maximum may vary by at least 50% depending upon the model chosen for the calculation. Better agreement may be obtained between the two experimental techniques by adjusting either the nitrogen adsorption data using a packed sphere model or the mercury penetration data by an earlier reported correction ratio. The difference between the two methods becomes less than 20% when a correction procedure is used; however, further studies are needed to define the range of material shaped that these procedures are applicable to.

Preparation, characterization, and micropatterning of laser-dye-doped sol-gel films

2002 ◽  
Vol 17 (8) ◽  
pp. 2095-2098 ◽  
Author(s):  
A. Arena ◽  
S. Patanè ◽  
G. Saitta ◽  
G. Rizzo ◽  
S. Galvagno ◽  
...  
Keyword(s):  
Soft Lithography ◽  
Sol Gel ◽  
Film Surface ◽  
Optical Microscope ◽  
Infrared Range ◽  
Patterned Films ◽  
A Charge ◽  
Sol Gel Films ◽  
Sol Gel Synthesis ◽  
Micrometer Scale

Planar thin films of dye-doped silica were prepared by sol-gel synthesis. The optical properties of the films were characterized by transmittance measurements in the visible-infrared range and by photoluminescence. Micropatterns whose feature size was on the order of 2.4 μm, were imprinted on the film surface by a simple soft lithography approach. An optical microscope interfaced to a charge-coupled device camera was used to image the imprinted patterns and to analyze the patterned films photoluminescence. A sensitive spectral narrowing of the emission, which occurred only in micropatterned films, was attributed to the lateral confinement of the luminescence due to the micrometer-scale modulation of refractive index produced by the embossing procedure.

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