Pore Structure Evolution of Silica Gel during Aging/ drying: Effect of Surface Tension

1992 ◽  
Vol 271 ◽  
Author(s):  
Ravindra Deshpande ◽  
Douglas M. Smith ◽  
C. Jeffrey Brinker

ABSTRACTTwo-step acid/base (B2) and acid/acid (A2) catalyzed silica gels have been aged in ethanol or water baths followed by various aprotic solvents with a range of surface tensions. The physical and chemical structures of xerogels dried from these aprotic solvents were studied by a series of techniques (nitrogen adsorption, elemental analysis, TGA, SAXS)and compared to the corresponding structures of low temperature (CO2) and high temperature (ethanol) aerogels. The aprotic solvents help to isolate the effects of pore fluid surface tension during drying since they do not react with the gel surface. B2 xerogels showed a linear decrease in surface area with increasing surface tension. Pore volume and pore size followed a similar trend. Micropore analysis on A2 xerogels showed an increase in micropore volume and surface area with increase in surface tension, whereas total surface area and pore volume showed an opposite trend. Thus, by varying surface tension and aging, one is able to independently control surface area, pore volume, and pore size.

Minerals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 298
Author(s):  
Chenlong Ding ◽  
Jinxian He ◽  
Hongchen Wu ◽  
Xiaoli Zhang

Ordos Basin is an important continental shale gas exploration site in China. The micropore structure of the shale reservoir is of great importance for shale gas evaluation. The Taiyuan Formation of the lower Permian is the main exploration interval for this area. To examine the nanometer pore structures in the Taiyuan Formation shale reservoirs in the Lin-Xing area, Northern Shaanxi, the microscopic pore structure characteristics were analyzed via nitrogen adsorption experiments. The pore structure parameters, such as specific surface area, pore volume, and aperture distribution, of shale were calculated; the significance of the pore structure for shale gas storage was analyzed; and the main controlling factors of pore development were assessed. The results indicated the surface area and hole volume of the shale sample to be 0.141–2.188 m2/g and 0.001398–0.008718 cm3/g, respectively. According to the IUPAC (International Union of Pure and Applied Chemistry) classification, mesopores and macropores were dominant in the pore structure, with the presence of a certain number of micropores. The adsorption curves were similar to the standard IV (a)-type isotherm line, and the hysteresis loop type was mainly similar to H3 and H4 types, indicating that most pores are dominated by open type pores, such as parallel plate-shaped pores and wedge-shaped slit pores. The micropores and mesopores provide the vast majority of the specific surface area, functioning as the main area for the adsorption of gas in the shale. The mesopores and macropores provide the vast majority of the pore volume, functioning as the main storage areas for the gas in the shale. Total organic carbon had no notable linear correlation with the total pore volume and the specific surface area. Vitrinite reflectance (Ro) had no notable correlation with the specific surface area, but did have a low “U” curve correlation with the total pore volume. There was no relationship between the quartz content and specific surface area and total pore volume. In addition, there was no notable correlation between the clay mineral content and total specific surface area and total pore volume.


2015 ◽  
Vol 22 (6) ◽  
Author(s):  
Nazile Ural

AbstractIn this study, the relationships between geotechnical index properties and the pore-size distribution of compacted natural silt and artificial soil mixtures, namely, silt with two different clays and three different clay percentages (10%, 20%, and 40%), were examined and compared. Atterberg’s limit tests, standard compaction tests, mercury intrusion porosimetry, X-ray diffraction, scanning electron microscopy (SEM) analysis, and Brunauer-Emmett-Teller specific surface analysis were conducted. The results show that the liquid limit, the cumulative pore volume, and specific surface area of artificially mixed soils increase with an increase in the percentage of clay. The cumulative pore volume and specific surface area with geotechnical index properties were compared. High correlation coefficients were observed between the specific areas and both the liquid limit and the plasticity index, as well as between the cumulative pore volume and both the clay percentage and the


2018 ◽  
Vol 6 (4) ◽  
pp. T819-T833 ◽  
Author(s):  
Yang Gu ◽  
Wenlong Ding ◽  
Min Yin ◽  
Ruyue Wang ◽  
Baocheng Jiao ◽  
...  

The marine shale in South China has great gas exploration potential, and exploration in the Sichuan Basin has been successful, but the degree of exploration remains low in the Guizhou Province. We used organic geochemical analyses (total organic carbon content and kerogen type), scanning electron microscopy (SEM), field emission SEM, nuclear magnetic resonance (NMR), X-ray diffraction analysis, and low-temperature [Formula: see text] and [Formula: see text] adsorption experimental methods to study the micropore types and pore structures and their effects on the methane adsorption capacity of organic-rich shales found in the Fenggang block in northern Guizhou Province. The results indicate that the microscopic surface porosity of the lower Cambrian Niutitang Formation ranges from 2.88% to 5.34%, with an average value of 3.86%. Based on nitrogen adsorption methods, the range of the average pore size distribution is 4.6–9.491 nm, with an average value of 6.68 nm. All of the samples exhibit significant unimodal distributions. The main pore size is less than 10 nm, and these pores account for most of the mesopore volume, which is generally consistent with the NMR results. The methane adsorption capacity of the shale samples gradually increases in the range of 0–8 MPa at 30°C and reaches a maximum at approximately 10 MPa. Positive correlations were found between the gas content and specific surface area, total pore volume, and micropore volume. These strong correlations indicate that the Niutitang Shale has a high specific surface area, a high pore volume, and narrow-diameter pores, demonstrating that it has a high gas adsorption capacity. The results of this study provide valuable information regarding the adsorption characteristics of marine shales and the factors that affect those characteristics.


2019 ◽  
Vol 10 ◽  
pp. 2217-2228 ◽  
Author(s):  
B Rabindran Jermy ◽  
Vijaya Ravinayagam ◽  
Widyan A Alamoudi ◽  
Dana Almohazey ◽  
Hatim Dafalla ◽  
...  

The combination of magnetic nanoparticles with a porous silica is a composite that has attracted significant attention for potential multifunctional theranostic applications. In this study, 30 wt % CuFe2O4 was impregnated into a matrix of monodispersed spherical hydrophilic silica (HYPS) nanoparticles through a simple dry impregnation technique. The chemotherapy drug cisplatin was loaded through electrostatic equilibrium adsorption over 24 h in normal saline solution. The presence of cubic spinel CuFe2O4 on HYPS was confirmed through powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR) and diffuse reflectance UV–vis spectroscopy (DR UV–vis) analysis. The HYPS particles showed a surface area of 170 m2/g, pore size of 8.3 nm and pore volume of 0.35 cm3/g. The cisplatin/CuFe2O4/HYPS nanoformulation showed the accumulation of copper ferrite nanoparticles on the surface and in the pores of HYPS with a surface area of 45 m2/g, pore size of 16 nm and pore volume of 0.18 cm3/g. Transmission electron microscopy (TEM) and energy dispersive X-ray (EDX) mapping analysis showed the presence of homogeneous silica particles with nanoclusters of copper ferrite distributed on the HYPS support. Vibrating sample magnetometry (VSM) analysis of CuFe2O4/HYPS showed paramagnetic behavior with a saturated magnetization value of 7.65 emu/g. DRS UV–vis analysis revealed the functionalization of cisplatin in tetrahedral and octahedral coordination in the CuFe2O4/HYPS composite. Compared to other supports such as mesocellular foam and silicalite, the release of cisplatin using the dialysis membrane technique was found to be superior when CuFe2O4/HYPS was applied as the support. An in vitro experiment was conducted to determine the potential of CuFe2O4/HYPS as an anticancer agent against the human breast cancer cell line MCF-7. The results show that the nanoparticle formulation can effectively target cancerous cells and could be an effective tumor imaging guide and drug delivery system.


1994 ◽  
Vol 346 ◽  
Author(s):  
D. E. Meyers ◽  
F. Kirkbir ◽  
H. Murata ◽  
S. Ray chaudhuri ◽  
A. Sarkar

ABSTRACTThe mechanical and microstructural properties of two-step acid-base catalyzed silica gels were examined as functions of aging time, catalyst concentration, and hydrolysis time. Cylindrical gels were prepared using Si(OC2H5)4, C2H5OH, and H2O, with HCl followed by NH3 as catalysts. Mechanical properties were obtained from three-point bend tests, and the microstructures of dried gels were analyzed using nitrogen adsorption/desorption techniques. Gel strength initially increased with aging time at 70 °C, then leveled off after about one week. When the sol was hydrolyzed for less than two hours, there were significant differences in the properties of gels catalyzed with relative molar amounts of 0.0001 and 0.0002 HCl. However, as the hydrolysis time was increased, the gels all had similar properties, independent of the amount of HC1. The amount of NH3 influenced gelation time and to a lesser extent, the strength, but had no observable effect on pore size. The two-step catalysis procedure produced gels with strength and pore size combinations intermediate to those of either single acid or base-catalyzed gels.


2014 ◽  
Vol 49 (1) ◽  
pp. 1-8
Author(s):  
US Akhtar ◽  
MK Hossain ◽  
MS Miran ◽  
MYA Mollah

Porous silica materials were synthesized from tetraethyl orthosilicate (TEOS) using Pluronic P123 (non-ionic triblock copolymer, EO20PO70O20) as template under acidic conditions which was then used to prepare polyaniline (PAni) and porous silica composites (PAnisilica) at a fixed molar ratio. These materials were characterized by nitrogen adsorption-desorption isotherm measured by Barrett-Joyner- Halenda (BJH) method and pore size distribution from desorption branch and surface area measured by the Brunauer-Emmett-Teller (BET) method, scanning electron microscopy (SEM), transmission electron microscopy (TEM), TEM-energy dispersive X-ray (EDX) and Fourier transform infrared (FT-IR) spectroscopy. The composite maintains its structure even after the polymerization and the polymer is dispersed on the inorganic matrix. The rod-like porous silica was about 1?m to 1.5 ?m long and on an average the diameter was in the range of 300- 500 nm. The SEM and TEM images show well ordered 2d hexagonal pore, high specific surface area (850 m2g-1) and uniform pore size of ca. 6.5 nm in diameter. After incorporation of PAni inside the silica pore, framework of porous silica did not collapse and the surface area of the composite was as high as 434 m2g-1 which was 5.5 time higher than our previous report of 78.3 m2g-1. Due to shrinkage of the framework during the incorporation of aniline inside the silica, the pore diameter slightly increase to 7.5 nm but still showing Type IV isotherm and typical hysteresis loop H1 implying a uniform cylindrical pore geometry. DOI: http://dx.doi.org/10.3329/bjsir.v49i1.18847 Bangladesh J. Sci. Ind. Res. 49(1), 1-8, 2014


2014 ◽  
Vol 2014 ◽  
pp. 1-13
Author(s):  
Xiaoshi Li ◽  
Yiwen Ju ◽  
Quanlin Hou ◽  
Zhuo Li ◽  
Mingming Wei ◽  
...  

The enrichment of coalbed methane (CBM) and the outburst of gas in a coal mine are closely related to the nanopore structure of coal. The evolutionary characteristics of 12 coal nanopore structures under different natural deformational mechanisms (brittle and ductile deformation) are studied using a scanning electron microscope (SEM) and low-temperature nitrogen adsorption. The results indicate that there are mainly submicropores (2~5 nm) and supermicropores (<2 nm) in ductile deformed coal and mesopores (10~100 nm) and micropores (5~10 nm) in brittle deformed coal. The cumulative pore volume (V) and surface area (S) in brittle deformed coal are smaller than those in ductile deformed coal which indicates more adsorption space for gas. The coal with the smaller pores exhibits a large surface area, and coal with the larger pores exhibits a large volume for a given pore volume. We also found that the relationship betweenSandVturns from a positive correlation to a negative correlation whenS>4 m2/g, with pore sizes <5 nm in ductile deformed coal. The nanopore structure (<100 nm) and its distribution could be affected by macromolecular structure in two ways. Interconversion will occur among the different size nanopores especially in ductile deformed coal.


2011 ◽  
Vol 239-242 ◽  
pp. 2274-2279 ◽  
Author(s):  
Ying Chun Wang ◽  
Wen Hai Huang ◽  
Ai Hua Yao ◽  
De Ping Wang

A simple method to prepare hollow hydroxyapatite (HAP) microspheres with mespores on the surfaces is performed using a precipitation method assisted with Li2O-CaO-B2O3(LCB) glass fabrication process. This research is concerned with the effect of sintering temperature on the microstructure evolution, phase purity, surface morphology, specific surface area, and porosity after sintering process. The microspheres were sintered in air atmosphere at temperatures ranging from 500 to 900 °C. The starting hollow HAP microspheres and the sintered specimens were characterized by scanning electron microscope, X-ray diffractometer, specific surface area analyzer, and Hg porosimetry, respectively. The as-prepared microspheres consisted of calcium deficient hydroxyapatite. The results showed that the as-prepared hollow HAP microspheres had the highest specific surface areas, and the biggest total pore volume. The pore size distribution of the as-prepared hollow HAP microspheres were mainly the mesopores in the range of 2~40 nm. The specific surface area and total pore volume of hollow HAP microspheres decreased with increasing sintering temperature. Whereas the mean pore size increased with increasing sintering temperature. It showed that at 700°C, Ca-dHAP decomposes into a biphasic mixture of HAP and β-calcium phosphate(TCP).


1988 ◽  
Vol 121 ◽  
Author(s):  
Gregory C. Frye ◽  
Antonio J. Ricco ◽  
Stephen J. Martin ◽  
C. Jeffrey Brinker

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.


2017 ◽  
Vol 733 ◽  
pp. 36-41
Author(s):  
Edidiong Okon ◽  
Habiba Shehu ◽  
Edward Gobina

In this study, esterification of lactic acid and ethanol to produce ethyl lactate using different cation-exchange resin catalysts was performed at 100 °C. The catalysts used for the esterification process were amberlyst 16 and dowex 50W8x cation-exchange resins. Two simplified mechanisms based on Langmuir-Hinshelwood model were employed to describe the components that adsorbed most on the surface of the catalysts. Fourier Transform Infrared (Nicolet iS10 FTIR) was employed to verify the rationality of the mechanisms. FTIR of the esterification product reflected C=O, H=O and C=C bonds on the spectra confirming water and ethanol as the most adsorbed components. The kinetic study of the retention time and the peak areas of the esterification produced with the different catalysts were compared using an autosampler gas chromatography/mass spectrometry (autosampler GC-MS). The chromatogram of the esterification product catalysed by amberlyst 16 showed a faster elution at 1.503 mins with the peak area of 1229816403 m2 in contrast to the dowex 50W8x. The BET surface area and BJH pore size distribution of the resin catalysts were determined using liquid nitrogen adsorption (Quantachrome, 2013) at 77 K. The BET surface area results of amberlyst 16 resin catalysts was found to be 1.659m2/g compared to 0.1m2/g for the dowex 50W8x. The BJH results of the catalysts exhibited a type IV isotherm with hysteresis confirming that the materials were mesoporous with pore size in the region of 2 – 50 nm.


Sign in / Sign up

Export Citation Format

Share Document