共查询到20条相似文献,搜索用时 109 毫秒
1.
Interest in improving the optical transmission of sodium silicate-based aerogels by ambient pressure drying led to the synthesis of aerogels using a two-step sol–gel process. To produce optically transparent silica aerogel granules, NH4F (1 M) and HCl (4 M) were used as hydrolyzing and condensation catalysts, respectively. The silica aerogels were characterized by their bulk density, porosity (%), contact angle and thermal conductivity. Optical transmission of as synthesized aerogels was studied by comparing the photos of aerogel granules. Scanning electron microscopic study showed the presence of fractal structures in these aerogels. The degree of transparency in two step sol–gel process-based aerogels is higher than the conventional single step aerogels. The N2 adsorption–desorption analysis depicts that the two step sol–gel based aerogels have large surface areas. Optically transparent silica aerogels with a low density of ∼0.125 g/cc, low thermal conductivity of ∼0.128 W/mK and higher Brunauer, Emmett, and Teller surface area of ∼425 m2/g were obtained by using NH4F (1 M), HCl (4 M), and a molar ratio of Na2SiO3::H2O::trimethylchlorosilane of 1::146.67::9.46. The aerogels retained their hydrophobicity up to 500 °C. 相似文献
2.
Uzma K. H. Bangi A. Parvathy Rao H. Hirashima A. Venkateswara Rao 《Journal of Sol-Gel Science and Technology》2009,50(1):87-97
Experimental results on the physico-chemical properties of ambiently dried sodium silicate based aerogels catalyzed with various
acids are reported. The aerogels were prepared by hydrolysis and polycondensation of sodium silicate followed by subsequent
washings, surface chemical modification and ambient pressure drying using 10 various acid catalysts consisting of strong and
weak acids. The strength and concentration of acids have the major effect on the gelation of sol and hence the physico-chemical
properties of the silica aerogels. Strong acids such as HCl, HNO3 and H2SO4 resulted in shrunk (70–95%) aerogels whereas weak acids such as citric and tartaric acids resulted in less shrunk (34–50%)
aerogels. The physical properties of silica aerogels were studied by measuring bulk density, volume shrinkage (%), porosity
(%), pore volume, thermal conductivity, contact angle with water, Transmission Electron Microscopy (TEM), Atomic Absorption
Spectroscopy (AAS), Fourier Transform Infrared Spectroscopy (FTIR), Thermo Gravimetric-Differential Thermal (TG-DT) analyses
and N2 adsorption–desorption BET surface analyzer. The best quality silica aerogels in terms of low density (0.086 g/cm3), low volume shrinkage (34%), high porosity (95%), low thermal conductivity (0.09 W/m K) and hydrophobic (148°) were obtained
for molar ratio of Na2SiO3:H2O:citric acid:TMCS at 1:146.67:0.72:9.46 with 20 min gelation time. The resulting aerogels exhibited the thermal stability
up to around 420 °C. 相似文献
3.
A. Venkateswara Rao G. M. Pajonk N. N. Parvathy 《Journal of Sol-Gel Science and Technology》1994,3(3):205-217
In continuation to our earlier work on aerogels, the experimental results on the monolithicity and physical properties of silica aerogels as a function of the molar ratios of tetramethoxysilane (TMOS) precursor, catalyst (NH4OH), methanol (MeOH) solvent and water, are reported. The molar ratios of NH4OH/TMOS, MeOH/TMOS and H2O/TMOS were varied from 7.1 × 10–6 to 9.6 × 10–1, 1 to 90 and 1 to 18 respectively. It has been found that larger molar ratios of NH4OH/TMOS (10–2), MeOH/TMOS (13 to 60) and H2O/TMOS (>10) resulted in transparent but cracked aerogels, and very low molar ratios of these combinations gave monolithic but less transparent or opaque aerogels. The best quality silica aerogels, in terms of monolithicity, transparency and low density, have been obtained with TMOS:MeOH:H2O:NH4OH in the molar ratio of 1:12:4:3.7 × 10–3 respectively. The aerogels have been characterized by density, optical transmission, surface area and porosity measurements. The results have been discussed by taking into account the hydrolysis and condensation reactions, and syneresis effects. 相似文献
4.
Uzma K. H. Bangi M. S. Kavale Seungsu Baek Hyung-Ho Park 《Journal of Sol-Gel Science and Technology》2012,62(2):201-207
The successful incorporation of multiwalled carbon nanotubes (MWCNTs) into silica aerogels prepared by sol–gel method is reported
herein. Pure silica aerogels prepared using sodium silicate precursor by ambient pressure drying are so fragile that they
cannot be used easily. MWCNTs were used as reinforcements to improve the mechanical properties of silica aerogels. Results
show that inserting small amounts of MWCNTs in the gels causes enhanced dimensional stability of silica aerogels. The silica
aerogels were prepared by doping MWCNTs in silica matrix before gelation. The influence of MWCNTs on some microstructural
aspects of silica matrix has been studied using nitrogen adsorption–desorption isotherms. From SEM study it is confirmed that
the silica particles get capped on the surface of MWCNTs suggesting an enhanced toughness. Further, FTIR, Raman, EDAX, thermal
conductivity and hydrophobicity studies of these doped aerogels were carried out. By addition of MWCNTs, silica aerogels were
formed with 706 m2/g BET and 1,200 m2/g Langmuir surface areas and 149o contact angle. Low density (0.052 g/cc) and low thermal conductivity (0.067 W/m K) MWCNTs doped silica aerogels were obtained
for the molar ratio of Na2SiO3::H2O::MWCNTs::citric acid::TMCS at 1::146.67::2.5 × 10−3::0.54::9.46 respectively with improved mechanical strength. 相似文献
5.
The experimental results by using various exchanging solvents in the preparation of two step (acid and base) processed ambient
pressure dried hydrophobic silica aerogels, are reported. Silica alcogels were prepared by hydrolysis with oxalic acid and
condensation with NH4OH of ethanol diluted tetraethylorthosilicate (TEOS) precursor and hexamethyldisilazane(HMDZ) methylating agent. The exchanging
solvents used were: hexane, cyclohexane, heptane, benzene, toluene and xylene. The physical properties such as % of volume
shrinkage, density, pore volume, % of porosity, thermal conductivity, % of optical transmission, surface area, pore size distribution
and contact angle (θ) of the silica aerogels with water, were measured as a function of EtOH/TEOS molar ratios (R) for all the exchanging solvents. It was found that the physical and hydrophobic properties of the silica aerogels strongly
depend on the nature of the solvent and R. Heptane solvent resulted in highly transparent (≈90% optical transmission at 700 nm for 1 cm thick sample), low density
(≈0.060 g/cm3), low thermal conductive (≈0.070 W/m·K), high % of porosity (97%), high surface area (750 m2/g), uniform porosity and hydrophobic (θ ≈ 160°) aerogels compared to other solvents. On the otherhand, xylene resulted in aerogels with higher hydrophobicity (θ ≈ 172°) among other solvents. 相似文献
6.
A. Venkateswara Rao Uzma K. H. Bangi Sunetra L. Dhere Hiroaki Imai Hiroshi Hirashima 《Journal of Sol-Gel Science and Technology》2011,57(1):95-100
The effect of iron acetylacetonate on the physico-chemical properties of waterglass based silica aerogels by ambient pressure
drying has been investigated. Doping the gels with iron acetylacetonat (FeAA) facilitates in the diminution of the density
of the aerogels. The well established silica network provides effective confinement of FeAA nanoparticles which resists the
collapse of silica network during ambient pressure drying. Therefore, in the present paper, the effects of FeAA on the physico-chemical
properties of the aerogels have been studied by varying the FeAA:Na2SiO3 molar ratio from 3 × 10−4 to 6 × 10−4. The aerogels were prepared via ambient pressure drying and characterized by the bulk density, thermal conductivity and water
contact angle. The aerogel’s surface morphology, elemental analysis and pore structure were characterized by means of EDAX
and FTIR, TEM and N2 adsorption- desorption analyzer. The high temperature hydrophobicity of these aerogels was checked by heating them in temperature
controlled furnace. Silica aerogels with low density ~0.050 g/cc have been obtained using the molar ratio of Na2SiO3:H2O:FeAA:Citric acid:TMCS at 1:146.67:3 × 10−4:0.54:9.46, respectively. EDAX and FTIR studies show that the iron species are entrapped in the mesoporous framework and not
took part in the bonding with silica. 相似文献
7.
The effect of four ionic liquids on the porous texture of silica aerogels synthesized from mixed tetramethoxysilane and methyltrimethoxysilane
and dried by the CO2 supercritical method, was studied. Two of these ionic liquids were composed of BF4
− anions while the other two included Cl− anions. The synthesis of gels from ionic liquids did not require another acidic catalyst for silica hydrolysis, nor a basic
catalyst for silica condensation. These aerogels were compared with traditional aerogels made according to a double step catalysis,
which first involved hydrolysis with HCl followed by condensation with pH 9 Tris HCl buffer. Gel mass analysis and thermogravimetric
data showed that, when the initial molar of ionic liquid to Si was 1.58, only ~2% (by mass) of the initial ionic liquids consisting
of BF4
− anions and ~10% (by mass) of ionic liquids containing Cl− anions, remained in the aerogels after supercritical drying. Moreover, X-ray diffraction confirmed that in ionic liquids
based on BF4
− anions, evaporation of the volatile components before supercritical CO2 drying led to the formation of regularly ordered mesopores. 相似文献
8.
The rapid growth of CO2 emissions in the atmosphere has attracted great attention due to the influence of the greenhouse effect. Aerogels’ application for capturing CO2 is quite promising owing to their numerous advantages, such as high porosity (~95%); these are predominantly mesoporous (20–50 nm) materials with very high surface area (>800 m2∙g−1). To increase the CO2 level of aerogels’ uptake capacity and selectivity, active materials have been investigated, such as potassium carbonate, K2CO3, amines, and ionic-liquid amino-acid moieties loaded onto the surface of aerogels. The flexibility of the composition and surface chemistry of aerogels can be modified intentionally—indeed, manipulated—for CO2 capture. Up to now, most research has focused mainly on the synthesis of amine-modified silica aerogels and the evaluation of their CO2-sorption properties. However, there is no comprehensive study focusing on the effect of different types of aerogels and modification groups on the adsorption of CO2. In this review, we present, in broad terms, the use of different precursors, as well as modification of synthesis parameters. The present review aims to consider which kind of precursors and modification groups can serve as potentially attractive molecular-design characteristics in promising materials for capturing CO2. 相似文献
9.
In the present paper, we report the synthesis of tetrapropoxysilane (TPOS)-based silica aerogels with high surface area and large pore volume. The silica aerogels were prepared by a two-step sol-gel process followed by surface modification via a simple ambient pressure drying approach. In order to minimize drying shrinkage and obtain hydrophobic aerogels, the surface of the alcogels was modified using trichloromethylsilane as a silylating agent. The effect of the sol-gel compositional parameters on the polymerization of aerogels prepared by TPOS, one of the precursors belonging to the Si(OR)4 family, was reported for the first time. The oxalic acid and NH4OH concentrations were adjusted to achieve good-quality aerogels with high surface area, low density, and high transparency. Controlling the hydrolysis and condensation reactions of the TPOS precursor turned out to be the most important factor to determine the pore characteristics of the aerogel. Highly transparent aerogels with high specific surface area (938 m2/g) and low density (0.047 g/cm3) could be obtained using an optimized TPOS/MeOH molar ratio with appropriate concentrations of oxalic acid and NH4OH. 相似文献
10.
Rao A. Venkateswara Kulkarni M.M. Pajonk G.M. Amalnerkar D.P. Seth T. 《Journal of Sol-Gel Science and Technology》2003,27(2):103-109
The hydrophobic property is one of the most important requirements for the long-term use of silica aerogels for transparent or translucent window insulation and opaque thermal insulating systems. Therefore, the present paper deals with the synthesis and characterization of hydrophobic silica aerogels using trimethylethoxysilane (TMES) as a co-precursor. Silica sol was prepared by keeping the molar ratio of tetramethoxysilane (TMOS) precursor, methanol (MeOH) solvent, water (H2O) and ammonia (NH4OH) catalyst constant at 1:12:4:3.7 × 10–3 respectively throughout the experiments and the TMES/TMOS molar ratio (A) was varied from 0 to 2.35. The resulting silica alcogels were dried supercritically by high-temperature alcohol solvent extraction. Hydrophobicity of the aerogels was tested by measuring the percentage of water adsorbed by the aerogels after putting them directly on the surface of water under humid conditions. Alternately, the hydrophobicity was also tested by contact angle measurements. It was found that as the A value increased, the hydrophobicity of the aerogels increased but the optical transmission decreased from 93% to less than 5% in the visible range. The thermal stability of the aerogels was studied in the temperature range from 25 to 400°C. The hydrophobic nature of the aerogels was maintained up to a temperature of 300°C. The aerogels were characterized by infrared spectroscopy, optical transmittance, Scanning electron microscopy (SEM) and contact angle measurements. The results have been discussed by taking into account the hydrolysis and condensation mechanisms. 相似文献
11.
P. R. Aravind P. Shajesh P. Mukundan K. G. K. Warrier 《Journal of Sol-Gel Science and Technology》2009,52(3):328-334
Ambient pressure drying has been carried out for the synthesis of silica–titania aerogel monoliths. The prepared aerogels
show densities in the range 0.34–0.38 g/cm3. The surface area and pore volume of these mixed oxide aerogels are comparable to those of the supercritically dried ones.
The surface area for 5wt% titania aerogel has been found to be as high as 685 m2/g with a pore volume of 2.34 cm3/g and the 10wt% titania aerogel has a surface area of 620 m2/g with a pore volume of 2.36 cm3/g. Some gels were also made hydrophobic by a surface treatment with methyltrimethoxysilane and trimethylchlorosilane. The
surface modified aerogels possess high surface areas in the range of 540–640 m2/g, and are thermally stable in terms of retaining hydrophobicity up to a temperature of 520 °C. The pore size distribution
of the aerogels clearly indicates the preservation of the aerogel structure. High Resolution Transmission Electron microscopy
has been employed to characterise the aerogels and Fourier Transform infrared spectroscopy to study the effect of titania
addition to silica and the surface modification. X-ray diffraction patterns were recorded to verify the molecular homogeneity
of the aerogel. 相似文献
12.
J. J. Calvino M. A. Cauqui G. Cifredo J. M. Rodríguez-Izquierdo H. Vidal 《Journal of Sol-Gel Science and Technology》1994,2(1-3):831-836
The influence of the preparation method on the microstructure and catalytic behavior of Rh and Ni dispersed on TiO2-SiO2 aerogels is investigated.The autoclave method has been followed to prepare titania-silica aerogels with TiO2 contents ranging between 0 and 10 mole %. These aerogels have been used as matrices to disperse catalytically active metals: Rh and Ni. The metals can be deposited by impregnation of aerogels, or alternatively, can be added into the hydrolysis water used in the synthesis of gels. The resulting catalysts present surface areas higher than 550 m2·g–1.The percentage of titania, the method followed for the introduction of the metal, and the nature of the metal itself affect both the activities and selectivities of the catalysts in the hydrogenolysis of n-butane. Thus, the presence of titania in Rh catalysts increases the activity values, and the samples prepared by impregnation present selectivities towards ethane higher than 80%. Whereas, the rhodium catalysts in which the metal has been introduced before gelling, do not orientate the reaction in favor of a definite product. For the case of Ni, it is quite frequent to obtain high selectivities towards the breakdown of the C-C terminal bonds. In summary, the preparation methods allow to modulate into very broad limits the catalytic behavior of the samples. 相似文献
13.
In the present paper the experimental results of the effect of sol-gel processing temperature on the physical properties of
the TEOS based silica aerogels are reported and discussed. The aerogels were produced by the two step sol-gel process at various
temperatures in the range of 26–70∘;C followed by supercritical drying using methanol solvent extraction. A remarkable reduction in the gelation time was observed
from three and a half days at room temperature to a mere 18 hours at 50∘;C. The best quality aerogels in terms of low density and high optical transmission were obtained for 6 hours hydrolysis time.
The aerogels were characterized by the measurements of bulk density, volume shrinkage, porosity, refractive index and optical
transmission. Monolithic aerogels with ultra low density (∼0.018 g/cm3), extremely high porosity (∼99%) and optimum optical transmission at 700 nm (∼75%) were obtained for the molar ratio of TEOS:MeOH:acidic
water:basic water at 1:99:10.42:14.58 respectively. 相似文献
14.
Ke Chen Zhihao Bao Ai Du Xiurong Zhu Jun Shen Guangming Wu Zhihua Zhang Bin Zhou 《Journal of Sol-Gel Science and Technology》2012,62(3):294-303
A rapid and facile synthesis of resorcinol/formaldehyde cross-linked silica (RF/SiO2) aerogels was carried out in one pot based on an acid-catalyzed route, instead of the previously reported base-catalyzed
ones. The gelation time was reduced to several hours at room temperature while it took several days even under heating conditions
in the base-catalyzed ones. The interpenetrating network of RF/SiO2 aerogels showed similar porous structures with those of silica aerogels or RF aerogels. Their thermal conductivity was as
low as that of the typical glass wool materials. The mechanical properties are characterized by dynamic mechanical analysis
and compression testing. At room temperature, the results of compression testing show that the compressive Young’s modulus
or ultimate failure strength of RF/SiO2 aerogel specimen is higher than that of native SiO2 aerogels with a similar density. The one-pot method improves the efficiency and reduces the cost of RF/SiO2 aerogels. The hierarchical porous carbon monoliths are also converted from carbonized RF/SiO2 aerogels by an additional HF treatment. Hence, they could be further explored as multifunctional candidate materials for
thermal, mechanical, and electrochemical applications. 相似文献
15.
The synthesis of silica aerogels reinforced with either carbon or silica fibre felts and which encapsulate the lipase PS of Amano (LPS AB025407) obtained from Burkholderia cepacia is described. The materials were further shaped by moulding them in Teflon® tubes. The silica aerogels were synthesized with various ratios of hydrophobic groups and dried according to the supercritical CO2 method. Both types of reinforcements improve the catalytic activity of the material per mass of lipase. The fibre felts reinforcements also enable the encapsulation of higher concentrations of lipase. The materials were shaped into small moulded monoliths, which were readily washed and recycled without significant mechanical deterioration or loss of catalytic activity. In addition, hydrophobic carbon felts reinforce more efficiently silica aerogels that incorporate a high ratio of hydrophobic groups, while silica felts strengthen those aerogels that carry a low proportion of hydrophobic groups. 相似文献
16.
The synthesis of silica aerogels was modified by addition of supercritical CO2 during the sol-gel process. It was shown, that CO2 acts as a catalyst and accelerates the gelation significantly. This effect was studied under a multitude of experimental conditions. The influence of the precursor concentration, temperature and the nature of the catalysts and solvent on the gel formation in presence of CO2 was studied. Several gels obtained by this method were dried and transparent silica aerogels were produced. 相似文献
17.
Rui Yan Minchao Zhang Wangqing Zhang Shuangxi Liu 《Journal of Sol-Gel Science and Technology》2011,59(2):315-326
Temperature dependent synthesis of micro- and meso-porous silica employing the thermo-responsive homopolymer poly(N-isopropylacrylamide) or the random copolymer poly(N-isopropylacrylamide-co-acrylic acid) as structure-directing agent (SDA) and Na2SiO3 as silica source is proposed. The thermo-responsive character of the SDA provides the advantages including (1) temperature
dependent synthesis of microporous silica, hierarchically micro-mesoporous silica, and mesoporous silica just by changing
the aging temperature below or above the low critical solution temperature of the thermo-responsive SDA, and (2) elimination
of the thermo-responsive SDA from silica matrix by water extraction. The synthesis mechanism is discussed, and the effect
of the aging temperature and the weight radio of SDA/Na2SiO3 on the synthesis of micro- and meso-porous silica are studied. Microporous silica, hierarchically micro-mesoporous silica
and mesoporous silica with the surface area at 3.5−9.0 × 102 m2/g and the pore volume at 0.28−1.13 cm3/g and the average pore size ranging from 1.1 to 9.0 nm are synthesized. The strategy affords a new and environmentally benign
way to fabricate porous silica materials, and is believed to bridge the gap between the synthesis of microporous and mesoporous
silica materials. 相似文献
18.
P. B. Wagh S. V. Ingale Satish C. Gupta 《Journal of Sol-Gel Science and Technology》2011,58(2):481-489
The new technology has been developed for rapid processing of silica aerogels at a rate 40 times faster than the conventional
method and is reported in the present paper. Silica gels were prepared using precursor chemicals Tetramethoxysilane: Methanol:
Water (0.05 mol L−1 NH4OH): Methyltrimethoxysilane at a molar ratio of 1: 12: 4: 0.8, respectively. Mixture of these precursors was stirred and transferred
to metallic moulds. These metallic moulds were kept in a 3-liter autoclave with an additional 400 mL of methanol. The autoclave
was pre-pressurized to 4 MPa with N2 gas and heated rapidly at the rate of 8 °C/min. to reach supercritical state of methanol. After 10 min, the vessel was depressurized at a rate of 0.45 MPa/min. The
sol in the mould when heated rapidly gets transformed to aerogel directly and the crucial alcogel handling step is skipped.
We successfully synthesized 50 mm diameter and 15 mm thick disc shaped and 40 mm diameter hemispherical monolithic aerogels
using the rapid process method. Retrieved aerogels were characterized for their density, surface area, optical transmittance,
fractal size, surface morphology and microstructure using SEM, TEM and SAXS. Aerogels synthesized by rapid process technology
shows improved physical properties than the aerogels derived by conventional method. 相似文献
19.
Masayuki Nogami Shohei Hotta Kazumasa Kugimiya Hideaki Matsubara 《Journal of Sol-Gel Science and Technology》2010,56(2):107-113
Silica-based aerogels with high transparency and high bending strength were prepared using methyltrimethoxysilane and non-ionic
surfactant under supercritical drying condition of CO2. Non-ionic surfactant, ethylene oxide/propylene oxide block copolymer, was appropriate to form the three dimensional-connected
thinner fibers of silica skeletons, which was extruded by soaking the wet gel in hot water at 50 °C, resulting in the formation
of porous materials having small pores with narrow size distribution. The transparency of aerogels increased with decreasing
the pore size, reaching to higher than 65 and 88% at 400 and 600 nm wavelength, respectively, for 10 mm thickness of sample.
The formation of fiber skeletons were discussed using small angle X-ray scattering experiments. 相似文献
20.
F. Ayari M. Mhamdi G. Delahay A. Ghorbel 《Journal of Sol-Gel Science and Technology》2009,49(2):170-179
A series of Cr/Al2O3 and Co/Al2O3 catalysts were tested in the selective ammoxidation of ethylene to acetonitrile. Catalysts were prepared either by sol–gel
method or by impregnation with chromium or cobalt acetylacetonate salts. Physicochemical properties of catalysts were accomplished
by several techniques such as chemical analysis, physisorption of N2, X-ray diffraction (XRD), 27Al MAS NMR, UV–Visible diffuse reflectance (DRS) and Raman spectroscopy and temperature programmed reduction of H2 (H2–TPR). Textural analysis reveals that mesoporous materials with pronounced surface areas were obtained using sol–gel procedure
while impregnation of the support produces a moderate decrease of its surface area and pore volume. XRD analysis confirms
the presence of highly dispersed metal species which reside essentially on the surface and measure less than 4 nm. Furthermore,
27Al MAS NMR shows that for xerogels, part of metal species occupies sites on/in A12O3 in close vicinity of octahedral 27Al. This, apparently, is not the case for aerogels. For Cr/Al2O3 catalysts, isolated Cr6+, mono and polychromate species were identified using DRS, Raman Spectroscopy and H2–TPR which seem to play a key role in the ammoxidation of ethylene. Furthermore, for cobalt doped catalysts, CoAl2O4 was identified as active phase on the basis of DRS and H2–TPR results. From the supercritical drying, it results generally better catalysts than catalysts calcined by ordinary procedure
which leads to inactive agglomerated Co3O4 and CoO–Al2O3 phase. 相似文献