Morphology and properties of silica/novolac hybrid xerogels synthesized using sol–gel polymerization at solvent vapor-saturated atmosphere

2015 ◽  
Vol 69 ◽  
pp. 190-196 ◽  
Author(s):  
Mohamad Mehdi Seraji ◽  
Azadeh Seifi ◽  
Ahmad Reza Bahramian
2013 ◽  
Vol 829 ◽  
pp. 41-45 ◽  
Author(s):  
Alireza Hajizadeh ◽  
Ahmad Reza Bahramian ◽  
Alireza Sharif

Nanostructured organic materials have received considerable attention over the past decade. This nanostructure is responsible for their unusual acoustic, thermal, and mechanical properties. One of the most studying of this field is sol-gel polymerization of resorcinol-formaldehyde, followed by organic solvent exchange, supercritical drying. However, the conventional process involves long gelation time, expensive monomer of resorcinol, high cost of supercritical drying device and so on, which makes it some distance away from being promoted to commercial production. In this work, to reduce cost and time, the reaction of novolac resin and hexamine and ambient pressure drying method was used for preparation and drying of organic gel. To reduce time, the polymerization in saturated atmosphere of solvent vapor instead of conventional sol-gel polymerization presented. These nanostructure materials have a nanoporous structure that constructed by colloidal like particles gathered up in filament-shaped. Because of this nanoporosity and structure, these materials have very low fracture energy and could including them as brittle materials. The goal of this research produces these nanostructure materials using novel method and enhances fractural resistance. To gain this proposes, the feasibility of using acrylonitrilebutadiene rubbers (NBR) has been investigated. For studying of morphology and properties of this structure, we used SEM, FTIR and porosimetry analysis. The results shows that the addition of 0.5, 1 and 2 wt% NBR to Novolac nanostructure increased density and decrease the pore volume and pore size.


2013 ◽  
Vol 594-595 ◽  
pp. 1009-1014
Author(s):  
S.A. Syed Nuzul Fadzli ◽  
S. Roslinda ◽  
Z. Firuz

Hybrid silica xerogel mesoporous composite was synthesized by a mild temperature acid catalysed sol-gel route where a natural copolymer; sodium alginate (Na-COOH) together with calcium oxide (CaO) powder were incorporated into silica sol precursor prior to gel formation. For this study, bulk xerogels samples were prepared with the amount of silica precursor and the natural copolymer was fixed meanwhile the loading of calcium oxide was varied at 10 and 20 wt%. The monolith silica was also synthesized as control parameter. The preliminary properties were investigated using XRD, FTIR and SEM together with EDS for elemental analysis. The calcium oxide powder used in this study was prepared from calcium hydroxide, CaOH compound, which was previously calcined at 1000°C for 3 hours in normal air. The component of calcium oxide and sodium alginate were found to be uniformly dispersed in matrixes without affecting the cross-linked silica formation. As the presence of the components in the silica matrixes, the synthesized hybrid xerogels were found to be crack-free, structurally amorphous and physically opaque. Furthermore, the hybrid xerogels samples were found to have denser bodies, smoother surface, and decreased in particle sizes and thus might produced less brittleness in nature compared to the monolith xerogels.


2015 ◽  
Vol 3 (14) ◽  
pp. 7477-7487 ◽  
Author(s):  
Ales Styskalik ◽  
David Skoda ◽  
Zdenek Moravec ◽  
Michal Babiak ◽  
Craig E. Barnes ◽  
...  

Non-hydrolytic sol–gel reactions of acetoxysilanes with trimethylsilyl esters of phosphoric and phosphonic acids provide hybrid xerogels with large surface areas (up to 700 m2 g−1). The presence of SiO6 structural units in bridged-phosphoryl xerogels is related to their microporosity while the absence of such moieties in bridged-acetoxysilane networks is congruent with significant mesoporosity.


2000 ◽  
Vol 628 ◽  
Author(s):  
Pedro J. Retuert ◽  
Raul Quijada ◽  
Catalina Lafourcade

ABSTRACTThe combination of sols containing silica polymers, prepared by the sol-gel method under conditions of nearly linear chain growth, with solutions of the biopolymer chitosan has allowed us to obtain hybrid materials in the form of films or particles. In these hybrid nanocomposites, the organic and inorganic phases are associated through hydrogen bonds. In this work we present the preparation of hybrid xerogels of spherical morphology and their transformation into hollow spherical particles of silica with high specific area (276 m2/g) and a pore volume of 0.23 cm3/g. The xerogel particles were obtained by precipitation and subsequent drying. Thereafter, chitosan was extracted partially with acetic acid (5%) and finally the product was calcined at 550°C for two hours. The SEM micrograph shows that the silica particles were obtained as hollow spheres with size in the range between 10 and 100 μm. By using larger magnification, it was found that much smaller spheres of about 0.01 μm constitute the surface of these hollow spheres. Porosimetry shows the presence of micropores as well as mesopores. The observed morphology is discussed on the basis of a coprecipitation process conditioned by an association of both organic and inorganic phases in the precursor hybrid sol.


2004 ◽  
Vol 16 (20) ◽  
pp. 3794-3799 ◽  
Author(s):  
Geneviève Cerveau ◽  
Robert J. P. Corriu ◽  
Eric Framery ◽  
Frédéric Lerouge

2013 ◽  
Vol 454 ◽  
pp. 152-159 ◽  
Author(s):  
Enéderson Rossetto ◽  
Marcela Caovilla ◽  
Daniel Thiele ◽  
Roberto F. de Souza ◽  
Katia Bernardo-Gusmão

Polymers ◽  
2021 ◽  
Vol 13 (13) ◽  
pp. 2082
Author(s):  
Guillermo Cruz-Quesada ◽  
Maialen Espinal-Viguri ◽  
María Victoria López-Ramón ◽  
Julián J. Garrido

The properties of hybrid silica xerogels obtained by the sol-gel method are highly dependent on the precursor and the synthesis conditions. This study examines the influence of organic substituents of the precursor on the sol-gel process and determines the structure of the final materials in xerogels containing tetraethyl orthosilicate (TEOS) and alkyltriethoxysilane or chloroalkyltriethoxysilane at different molar percentages (RTEOS and ClRTEOS, R = methyl [M], ethyl [E], or propyl [P]). The intermolecular forces exerted by the organic moiety and the chlorine atom of the precursors were elucidated by comparing the sol-gel process between alkyl and chloroalkyl series. The microstructure of the resulting xerogels was explored in a structural theoretical study using Fourier transformed infrared spectroscopy and deconvolution methods, revealing the distribution of (SiO)4 and (SiO)6 rings in the silicon matrix of the hybrid xerogels. The results demonstrate that the alkyl chain and the chlorine atom of the precursor in these materials determines their inductive and steric effects on the sol-gel process and, therefore, their gelation times. Furthermore, the distribution of (SiO)4 and (SiO)6 rings was found to be consistent with the data from the X-Ray diffraction spectra, which confirm that the local periodicity associated with four-fold rings increases with higher percentage of precursor. Both the sol-gel process and the ordered domains formed determine the final structure of these hybrid materials and, therefore, their properties and potential applications.


2004 ◽  
Vol 847 ◽  
Author(s):  
Douglas A. Loy ◽  
James H. Small ◽  
Kimberly A. DeFriend ◽  
Kennard V. Wilson ◽  
McKenzie Minke ◽  
...  

ABSTRACTThe introduction of organic substituents into sol-gel materials can often result in networks that collapse during drying to afford non-porous xerogels. This can prove useful if non-porous coatings or membranes are the ultimate objectives. Collapse of porosity is also manifested in bridged polysilsesquioxanes with flexible bridging groups. Alkylene-bridged polysilsesquioxanes are hybrid xerogels whose organic bridging group is an integral constituent of the network polymer that can be systematically varied to probe the influence of its length on the xerogels' porosity and morphology. Our previous studies have shown that hexylene-bridged polysilsesquioxane xerogels prepared from 1, 6-bis(triethoxysilyl)hexane under acidic conditions are nonporous while the pentylene-bridged polysilsesquioxanes prepared under the same conditions are porous. We also discovered that the more reactive 1, 6-bis(trimethoxysilyl)hexane monomer could polymerize under acidic conditions to afford porous xerogels. Here, we have extended our study of bis(trimethoxysilyl)alkanes to include the heptylene (C7), octylene (C8), nonylene(C9) and decylene (C10) bridges so as to ascertain at what bridging group length the porosity collapses. The morphology of the resulting xerogels was characterized by nitrogen sorption porosimetry and electron microscopy. Solid state NMR was used to structurally characterize the materials.


1998 ◽  
Vol 519 ◽  
Author(s):  
H.K. Schmidt ◽  
E. Arpac ◽  
H. Schirra ◽  
S. Sepeur ◽  
G. Jonschker ◽  
...  

AbstractSol-gel reactions, in general, have to take place in organic solvents in order to control the hydrolysis and condensation reaction. This leads to drawbacks in applications, since the organic solvent vapor concentration has to be controlled for example in coating applications for environmental, health or security reasons. For this reason, a reaction route has been developed to produce coating precursors stable against water as solvent. To achieve this, conventional electrostatically stabilized sols obtained either by hydrolysis and condensation or commercially available sols (e.g. SiO2sols) have been surface-modified to reduce the particle-to-particle interaction and electrosterically stabilized precursors compatible to water have been obtained. By use of alkoxy silanes as surface modifiers, water-dispersable nanoparticulate liquid coating systems have been prepared, for example, with boehmite, SiO2 or TiO2 as nanoparticles to be crosslinked after coating thermally by inorganic condensation and organic condensation or polymerization reactions. Thus, aqueous sol-gel coating systems have been prepared with EtOH contents below 5 %. In the paper, the basic reaction as well as material properties will be discussed.


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