A General Nonhydrolytic Sol‐Gel Route to Oxides

1994 ◽  
Vol 346 ◽  
Author(s):  
Sylvie Acosta ◽  
Pascal Arnal ◽  
Robert J.P. Corriu ◽  
Dominique Leclercq ◽  
P. Hubert Mutin ◽  
...  

ABSTRACTA nonhydrolytic sol‐gel route based on the condensation between chlorides and oxygen donors such as ethers and alkoxides is presented. Four examples, silica, alumina, titania and binary oxides in the Al/Si system show that this is a general route. The mechanism of this condensation is completely different from the one of classical sol‐gel process, since it implies nucleophilic substitution at the carbon center instead of the metal center. As a consequence, the differences in reactivity between different metals are reduced. In addition, the structure of the precursors may be retained in the gel. Thus, the nonhydrolytic sol‐gel process is very efficient for the preparation of homogeneous bicomponent oxides. Futhermore, nonhydrated gels are formed, which allowed us to prepare amorphous aluminas with high surface areas.

2010 ◽  
Vol 146-147 ◽  
pp. 1801-1805 ◽  
Author(s):  
You Ji Li ◽  
Wei Chen ◽  
Lei Yong Li ◽  
Ming Yuan Ma

TiO2-SBA-15 surface (TSS) composites were prepared by the supercritical pretreatment and then sol-gel process with using paraffin used as a clogging agent. The as-grown materials were characterized by using X-ray diffraction, UV-VIS spectroscopy and nitrogen absorption. The photocatalytic activities of TSS were evaluated by quantifying the degradation of methylene blue solution under UV light. Compared with TiO2-SBA-15 (TS) composites prepared only by the sol–gel method, TSS composites remain in mesostructure with high surface areas due to clogging effect of paraffin on SBA-15 cavity. Additionally, the small crystalline size of TiO2 in TSS is attributed to the fact that silica support baffles the agglomeration ofTiO2 nanoparticles. In comparison of TS composites and pure TiO2, higher photocatalytic activity of TSS is obtained and mainly attributed to larger surface areas and greater band-gap energy.


2013 ◽  
Vol 284-287 ◽  
pp. 230-234
Author(s):  
Yu Jen Chou ◽  
Chi Jen Shih ◽  
Shao Ju Shih

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.


Materials ◽  
2020 ◽  
Vol 13 (4) ◽  
pp. 992
Author(s):  
Seray Schmitz ◽  
Ana M. Beltrán ◽  
Mark Cresswell ◽  
Aldo R. Boccaccini

One of the key benefits of sol-gel-derived glasses is the presence of a mesoporous structure and the resulting increase in surface area. This enhancement in textural properties has a significant effect on the physicochemical properties of the materials. In this context the aim of this study was to investigate how sol-gel synthesis parameters can influence the textural and structural properties of mesoporous silicate glasses. We report the synthesis and characterization of metal ion doped sol-gel derived glasses with different dopants in the presence or absence of a surfactant (Pluronic P123) used as structure-directing templating agent. Characterization was done by several methods. Using a structure directing agent led to larger surface areas and highly ordered mesoporous structures. The chemical structure of the non-ordered glasses was modified to a larger extent than the one of the ordered glasses due to increased incorporation of dopant ions into the glass network. The results will help to further understand how the properties of sol-gel glasses can be controlled by incorporation of metal dopants, in conjunction with control over the textural properties, and will be important to optimize the properties of sol-gel glasses for specific applications, e.g., drug delivery, bone regeneration, wound healing, and antibacterial materials.


2013 ◽  
Vol 706-708 ◽  
pp. 897-900 ◽  
Author(s):  
Rui He ◽  
Xuan Liu ◽  
Zhen Fa Liu ◽  
Li Hui Zhang

In this research the fabrication of carbon aerogel is reported. nanopore carbon aerogels were prepared via a sol-gel process with resorcinol and formaldehyde (RF) aerogels,which were cost-effectively manufacture form Rf wet gels by an ambient drying technique instead of conventional supercritical drying. The key of the work is to fabricate carbon aerogels with controllable nanopore structure, which means sharp pore size distribution and extremely high surface area.The influence of preparation condition of carbon aerogels was studied by scanning electron microscope and Micropore Physisorption Analyzer. The BET surface of the carbon aerogels are from 749m2/g to 1156m2/g .The size of the carbon nanoparticles are in the range of 20nm~40nm. The micro-pore volume and bore diameter can be controlled by gelation conditions such as RF mass fraction.


1994 ◽  
Vol 346 ◽  
Author(s):  
Kyung Moon Choi ◽  
Kenneth J. Shea

ABSTRACTPoly(l,4-phenylene)-bridged and poly(1,6-hexylene)-bridged silsesquioxanes (PPS and HPS) were prepared by the sol-gel process. The surface areas and pore diameters of these porous xerogels were obtained by BET and BJH methods, respectively. These porous materials were used as a confinement matrix for the growth of small-sized semiconductor and transition metal clusters. Quantum-sized CdS particles in PPS (approximately 58+12 Â) and HPS (91+16 Â) matrices were prepared by first soaking the xerogel in a CdCl2 solution. Following a washing with water, a Na2S solution was then added. EDAX and electron diffraction techniques were used to identify the CdS particles. The particle sizes of CdS in PPS and HPS were determined by both UV measurements and from TEM images. Small-sized Cr clusters were prepared in dried xerogels by an internal doping method. Mixed Cr/CdS phases were also prepared by internal loading of a chromium metal precursor. Following deposition of CdS the xerogel was heated at 120 °C under high vacuum, resulting in formation of intimately mixed phases of Cr metal and CdS. Changes in morphology, in particular the surface area and pore size distribution were noted. A decrease in surface area and an increase in pore size were observed as a result of Cr metal deposition.


1986 ◽  
Vol 73 ◽  
Author(s):  
Joseph R. Fox ◽  
Douglas A. White ◽  
Susan M. Oleff ◽  
Robert D. Boyer ◽  
Phyllis A. Budinger

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.


2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Simon Carstens ◽  
Christian Splith ◽  
Dirk Enke

AbstractOne of the major routes to synthesize macroporous α-Al2O3 is the sol-gel process in presence of templates. Templates include polymers as well as carboxylic acids, such as citric acid. By careful choice of the template, pore diameters can be adjusted between 110 nm and several µm. We report the successful establishment of plain short-chain dicarboxylic acids (DCA) as porogenes in the sol-gel synthesis of macroporous α-Al2O3. By this extension of the recently developed synthesis route, a very precise control of pore diameters is achieved, in addition to enhanced macropore volumes in α-Al2O3. The formation mechanism thereof is closely related to the one postulated for citric acid, as thermal analyses show. However, since branching in the DCA-linked alumina nuclei is not possible, close monomodal pore width distributions are attained, which are accompanied by enhanced pore volumes. This is a significant improvement in terms of controlled enhanced porosity in the synthesis of macroporous α-Al2O3.


1990 ◽  
Vol 180 ◽  
Author(s):  
R.W. Pekala ◽  
C.T. Alviso

ABSTRACTThe aqueous, sol-gel polymerization of melamine with formaldehyde, followed by supercritical extraction, leads to the formation of a new type of organic aerogel. Synthetic conditions (e.g. reaction time, pH) affect the density, transparency, and microstructure of the resultant aerogels. Unlike previous organic aerogels based upon resorcinol-formaldehyde, the melamine-formaldehyde aerogels are both colorless and transparent. Low densities (0.1–0.8 g/cc), high surface areas (∼1000 m2/g), and optical clarity are only a few of the promising characteristics of this new material.


Sign in / Sign up

Export Citation Format

Share Document