Carbon Aerogels and Xerogels

1992 ◽  
Vol 270 ◽  
Author(s):  
Richard W. Pekala ◽  
Cynthia T. Alviso

ABSTRACTThe aqueous polycondensation of resorcinol with formaldehyde proceeds through a sol-gel transition and results in the formation of highly crosslinked, transparent gels. If the solvent is simply evaporated from the pores of these gels, large capillary forces are exerted and a collapsed structure known as a xerogel is formed. In order to preserve the gel skeleton and minimize shrinkage, the aforementioned solvent or its substitute must be removed under supercritical conditions. The microporous material that results from this operation is known as an aerogel. Because resorcinol-formaldehyde aerogels and xerogels consist of a highly crosslinked aromatic polymer, they can be pyrolyzed in an inert atmosphere to form vitreous carbon monoliths. The resultant porous materials are black in color and no longer transparent, yet they retain the ultrafine cell size (< 50 nm), high surface area (600-800 m2 /g), and the interconnected particle morphology of their organic precursors. The thermal, acoustic, mechanical, and electrical properties of carbon aerogels/xerogels primarily depend upon polymerization conditions and pyrolysis temperature. In this paper, the chemistry-structure-property relationships of these unique materials will be discussed in detail.

1995 ◽  
Vol 393 ◽  
Author(s):  
R.W. Pekala ◽  
C.T. Alviso ◽  
J.K. Nielsen ◽  
T.D. Tran ◽  
G.A.M. Reynolds ◽  
...  

ABSTRACTThe ability to tailor the structure and properties of porous carbons has led to their increased use as electrodes in energy storage devices. Our research focuses on the synthesis and characterization of carbon aerogels for use in electrochemical double layer capacitors. Carbon aerogels are formed from the sol-gel polymerization of (1) resorcinol-formaldehyde or (2) phenolic-furfural, followed by supercritical drying from carbon dioxide, and subsequent pyrolysis in an inert atmosphere. These materials can be produced as monoliths, composites, thin films, powders, or microspheres. In all cases, the aerogels have an open-cell structure with an ultrafine pore size (<100 nm), high surface area (400-1100 m2/g), and a solid matrix composed of interconnected particles, fibers, or platelets with characteristic dimensions of 10 nm. This paper examines the effects of the carbon precursor and processing conditions on electrochemical performance in aqueous and organic electrolytes.


1996 ◽  
Vol 431 ◽  
Author(s):  
J. Gross ◽  
C. T. Alviso ◽  
R. W. Pekala

AbstractSeveral organic reactions that proceed through a sol-gel transition have been identified at LLNL. The most-studied reaction involves the aqueous polycondensation of resorcinol (1,3- dihydroxybenzene) with formaldehyde. Recently, we have shown that phenol can be added to this polymerization as a comonomer. The resultant crosslinked gels are supercritically dried from carbon dioxide (Tc=31°C, Pc = 7.4 MPa) to give resorcinol-phenol-formaldehyde (RPF) aerogels. Because RPF aerogels are composed of a highly crosslinked aromatic polymer, they can be pyrolyzed in an inert atmosphere to form vitreous carbon monoliths (CRPF). The resultant aerogels are black in color and no longer transparent, yet they retain the high porosity (40–98 %), ultrafine cell/pore size (< 50 nm), high surface area (600–800 m2/g), and interconnected particle (˜10 nm) morphology of their organic precursors. In this study, we examine the acoustic and mechanical properties of these materials as a function of precursor material and pyrolysis temperature. It is shown that the elastic moduli of RPF and CRPF is higher than that of pure RF / CRF aerogels at a given density. Upon pyrolysis RPF aerogels tend to shrink to a larger extent.


2009 ◽  
Vol 24 (12) ◽  
pp. 3495-3502 ◽  
Author(s):  
Ana C. Marques ◽  
Rui M. Almeida ◽  
Amath Thiema ◽  
Shaojie Wang ◽  
Matthias Falk ◽  
...  

We report on the preparation of a bioactive CaO–SiO2 monolithic scaffold with interconnected bimodal nanomacro porosity, which simulates the morphology of a natural trabecular bone, by a newly developed modified sol-gel process. This method inherently creates nanopores, whose average diameter can be tailored to approximately 5–20 nm by solvent exchange. To achieve interconnected macroporosity (pores ∼5–300 μm in size), a polymer [poly(ethylene oxide)] is added, which causes phase separation simultaneously with the sol-gel transition. High-resolution scanning electron microscopy and mercury intrusion porosimetry demonstrate a high degree of three-dimensional interconnectivity and sharp distributions of pore size. In vitro bioactivity tests in simulated body fluid (SBF) show bioactivity of the material after soaking for approximately 5 h, as verified by the formation of a hydroxyapatite layer deep into the scaffold structure. Analysis of the SBF after the reaction indicates the dissolution of the samples, another desired feature of temporary scaffolds for bone regeneration. MG63 osteoblast-like cells seeded on our sol-gel glass samples responded better to samples with nanopores enlarged by a solvent exchange process than to the one with normal nanopores. Thus, the benefits of the high surface area achieved by sol-gel and solvent exchange procedures are most clearly demonstrated for the first time.


RSC Advances ◽  
2018 ◽  
Vol 8 (48) ◽  
pp. 27326-27331 ◽  
Author(s):  
Miralem Salihovic ◽  
Nicola Hüsing ◽  
Johannes Bernardi ◽  
Volker Presser ◽  
Michael S. Elsaesser

Using soft templating, mechanically reversible compressible resorcinol–formaldehyde aerogels can be converted into mechanically reversible compressible carbon aerogels with high surface area by carbonization in an inert atmosphere.


MRS Bulletin ◽  
1990 ◽  
Vol 15 (12) ◽  
pp. 30-36

Aerogels are a special class of open-cell foams derived from the supercritical drying of highly cross-linked inorganic or organic gels. These materials have ultrafine cell/pore sizes (less than 1,000 Å), continuous porosity, high surface area (400–1000 m2/g), and a microstructure composed of interconnected colloidal-like particles or polymeric chains with characteristic diameters of 100 Å. This microstructure is responsible for the unusual optical, acoustic, thermal, and mechanical properties of aerogels. For example, aerogels can be prepared as transparent, porous solids because their ultrafine cell/pore size minimizes light scattering in the visible spectrum. Figure 4.1 shows the different aerogels that will be discussed in this article.The hydrolysis and condensation of metal alkoxides is the most common synthetic route for the formation of inorganic aerogels. Inorganic aerogels have been prepared from monomers such as tetraisopropoxy titanate, aluminum secbutylate, and zirconium isopropoxide. Nevertheless, the majority of scientific research has concentrated on the sol-gel polymerization of tetramethoxysilane (TMOS), or the less toxic tetraethoxysilane (TEOS). The resultant silica aerogels are being investigated for applications ranging from window insulation to the collection of hypervelocity partis cles in space.The sol-gel polymerization of a multifunctional monomer in solution, leading to the formation of an aerogel, is not unique to metal alkoxides. Organic reactions that proceed through a sol-gel transition have been discovered recently.


RSC Advances ◽  
2016 ◽  
Vol 6 (62) ◽  
pp. 57217-57226 ◽  
Author(s):  
A. R. Passos ◽  
S. H. Pulcinelli ◽  
V. Briois ◽  
C. V. Santilli

Mechanism of gelation process and phase separation for production of hierarchical porous alumina with high surface area.


2010 ◽  
Vol 93 (12) ◽  
pp. 4047-4052 ◽  
Author(s):  
Padmaja Parameswaran Nampi ◽  
Padmanabhan Moothetty ◽  
Wilfried Wunderlich ◽  
Frank John Berry ◽  
Michael Mortimer ◽  
...  

2018 ◽  
Vol 29 (7) ◽  
pp. 075702 ◽  
Author(s):  
Feng Qingge ◽  
Cai Huidong ◽  
Lin Haiying ◽  
Qin Siying ◽  
Liu Zheng ◽  
...  

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.


2021 ◽  
Author(s):  
Nuray Kizildag

Ceramic materials are well known for their hardness, inertness, superior mechanical and thermal properties, resistance against chemical erosion and corrosion. Ceramic nanofibers were first manufactured through a combination of electrospinning with sol–gel method in 2002. The electrospun ceramic nanofibers display unprecedented properties such as high surface area, length, thermo-mechanical properties, and hierarchically porous structure which make them candidates for a wide range of applications such as tissue engineering, sensors, water remediation, energy storage, electromagnetic shielding, thermal insulation materials, etc. This chapter focuses on the most recent advances in the applications of ceramic nanofibers.


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