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Journal ArticleDOI

Novel synthesis of porous carbons with tunable pore size by surfactant-templated sol-gel process and carbonisation.

04 Nov 2002-Chemical Communications (The Royal Society of Chemistry)-Iss: 22, pp 2722-2723
TL;DR: Surfactant-templated sol-gel polymerisation was explored to synthesize the resorcinol-formaldehyde gels without supercritical drying step, which were further carbonised to obtain porous carbons of a tunable pore size.
About: This article is published in Chemical Communications.The article was published on 2002-11-04 and is currently open access. It has received 77 citations till now. The article focuses on the topics: Supercritical drying.

Summary (1 min read)

T h i s j o u r n a l i s © T h e R o y a l S o c i e t y o f

  • The pore size is primarily determined by the size of gel clusters, which is in turn controlled by the monomer/surfactant concentration.
  • It is thus very likely that, in acidic conditions, the cross-linking between gel clusters becomes more facilitated to produce a more rigid gel network, and the pore collapse or shrinking at both the drying step and subsequent carbonisation step is suppressed.
  • To test this possibility, the sol-gel polymerisation was performed at different pH by varying the R/F ratio in this work (samples C5-C7).
  • When the pore properties are compared for samples C5-C7, there appears a strong correlation between the porosity and pH of the sol-gel medium even if the carbon cluster size is comparable for the three because the monomer/surfactant concentration is the same.
  • Fig. 3(b) shows the pore size distribution of samples C3-C7 as calculated by the Barrett-Joyner-Halenda (BJH) method from the desorption branch of the isotherm.

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Citations
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Journal ArticleDOI
TL;DR: In this paper, resorcinol-formaldehyde (RF) gels were synthesized via sol-gel polymerization in the presence of sodium dodecylbenzene sulfonate (NaDBS) followed by ambient and supercritical drying.
Abstract: In the past two decades, resorcinol–formaldehyde (RF) gels have found widespread applications owing to their low density and adjustable pore size. They are usually prepared through sol–gel polymerization of the monomers in an aqueous media followed by evaporative or supercritical drying. In this study, RF gels were synthesized via sol–gel polymerization in the presence of sodium dodecylbenzene sulfonate (NaDBS) followed by ambient and supercritical drying. Dimensional measurements along with N2 sorption analysis and Scanning electron microscopy (SEM) micrographs revealed that pore structure of the gel is chiefly affected by NaDBS. In all samples (xerogels and aerogels), maximum densities were observed at a critical NaDBS concentration (~1 w/v%), whereas considerable pore size increments and pore size distribution broadenings were found at higher concentrations of NaDBS (≥5 w/v%). The most increased mesopore volumes were detected in xerogels (133% for acetone-dried and 67% for water-dried samples), while concerning aerogels, the pore sizes enlargement to macropore regime was observed at 5 w/v% of NaDBS. SEM micrographs, in agreement with porosity analysis, depicted that very large pore volumes could be obtained when supercritical drying was employed. However, in the case of xerogels, a more dense structure with smaller pores (micro and mesopores) exists which can only be altered slightly when using large amounts of NaDBS. The results showed that the RF gel pore texture, independent of drying technique, was strongly influenced by the addition of NaDBS, which should be taken into account when using this surfactant in the gel formulation for a wide variety of applications.

11 citations

Journal ArticleDOI
TL;DR: In this article, a high acid induced heterogeneous nucleation and growth approach to synthesize dual-mesoporous carbon nanospheres (DMCN) with well-controlled small diameters is reported.

11 citations

Journal ArticleDOI
TL;DR: In this paper, the microstructure of ordered mesoporous carbons doped with MnO nanoparticles was analyzed by the small-angle X-ray scattering, Xray diffraction, nitrogen adsorption isotherms and transmission electron microscopy.

10 citations

Book ChapterDOI
01 Jan 2017
TL;DR: In this paper, the mesoporous materials have been used to create interactions with drug molecules for targeted drug delivery and designed release profiles, such as impregnation, absorption, spray drying, and super critical fluid processes.
Abstract: To enhance the therapeutic efficacy of oral dosage forms, the development and application of mesoporous excipients with pore size ranging 2–300 nm has attracted much attention from both academia and industry in recent years. As drug carriers, mesoporous excipients rank among the top few that have the highest specific surface area to volume ratios. This enables high drug loading for bioenhancement, target delivery, controlled and sustained release applications. Various mesoporous materials, such as silica, carbon, and bioactive glass have been fabricated with uniform nanoscale pores. Poorly water-soluble drugs [such as BCS-II active pharmaceutical ingredients (APIs)] were loaded into the porous excipients, so as to enhance the dissolution properties and improve the bioavailability of these APIs. Due to the mesoporous nature of the carrier, the APIs were confined and stabilized within the nanochannels in a metastable amorphous state without long-range molecular order. The surface of the mesoporous materials could be functionalized to create interactions with drug molecules for targeted drug delivery and designed release profiles. The developments in drug-loading techniques, such as impregnation, absorption, spray drying, and super critical fluid processes are also reviewed.

9 citations

References
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Journal ArticleDOI
TL;DR: In this paper, the polycondensation of resorcinol with formaldehyde under alkaline conditions results in the formation of surface functionalized polymer "clusters" which are processed under supercritical conditions to obtain low density, organic aerogels.
Abstract: The polycondensation of resorcinol with formaldehyde under alkaline conditions results in the formation of surface functionalized polymer “clusters”. The covalent crosslinking of these “clusters” produces gels which are processed under supercritical conditions to obtain low density, organic aerogels ( ⩽ 0.1 g cm−3). The aerogels are transparent, dark red in colour, and consist of interconnected colloidal-like particles with diameters of approximately 10 nm. The polymerization mechanism, structure and properties of the resorcinol-formaldehyde aerogels are similar to the sol-gel processing of silica.

1,603 citations

Journal ArticleDOI
TL;DR: Ordered mesoporous carbons have been synthesized using ordered mesopore silica templates as discussed by the authors, where the template needs to exhibit three-dimensional pore structure in order to be suitable for the ordered mesophorous carbon synthesis, otherwise disordered microporous carbon is formed.
Abstract: Ordered mesoporous carbons have recently been synthesized using ordered mesoporous silica templates. The synthesis procedure involves infiltration of the pores of the template with appropriate carbon precursor, its carbonization, and subsequent template removal. The template needs to exhibit three-dimensional pore structure in order to be suitable for the ordered mesoporous carbon synthesis, otherwise disordered microporous carbon is formed. MCM-48, SBA-1, and SBA-15 silicas were successfully used to synthesize carbons with cubic or hexagonal frameworks, narrow mesopore size distributions, high nitrogen Brunauer–Emmett–Teller (BET) specific surface areas (up to 1800 m2 g–1), and large pore volumes. Ordered mesoporous carbons are promising in many applications, including adsorption of large molecules, chromatography, and manufacturing of electrochemical double-layer capacitors.

1,467 citations

Journal ArticleDOI
TL;DR: In this paper, the authors reviewed the mechanisms of gel formation in silicate systems derived from metal alkoxides and proposed that the resulting polysilicate species formed prior to gelation is not a dense colloidal particle of anhydrous silica but instead a solvated polymeric chain or cluster.
Abstract: The mechanisms of gel formation in silicate systems derived from metal alkoxides were reviewed. There is compelling experimental evidence proving, that under many conditions employed in silica gel preparation, the resulting polysilicate species formed prior to gelation is not a dense colloidal particle of anhydrous silica but instead a solvated polymeric chain or cluster. The skeletal gel phase which results during desiccation is, therefore, expected to be less highly crosslinked than the corresponding melted glass, and perhaps to contain additional excess free volume. It is proposed that, during gel densification, the desiccated gel will change to become more highly crosslinked while reducing its surface area and free volume. Thus, it is necessary to consider both the macroscopic physical structure and the local chemical structure of gels in order to explain the gel to glass conversion.

511 citations

Journal ArticleDOI
01 Jan 1997-Carbon
TL;DR: In this article, mesoporous carbon xerogels were prepared from the sol-gel polymerization of resorcinol with formaldehyde (RF) followed by carbonization.

346 citations

Journal ArticleDOI
01 Jan 1999-Carbon
TL;DR: In this paper, a solgel polycondensation of resorcinol with formaldehyde and freeze drying with t -butanol was used to obtain mesoporous materials with high surface areas and large mesopore volumes.

278 citations

Frequently Asked Questions (1)
Q1. What have the authors contributed in "Novel synthesis of porous carbons with tunable pore size by surfactant-templated sol–gel process and carbonisation" ?

Here, the authors report another low-cost preparation method for RF xerogels, where a normal drying is still applicable because the pore collapse can be minimized during the water evaporation. The microto nanosized spherical gel clusters are formed within the micelles, which are further three-dimensionally connected via a crosslinking reaction. The resulting RF gels are dried at 85 °C and further heat-treated at 1000 °C for 3 h under argon atmosphere to obtain porous carbons in monolithic shape.