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Title: Electron microscopy and nitrogen adsorption studies of film-type carbon replicas with large pore volume synthesized by using collodial silica and SBA-15 as templates

Abstract

Mesoporous carbons synthesized by the film-type replication of colloidal silica and SBA-15 templates are studied by electron microscopy and nitrogen adsorption. This synthesis strategy involves the formation of thin carbon film on the pore walls of these templates using resorcinol-crotonaldehyde polymer as carbon precursor. For the silica templates consisting of 20-80 nm colloids this synthesis affords carbons with extremely large pore volumes (5-9 cm{sup 3}/g) and uniform spherical pores reproducing the size of the colloids used.

Authors:
 [1];  [1];  [2];  [2]
  1. Kent State University
  2. ORNL
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Center for Nanophase Materials Sciences
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
964309
DOE Contract Number:
DE-AC05-00OR22725
Resource Type:
Journal Article
Resource Relation:
Journal Name: Carbon; Journal Volume: 45; Journal Issue: 11
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CARBON; COLLOIDS; POLYMERS; PRECURSOR; SILICA; SYNTHESIS; POROUS MATERIALS; FILMS

Citation Formats

Gierszal, Kamil P., Jaroniec, Mietek, Liang, Chengdu, and Dai, Sheng. Electron microscopy and nitrogen adsorption studies of film-type carbon replicas with large pore volume synthesized by using collodial silica and SBA-15 as templates. United States: N. p., 2007. Web. doi:10.1016/j.carbon.2007.06.053.
Gierszal, Kamil P., Jaroniec, Mietek, Liang, Chengdu, & Dai, Sheng. Electron microscopy and nitrogen adsorption studies of film-type carbon replicas with large pore volume synthesized by using collodial silica and SBA-15 as templates. United States. doi:10.1016/j.carbon.2007.06.053.
Gierszal, Kamil P., Jaroniec, Mietek, Liang, Chengdu, and Dai, Sheng. Mon . "Electron microscopy and nitrogen adsorption studies of film-type carbon replicas with large pore volume synthesized by using collodial silica and SBA-15 as templates". United States. doi:10.1016/j.carbon.2007.06.053.
@article{osti_964309,
title = {Electron microscopy and nitrogen adsorption studies of film-type carbon replicas with large pore volume synthesized by using collodial silica and SBA-15 as templates},
author = {Gierszal, Kamil P. and Jaroniec, Mietek and Liang, Chengdu and Dai, Sheng},
abstractNote = {Mesoporous carbons synthesized by the film-type replication of colloidal silica and SBA-15 templates are studied by electron microscopy and nitrogen adsorption. This synthesis strategy involves the formation of thin carbon film on the pore walls of these templates using resorcinol-crotonaldehyde polymer as carbon precursor. For the silica templates consisting of 20-80 nm colloids this synthesis affords carbons with extremely large pore volumes (5-9 cm{sup 3}/g) and uniform spherical pores reproducing the size of the colloids used.},
doi = {10.1016/j.carbon.2007.06.053},
journal = {Carbon},
number = 11,
volume = 45,
place = {United States},
year = {Mon Jan 01 00:00:00 EST 2007},
month = {Mon Jan 01 00:00:00 EST 2007}
}
  • Mesoporous carbons synthesized by the film-type replication of colloidal silica and SBA-15 templates are studied by electron microscopy and nitrogen adsorption. This synthesis strategy involves the formation of thin carbon film on the pore walls of these templates using resorcinol-crotonaldehyde polymer as carbon precursor. For the silica templates consisting of 20-80 nm colloids this synthesis affords carbons with extremely large pore volumes (5-9 cm3/g) and uniform spherical pores reproducing the size of the colloids used.
  • Polypyrrole-based ordered mesoporous carbons (OMCs) were synthesized via chemical vapor infiltration of pyrrole into pores of the SBA-15 and SBA-16 silica templates containing iron(III) chloride catalyst (FeCl{sub 3}). After carbonization of polypyrrole at 800 C and etching of the silica templates with hydrofluoric acid solution, nitrogen-doped and graphitic OMCs with incorporated magnetic nanoparticles were obtained. These materials were analyzed by CHNS elemental analysis, thermogravimetry (TG), nitrogen adsorption, small and wide angle powder X-ray diffraction (XRD), Raman spectroscopy, scanning, and transmission electron microscopy (TEM). The resulting carbon replicas retained the crystallographic symmetry of the silica templates: namely, P6mm in the casemore » of the SBA-15 template, and Im3m in the case of the SBA-16 template. The uniformity, size, and volume of ordered mesopores in the carbon replicas were affected by structural properties of the templates used as shown by analysis of nitrogen adsorption isotherms and pore size distributions. A better infiltration of carbon precursor was achieved for the templates with larger pores, which resulted in the carbon replicas of improved adsorption and structural properties. Elemental analysis revealed the presence of nitrogen in the carbon replicas studied in the range of 3-8 wt %, whereas TG analysis of the replica samples in air gave about 2-5% residue, which was identified as hematite (Fe{sub 2}O{sub 3}). The presence of graphitic domains was confirmed by characteristic TG oxidation profile above 400 C, the D and G bands on the Raman spectra, and the intense reflections on the wide angle XRD patterns. Powder XRD also showed the presence of extra-framework magnetic iron ({alpha}-Fe) and iron carbide (Fe{sub 3}C) nanoparticles having crystallite size in the ranges of 40-80 and 20-40 nm, respectively. TEM images also revealed that these nanoparticles were larger than the carbon rods and pore widths of the SBA-15 carbon replica, which is in good agreement with the XRD-based estimation. The in situ EDS analysis of carbon rods and spheres showed that iron was present in the carbonaceous framework, which does not exclude the existence of much smaller nanoparticles, below 5 nm.« less
  • A new SBA-15 supported 1,4,7-triazacyclononane modified mesoporous silica adsorbent (SBA-TACN) has been synthesized using post grafting route and has thoroughly been characterized by small angle X-ray scattering (SAXS), N{sub 2} adsorption–desorption measurements, Fourier-transform infrared (FT-IR), solid-state {sup 29}Si MAS and {sup 13}C CP MAS NMR spectroscopy, transmission electron (TEM) and scanning electron microscopy (SEM), elemental analysis (EA) and thermogravimetric analysis (TGA). The synthesized material shows excellent copper (II) ion adsorption selectivity at pH 5 in mixed metal ion solution containing Cu{sup 2+}, Cr{sup 3+}, Ni{sup 2+}, Co{sup 2+} and Li{sup +}. The copper ion adsorption capacity of the SBA-TACN canmore » reach a maximum value of 0.67 mmol/g. Possible adsorption mechanism of metal ions on SBA-TACN has been discussed. The adsorbent can be readily regenerated by HNO{sub 3}–NH{sub 3} treatment. -- Graphical abstract: A new SBA-15 supported 1,4,7-triazacyclononane (TACN) modified mesoporous silica (SBA-TACN) adsorbent has been developed which shows excellent selectivity in Cu{sup 2+} adsorption from aqueous mixed metal ion solutions at pH 5. The copper ion adsorption capacity of the SBA-TACN can reach a maximum value of 0.67 mmol/g. The adsobent is stable enough to be used atleast for three cycles. Highlights: • Synthesis of a new TACN modified mesoporous silica SBA-15 type adsorbent. • The density of 1,4,7-triazacyclononane on SBA-15 is 1.22 mmol/g. • First report on the selective Cu{sup 2+} adsorption by TACN modified mesoporous silica. • Cu{sup 2+} adsorption capacity of the SBA-TACN can reach a maximum value of 0.67 mmol/g. • Potential candidate for selective removal of Cu{sup 2+} from contaminated water samples.« less
  • No abstract prepared.