Abstract:A polymer, polydicyclopentadiene (PDCPD), is hybridized within the pores of activated carbon (AC) that has micropores and mesopores of ∼4 nm. The hybridization is performed via gas-phase adsorption of dicyclopentadiene (DCPD) on AC and subsequent thermal polymerization. It is confirmed from a variety of analytical techniques, such as scanning and transmittance electron microscopies, a nitrogen adsorption− desorption analysis, and electrochemical measurements, that there is little PDCPD on the particle surfaces… Show more
“…The results of the AC-4/PNBD hybrids are in good agreement with the results of the hybrids prepared from AC-4 and polydicyclopentadiene (PDCPD) . We have previously reported the hybridization of PDCPD within the pores of AC-4, and three models of PDCPD were considered for the AC-4/PDCPD hybrids, as shown in Figure : layer (a), agglomeration (b), and micropore-filling (c) models.…”
Section: Resultssupporting
confidence: 84%
“…, ∼2 nm) and AC-4 with both micropores and mesopores below 4 nm . Unless the amount of NBD exceeds the saturation amount of AC, NBD is completely adsorbed on AC by using a gas-phase adsorption technique. , Therefore, the amount of the adsorbed NBD can be accurately controlled. The NBD-adsorbed ACs are denoted as AC-2/NBD ( X ) and AC-4/NBD ( X ) for the samples prepared using AC-2 and AC-4, respectively, where X represents the amount of the adsorbed NBD per 1 g of AC ( i.e.…”
Section: Resultsmentioning
confidence: 99%
“…The dried AC was added to a glass vial under a nitrogen atmosphere, and the mass of the dried AC was calculated by the weight difference of the glass ampoule. Subsequently, NBD (Tokyo Chemical Industry Co., Ltd.) was added to a glass tube, and the glass tube was frozen by liquid nitrogen so as not to evaporate during a subsequent procedure . The amount of NBD was adjusted to make accurate AC/NBD weight ratios.…”
Section: Methodsmentioning
confidence: 99%
“…The following characterizations were done as described in ref : nitrogen adsorption/desorption, Raman spectroscopy, and XRD analyses; TEM and SEM observations. The Brunauer–Emmett–Teller (BET) specific surface area was calculated using the adsorption isotherm in a P / P 0 range of 0.05–0.20.…”
Section: Methodsmentioning
confidence: 99%
“…The structures of the redox-active materials hybridized within the pores of porous carbons seem to have an effect on the charge/discharge characteristics but cannot be identified by conventional spectroscopic and observation techniques because the amorphous structure of porous carbons hampers the observation of the confined materials, and conductive polymers and redox-active organic compounds consist of light elements. We have reported the existing form of the hybridized polydicyclopentadiene (PDCPD) within the pores of activated carbon (AC) by combining conventional structural characterizations with nitrogen adsorption/desorption and electrochemical measurements . The AC had micropores and mesopores below 4 nm, and PDCPD was not hybridized as a layer nor preferentially localized inside micropores but was uniformly distributed inside both micropores and mesopores as an agglomerate.…”
Norbornadiene (NBD) is adsorbed on activated carbon (AC), and the adsorbed NBD is polymerized within the pores of AC. Two kinds of ACs�AC-2 with only micropores of ∼2 nm and AC-4 with not only micropores but also mesopores below 4 nm�are examined to study the effects of the hybridized polynorbornadiene (PNBD) on the electric double-layer capacitor and hydrogen adsorption performance. Various measurements are performed to determine the form of the hybridized PNBD inside the pores of AC. Scanning and transmittance electron microscopy observations of the AC/PNBD hybrids confirm that PNBD is hybridized inside the pores of AC, and there is little PNBD on the surface of AC particles. The nitrogen adsorption/desorption measurement for the hybrids of AC-4 reveals that PNBD is not hybridized preferentially inside micropores rather than mesopores irrespective of the amount of PNBD. In addition, both micropore and mesopore volumes decrease at a constant rate with increasing amounts of PNBD. These results suggest that PNBD is hybridized not as a layer but as an agglomerate for both ACs, and the agglomerate delocalizes over the whole AC pores, which is supported by the results of electrochemical measurements and hydrogen adsorption behavior of the hybrids.
“…The results of the AC-4/PNBD hybrids are in good agreement with the results of the hybrids prepared from AC-4 and polydicyclopentadiene (PDCPD) . We have previously reported the hybridization of PDCPD within the pores of AC-4, and three models of PDCPD were considered for the AC-4/PDCPD hybrids, as shown in Figure : layer (a), agglomeration (b), and micropore-filling (c) models.…”
Section: Resultssupporting
confidence: 84%
“…, ∼2 nm) and AC-4 with both micropores and mesopores below 4 nm . Unless the amount of NBD exceeds the saturation amount of AC, NBD is completely adsorbed on AC by using a gas-phase adsorption technique. , Therefore, the amount of the adsorbed NBD can be accurately controlled. The NBD-adsorbed ACs are denoted as AC-2/NBD ( X ) and AC-4/NBD ( X ) for the samples prepared using AC-2 and AC-4, respectively, where X represents the amount of the adsorbed NBD per 1 g of AC ( i.e.…”
Section: Resultsmentioning
confidence: 99%
“…The dried AC was added to a glass vial under a nitrogen atmosphere, and the mass of the dried AC was calculated by the weight difference of the glass ampoule. Subsequently, NBD (Tokyo Chemical Industry Co., Ltd.) was added to a glass tube, and the glass tube was frozen by liquid nitrogen so as not to evaporate during a subsequent procedure . The amount of NBD was adjusted to make accurate AC/NBD weight ratios.…”
Section: Methodsmentioning
confidence: 99%
“…The following characterizations were done as described in ref : nitrogen adsorption/desorption, Raman spectroscopy, and XRD analyses; TEM and SEM observations. The Brunauer–Emmett–Teller (BET) specific surface area was calculated using the adsorption isotherm in a P / P 0 range of 0.05–0.20.…”
Section: Methodsmentioning
confidence: 99%
“…The structures of the redox-active materials hybridized within the pores of porous carbons seem to have an effect on the charge/discharge characteristics but cannot be identified by conventional spectroscopic and observation techniques because the amorphous structure of porous carbons hampers the observation of the confined materials, and conductive polymers and redox-active organic compounds consist of light elements. We have reported the existing form of the hybridized polydicyclopentadiene (PDCPD) within the pores of activated carbon (AC) by combining conventional structural characterizations with nitrogen adsorption/desorption and electrochemical measurements . The AC had micropores and mesopores below 4 nm, and PDCPD was not hybridized as a layer nor preferentially localized inside micropores but was uniformly distributed inside both micropores and mesopores as an agglomerate.…”
Norbornadiene (NBD) is adsorbed on activated carbon (AC), and the adsorbed NBD is polymerized within the pores of AC. Two kinds of ACs�AC-2 with only micropores of ∼2 nm and AC-4 with not only micropores but also mesopores below 4 nm�are examined to study the effects of the hybridized polynorbornadiene (PNBD) on the electric double-layer capacitor and hydrogen adsorption performance. Various measurements are performed to determine the form of the hybridized PNBD inside the pores of AC. Scanning and transmittance electron microscopy observations of the AC/PNBD hybrids confirm that PNBD is hybridized inside the pores of AC, and there is little PNBD on the surface of AC particles. The nitrogen adsorption/desorption measurement for the hybrids of AC-4 reveals that PNBD is not hybridized preferentially inside micropores rather than mesopores irrespective of the amount of PNBD. In addition, both micropore and mesopore volumes decrease at a constant rate with increasing amounts of PNBD. These results suggest that PNBD is hybridized not as a layer but as an agglomerate for both ACs, and the agglomerate delocalizes over the whole AC pores, which is supported by the results of electrochemical measurements and hydrogen adsorption behavior of the hybrids.
In this work development of structural and chemical properties of four nanoporous hybrid carbons has been presented. The carbons were synthesized by direct carbonization at 450, 600, 750 and 900 °C of the terpolymeric hybrid precursor composed of methacrylamide, divinylbenzene and trimethoxyvinylsilane and impregnated with sulfanilic acid (SA) as the surface modifier. The conditions of the carbonization process were set on the basis of the thermogravimetric analysis combined with FTIR analysis of the evolved gases (TGA-EGA). The use of SA contributed to the reduction of the carbonization temperature by about 100 °C and resulted in carbons with very uniform and bimodal porosity with the width range of about 1 and 14–28 nm. Spectral (ATR, Raman, XPS) and X-ray diffraction methods used to characterize the resulting carbon products allowed to define the gradual changes taking place in the morphological and chemical structure of the prepared materials. Cyclic and symmetrical structures of silicates species were gradually replaced by amorphous arrangements. At the same time, the increase in the sp2/sp3 carbon ratio from 1 to 65% proved progressive ordering and aromatization of the carbonized polymeric hybrid precursor. Some functional groups (e.g., N-containing) were built into carbon clusters forming pyridinic, pyrrolic and N-graphitic like structures, while others (e.g., carbonyls) were removed from the surface.
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