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Influence of evaporation drying on the porous properties of carbon/carbon composite xerogels
(2021-08-02)
Kraiwattanawong, Kriangsak
;
Sano, Noriaki
;
Tamon, Hajime
Carbon/carbon (C/C) composite xerogels dried by evaporation were prepared in this study to observe the change of their porous properties and their morphology by nitrogen sorption apparatus and a scanning electron microscope. Resorcinol and formaldehyde (RF) sols as a matrix phase and cotton fibers (CF) as a dispersed phase were mixed and gelated to be CF/RF composite hydrogels. The composite hydrogels were exchanged by t-butanol (TBA), dried by evaporation at 50◦C, and carbonized at 1000◦C to become the C/C composite xerogels. The results show that the CF addition does not decrease the mesoporous properties of the C/C composite xerogels. Moreover, the CF addition can alleviate the pore shrinkage, and it can maintain the mesopore structure. The mesopore size and the micropore size of C/C composites are insignificantly changed because the CF addition and the solvent exchange using TBA may suppress the pore shrinkage despite the gas-liquid interface existing during the evaporation drying.
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Investigation on porous properties of carbon/carbon composite cryogels by using weighted arithmetic mean
(2016-09-01)
Kraiwattanawong, Kriangsak
;
Sano, Noriaki
;
Tamon, Hajime
Cotton fibers (CF) and resorcinol and formaldehyde (RF) sol were used to synthesize composite cryogels. They were carbonized to prepare carbon/carbon (C/C) composite cryogels. In this work, the molar ratio of resorcinol to sodium carbonate (R/C), the mass concentration of resorcinol to distilled water (R/W) and the mass ratio of CF to RF (CF/RF) were changed as 100 and 200 mol/mol, 0.25 and 0.50 g/cm3 and 0.00 up to 0.64 g/g, respectively. The C/C composites were characterized by nitrogen adsorption and scanning electron microscopy. The results showed that the mesopore structure of C/C composites could be controlled by the adjustment of an R/W or R/C ratio. Moreover, the mean micropore sizes of C/C composite cryogels were kept equivalently to those of normal carbon cryogels. The weighted arithmetic mean was well applied to the BET surface area and micropore surface area of C/C composites with the deviation of about 21% for the high R/C ratio; however, it poor for the low R/C ratio. The weighted arithmetic mean also estimated the micropore volume of C/C composite cryogels with the deviation of about 20% for the CF/RF ratio smaller than 0.40 g/g. Moreover, the weighted arithmetic mean can be used as a guideline to estimate the mesopore volume.
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Capacitive performance of binder-free carbon/carbon composite cryogels
(2013-01-01)
Kraiwattanawong, Kriangsak
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Sano, Noriaki
;
Tamon, Hajime
A carbon/carbon (C/C) composite cryogel was prepared by pouring a resorcinol-formaldehyde (RF) sol into vials containing cotton fibers, followed by solvent exchange with t-butanol, freeze drying and pyrolysis under inert atmosphere. The porous properties of C/C composites were analyzed by nitrogen adsorption, and their mesopore texture was observed by a scanning electron microscope. The capacitive performance of C/C composites was also analyzed by galvanostatic charge/discharge method and cyclic voltammetry. The results demonstrate that the capacitance can be increased with the increase of amount of cotton fibers added to C/C composites, because the broader micropore size distribution and the carbon tunnels of C/C composites promote the charge propagation inside the pore structure. The suitable pore texture and the carbon tunnels can play the crucial role relevant to the high surface area in order to obtain the high capacitance value. © 2012 Elsevier Inc. All rights reserved.
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Carbon tunnels formed in carbon/carbon composite cryogels
(2012-05-01)
Kraiwattanawong, Kriangsak
;
Sano, Noriaki
;
Tamon, Hajime
A carbon/carbon (C/C) composite cryogel was prepared by putting almost the maximum content of cotton fibers in vials and then filling them with resorcinol-formaldehyde (RF) sols, followed by solvent exchange with t-butanol, freeze drying and pyrolysis under inert atmosphere. The mesopore structure of C/C composite cryogels was observed by a scanning electron microscope (SEM) and their porous structures were characterized by nitrogen adsorption and mercury porosimetry. The SEM images confirm that the C/C composite cryogels, being heterogeneous carbon materials, possess ordinary carbon cryogels and carbon tunnels. Here, the tunnels are comprised of (i) carbon fibers, (ii) spaces between carbon fibers and nanoporous carbon spheres, (iii) nanoporous carbon spheres with surrounding nanocages, and (iv) dense ring structures. The formation model of carbon tunnels is also proposed. The porous properties of cryogels could be changed by the cotton fiber addition and the synthesis conditions. The results support that the synthesis condition of RF sol determines the porous properties of C/C composite cryogels. © 2011 Elsevier Inc. All rights reserved.
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Low-cost production of mesoporous carbon/carbon composite cryogels
(2011-09-01)
Kraiwattanawong, Kriangsak
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Sano, Noriaki
;
Tamon, Hajime
A carbon/carbon (C/C) composite cryogel was prepared by dispersing cotton fibers (CF) in a resorcinol and formaldehyde (RF) sol, followed by solvent exchange with t-butanol, freeze drying and pyrolysis under inert atmosphere. The mass ratio of CF to RF was increased from 0% up to 25% to observe the mesopore structure change of C/C composites under a selected RF synthesis condition. The porous structures were characterized by nitrogen adsorption and mercury porosimetry, and their structure was observed by a scanning electron microscope (SEM). The mesopore diameter of the C/C composites increases slightly with the increase of CF content. The preparation can increase the mesopore volume and also reduce the production cost compared with carbon cryogels prepared without CF. The SEM images show that nanoporous gel spheres appeared after the freeze drying step. These spheres are converted to be nanoporous carbon spheres with surrounding nanocages, and CF are converted into carbon fibers at the same time by pyrolysis. © 2011 Elsevier Ltd. All rights reserved.
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HCl treatment on micropore and mesopore structures of carbon cryogels from resorcinol and formaldehyde
(2011-02-25)
Kraiwattanawong, Kriangsak
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Tamon, Hajime
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Praserthdam, Piyasan
The effect of HCl treatment on the porous properties of carbon cryogels synthesized from resorcinol and formaldehyde (RF) is investigated in this work. The treated and untreated carbon cryogels were analyzed with a nitrogen adsorption-desorption apparatus, scanning electron microscope (SEM) and high performance liquid chromatograph (HPLC). The results show that the HCl treatment can enlarge the micropore diameter which is advantageous to electric double layer capacitors, and can broaden the mesopore diameter, which is advantageous to mesoporous carbon supports of catalysts. The micropore volume, mesopore volume and weight loss of the carbon cryogel are not significantly changed by the HCl treatment. Moreover, SEM images and HPLC chromatograms support that the HCl treatment can promote the Ostwald ripening effect for RF carbon cryogels. © 2011 The Society of Chemical Engineers, Japan.
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Influence of solvent species used in solvent exchange for preparation of mesoporous carbon xerogels from resorcinol and formaldehyde via subcritical drying
(2011-02-01)
Kraiwattanawong, Kriangsak
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Tamon, Hajime
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Praserthdam, Piyasan
Carbon cryogels are dried by 3 days of freeze drying with 6 h of pre-freezing whereas the carbon xerogels are prepared by 1 day of subcritical drying in the selective range of synthesis condition, but the mesoporosity of carbon xerogels are not well controlled. This research is to study the influence of solvent species in the solvent exchange for the preparation of carbon xerogels cooperated by the evaporation drying and the vacuum drying. The good solvent for the high mesoporous properties of carbon xerogels is desirable in the wide range of synthesis condition. The carbon xerogels prepared from resorcinol and formaldehyde were characterized by the nitrogen adsorption apparatus and the field emission scanning electron microscope (FE-SEM). The results illustrate that the mesoporous carbon xerogels in the two subcritical dryings can be easily prepared by solvent exchange. Among the solvents, t-butanol allows the great results in the preparation of high mesoporous carbon xerogels and is well applied in the wide range of synthesis conditions. The FE-SEM images elucidate that the carbon xerogels dried by the vacuum drying contain the particles interconnection larger than the evaporation drying. © 2010 Elsevier Inc. All rights reserved.
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Control of mesoporous properties of carbon cryogels prepared from wattle tannin and furfural
(2008-12-01)
Kraiwattanawong, Kriangsak
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Mukai, Shin R.
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Tamon, Hajime
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Lothongkum, Anchaleeporn W.
Wattle tannin-furfural (TFu) carbon cryogels are synthesized by sol-gel polycondensation of wattle tannin with furfural by using sodium hydroxide (NaOH) as a catalyst, dried by freeze-drying technique and then pyrolyzed under inert atmosphere, respectively. The amounts of wattle tannin (T), furfural (Fu), NaOH (C) and distilled water (W) are changed for preparing the mesoporous TFu carbon cryogels. The mole ratio of tannin to catalyst T/C plays a crucial role for the synthesis of TFu organic and carbon cryogels. The results suggest that the T/C ratio should be above 0.25 but <1.0 to prepare the mesoporous and homogeneous cryogels. Although TFu carbon cryogels have the broad mesopore size distribution, the mesoporous structure is controllable by the synthesis conditions. The carbon cryogels possess the mesopore volume less than 0.56 cm3/g and the BET surface area less than 600 m2/g. Moreover, the ratio of catalyst to water C/W can be used to prepare the homogeneous and mesoporous carbon cryogels, and to control the mesopore radius of carbon cryogels in the range of 1.6-9.6 nm. © 2007 Springer Science+Business Media, LLC.
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Improvement of mesoporosity of carbon cryogels by acid treatment of hydrogels
(2008-11-01)
Kraiwattanawong, Kriangsak
;
Mukai, Shin R.
;
Tamon, Hajime
;
Lothongkum, Anchaleeporn W.
Wattle tannin-furfural (TFu) gels are synthesized by the sol-gel polycondensation of wattle tannin with furfural by using sodium hydroxide as a catalyst and cured at 363 K. After cured, the TFu hydrogels are treated in hydrochloric acid (HCl) solutions with various variables as follows: aging temperature, HCl concentration and pH. TFu cryogels aged are then freeze-dried and pyrolyzed under an inert atmosphere to obtain TFu carbon cryogels. The TFu and carbon cryogels were characterized by N<inf>2</inf> adsorption and scanning electron microscope. The high HCl concentration yields the increase of mesopore volume almost twice especially at high temperature and the mesopore size distribution can be greatly developed sharper and narrower when the high concentration of HCl or/and the high temperature are used. Moreover, this method is the versatile approach for developing the mesopore structure of the low and high porous TFu hydrogels and has no serious problem of weight loss after treatment. © 2008 Elsevier Inc. All rights reserved.

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