Energy Fuels 2010, 24, 33343339

Published on Web 02/26/2010

: DOI:10.1021/ef901465j

Exploring New Routes in the Synthesis of Carbon Xerogels for Their Application in
Electric Double-Layer Capacitors
E. G. Calvo, C. O. Ania, L. Zubizarreta, J. A. Men
endez, and A. Arenillas*
Instituto Nacional del Carb

on, Consejo Superior de Investigaciones Cientficas (CSIC), Apartado 73, 33080 Oviedo, Spain
Received December 2, 2009. Revised Manuscript Received February 11, 2010

Resorcinol-formaldehyde carbon xerogels were prepared by means of two different synthesis methods:
conventional (C) and microwave heating (MW). The influence of the heating method and the pH of the
precursor solution on the textural and chemical properties of the carbon xerogels was investigated. It was
found that by modifying the initial pH, it is possible to control the porosity of carbon xerogels independent
of the heating method used. The electrochemical performance of a selection of synthesized carbon xerogels
as electrode materials in electric double-layer capacitors was studied by cyclic voltammetry and charge/
discharge experiments in an acidic medium (1 M H2SO4). The electrochemical performance of the carbon
xerogels was compared to that of an activated carbon commercialized for this application (Norit Super
DLC-50), and it can be seen that the carbon xerogels display similar specific capacitances to those of the
commercial carbon. Moreover, carbon xerogels have a good cycle durability after 18 000 galvanostatic
cycles, with a drop in specific capacitance of around 10%. This excellent cycle durability, together with the
attractive properties of carbon xerogels and the saving of time and energy achieved with microwaveassisted synthesis, would make resorcinol-formaldehyde carbon xerogels promising materials for
applications of an electric double-layer capacitor (EDLC).

The synthesis of carbon gels from the polycondensation of

resorcinol and formaldehyde involves three steps: (i) gel
synthesis, where the stages of gelation and curing take place,
(ii) drying of the gel saturated with solvent, and finally,
(iii) carbonization of organic gel to obtain carbon gel. With
regard to the drying step, several methods can be used, each of
which producing materials with different characteristics.
Nowadays, the most widely studied drying methods are
supercritical drying, freeze-drying, and evaporative drying.
The carbon gels obtained are referred to as aerogels, cryogels,
and xerogels, respectively.13 Among these methods, evaporative drying is the simplest and most rapid method.
Despite the advantages of carbon gels, the main obstacle to
their application at the industrial level is the long time required
for their production, because several days are needed for the
processes of gelation, curing, and drying to be completed by
conventional methods. It is therefore necessary to find alternative techniques to reduce the synthesis time and make
carbon gels competitive with respect to other materials that
are used as electrodes in supercapacitors (i.e., activated
carbons). In a previous work by our research group,14 microwave drying was used to obtain organic gels, resulting in a
considerable savings of time and energy compared to conventional drying (i.e., using a conventional oven). However, it still
took 3 days for the polycondensation of resorcinol and
formaldehyde (i.e., gelation and curing steps) to take place.
Kang et al.15 used microwave radiation during the stages of
gelation and aging in a microwave digestion system at 120 C

1. Introduction
Carbon gels have been extensively studied over the past few
decades because of their great potential and versatility.1,2 Their
textural and structural characteristics can be controlled according to the synthesis and processing conditions; thus, the main
advantage of carbon gels is the possibility of tailoring their properties to fit specific applications.3,4 For this reason, carbon gels
are used in a wide range of applications, including catalysis,5,6
adsorption,7,8 and energy storage.9,10 In this last application,
carbon gels are considered perfect materials for their use as
electrodes in energy storage devices because of their high specific
surface area and pore volume, low density, and high electrical
conductivity.11 In addition, these materials can be obtained in
diverse forms, such as monoliths, powder, films, microspheres,
etc., which is another reason for their wide applicability.12

This paper has been designated for the special section Carbon for Energy
Storage and Environment Protection.
*To whom correspondence should be addressed. E-mail: aapuente@
incar.csic.es.
(1) Lin, C.; Ritter, J. A. Carbon 1997, 35, 12711278.
(2) Mahata, N.; Pereira, M. F. R.; Su
arez-Garc a, F.; Mart nezAlonso, A.; Tasc

on, J. M. D.; Figueiredo, J. L. J. Colloid Interface
Sci. 2008, 324, 150155.
(3) Al-Muhtaseb, S. A.; Ritter, A. Adv. Mater. 2003, 15, 101113.
(4) Job, N.; Th
ery, A.; Pirard, R.; Marien, J.; Kocon, L.; Rouzaud,
J. N.; B
eguin, F.; Pirard, J. P. Carbon 2005, 43, 24812494.
(5) Job, N.; Heinrichs, B.; Ferauche, F.; Noville, F.; Marien, J.;
Pirard, J. P. Catal. Today 2005, 102-103, 234241.
(6) Job, N.; Heinrichs, B.; Lambert, S.; Pirard, J. P.; Colomer, J. F.;
Vertruyen, B.; Marien, J. AIChE J. 2006, 52, 26632676.
(7) Jayne, D.; Zhang, Y.; Shaker, H.; Erkey, C. Int. J. Hydrogen
Energy 2005, 30, 12871293.
(8) Kang, Y. K.; Lee, B. I.; Lee, J. S. Carbon 2009, 47, 11711180.
(9) Frackowiak, E.; B
eguin, F. Carbon 2001, 39, 937950.
(10) Fang, B.; Binder, L. J. Power Sources 2006, 163, 616622.
(11) Schmit, C.; Probstle, H.; Fricke, J. J. Non-Cryst. Solids 2001, 285,
277282.
(12) Al-Muhtaseb, S. A.; Ritter, A. Adv. Mater. 2003, 15, 101104.

r 2010 American Chemical Society

(13) Zubizarreta, L.; Arenillas, A.; Pirard, J. P.; Pis, J. J.; Job, N.
Microporous Mesoporous Mater. 2008, 115, 480490.
(14) Zubizarreta, L.; Arenillas, A.; Men
endez, J. A.; Pis, J. J.; Pirard,
J. P.; Job, N. J. Non-Cryst. Solids 2008, 354, 40244026.
(15) Kang, K. Y.; Hong, S. J.; Lee, B. I.; Lee, J. S. Electrochem.
Commun. 2008, 10, 11051108.

3334

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Energy Fuels 2010, 24, 33343339

: DOI:10.1021/ef901465j

Calvo et al.

for 1 h, but the drying step was performed in a vacuum oven at

60 C, with the resulting prolongation of synthesis time. In
addition, these carbon gels were ammonia-assisted carbonized
to improve their properties for specific applications.
In the present work, microwave radiation was used in the
global synthesis of organic xerogels; therefore, the gelation,
aging, and drying of the samples were carried out in one single
device.16 The carbon xerogels obtained by microwave heating
were compared to conventionally synthesized carbon xerogels
by studying their textural and chemical characteristics. Their
electrochemical performance as electrode materials in electric
double-layer capacitors (EDLCs) was also investigated using
a selection of samples obtained by both heating methods.

at saturation, Vp, matches the total pore volume of the material,

VT. However, in the case of materials with macropores, the total
pore volume cannot be determined exclusively from the nitrogen
adsorption data. For this kind of material, mercury porosimetry
was used to determine the total pore volume and the average
mesopore diameter, dm. Mercury porosimetry measurements
were performed using a Micromeritics AutoPore IV, and they
are limited to pores larger than 5.5 nm. The total pore volume,
VT, was then estimated as the sum of VHg and Wo-N2.
The chemical properties of the samples were determined by
means of elemental analysis and temperature-programmed
desorption (TPD) experiments. The C, N, H, and S were
evaluated on a LECO-CHNS-932 microanalyzer, and the oxygen content was determined directly using a LECO-TF-900
furnace. To evaluate the amount and type of oxygen functionalities, TPD analyses in an automatic chemisorption analyzer,
Micromeritics Autochem II, were carried out under an inert
atmosphere (Ar) with a flow rate of 50 cm3 min-1. The samples
were heated to 1000 C at a rate of 10 C min-1, and the
decomposition products (CO and CO2) were identified by means
of an online Onmistar Pfeiffer mass spectrometer.
2.3. Electrode Preparation. The carbon electrodes were prepared according to the following procedure. A slurry with the
carbon xerogel, binder, and carbon black was prepared in
acetone and homogenized in a mortar. The mass ratio of the
reagents was 70 wt % carbon xerogel, 25 wt % poly(vinylidene
fluoride) (PVDF, Sigma-Aldrich), and 5 wt % carbon black.
The electrodes were prepared in the form of pressed pellets, with
a diameter of 10 mm. Afterward, the electrodes were dried in an
oven at 60 C for 2 h to remove the acetone. The mass of each
electrode was around 10-15 mg. Before performing any measurement, the carbon xerogel electrodes were placed in an excess
of 1 M H2SO4 electrolyte solution overnight, to ensure the
complete wetting of the electrode porosity by the electrolyte.
2.4. Electrochemical Measurements. All of the electrochemical
tests were carried out in a Biologic multichannel potentiostat at
room temperature, employing a solution 1 M H2SO4 as the
electrolyte. The capacitors were constructed using a Teflon
Swagelok-type cell formed by two carbon electrodes of comparable mass (10-15 mg), electrically isolated by a glassy fibrous
separator. The specific capacitance was evaluated by cyclic
voltammetry at different scan rates in a voltage range of 0.8 V
and by galvanostatic charge/discharge cycles at several current
densities (50 and 500 mA g-1) within the same voltage window
(0.8 V). The gravimetric capacitance (C) expressed in farads per
gram of carbon material (F g-1) was estimated using voltammetry at a scan rate of 2-100 mV s-1 and galvanostatic charge/
discharge at current densities between 50 and 500 mA g-1. To
assess the long-term electrochemical stability of the samples,
charge/discharge tests at a current load of 200 mA g-1 were
carried out up to 18 000 galvanostatic cycles. In addition, the
carbon xerogels were electrochemically characterized by means
of cyclic voltammetry tests at 2 mV s-1 in a Teflon threeelectrode cell, using a carbon xerogel pellet as the working
electrode, a graphite rod as the counter electrode, and Hg/
Hg2SO4 as the reference electrode.

2. Experimental Section
2.1. Synthesis of Organic and Carbon Xerogels. Aqueous
organic xerogels were synthesized by the polycondensation of
resorcinol (R) and formaldehyde (F) solubilized in water. A
sodium hydroxide solution (1.0 M) was used as the basification
agent. Resorcinol (VWR International, 99%) was first dissolved
in deionized water in a sealed flask under magnetic stirring.
Once a dissolution was obtained, formaldehyde (Aldrich,
37 wt % in water, stabilized by 10.7 wt % methanol) was added
under stirring. In all cases, the molar ratio of resorcinol/formaldehyde (R/F) was kept at 0.5, and the dilution ratio, D (i.e.,
the total solvent/reactant molar ratio) was fixed at 5.7. Four
different organic xerogels were prepared, varying the pH of the
initial solution between 5.8 and 6.5, adjusted by the addition of
the NaOH solution. In the case of the conventional synthesis (C
series), the solutions were heated in an oven at 85 C for 72 h for
gelation and curing to take place and the organic gels were then
dried by evaporation of the solvent at 150 C for 24 h. The
synthesis of organic xerogels by means of microwave heating
(MW series) was carried out as follows: the solutions were
placed in a microwave oven at 40 C to undergo gelation.
Afterward, the temperature was increased to 60 C for curing
and drying. The final drying of the samples was controlled by
weight stabilization, and the time employed for the whole
synthesis was approximately 3-4 h. Because of the rapidity of
the process in the microwave oven, it is only possible to
appreciate the point at which the solution loses fluidity and
gel formation occurs. However, the curing and drying steps are
not easy to distinguish.
All of the organic gels prepared (i.e., the C and MW series)
were pyrolyzed at 800 C under nitrogen flow in a horizontal
tube reactor according to a heating program described elsewhere.13 The carbon xerogels (carbonized organic gels) were
designated as follows: C or MW, depending upon the heating
mechanism used, followed by the pH of the resorcinolformaldehyde aqueous solution.
2.2. Evaluation of the Textural and Chemical Properties of the
Samples. The textural properties of the carbon xerogels were
evaluated by means of N2 adsorption-desorption isotherms at
-196 C and CO2 adsorption isotherms at 0 C, in a Micromeritics Tristar 3000. The micropore volume was evaluated by
applying the Dubinnin-Raduskevich equation to the CO2 (WoCO2) and N2 (Wo-N2) adsorption isotherms, and the total pore
volume (VP) was calculated from the adsorbed volume at
saturation.17 The Brunauer-Emmett-Teller (BET) surface
area (SBET) was estimated from the nitrogen adsorption isotherms.18 If the samples are micro/mesoporous, the pore volume

3. Results and Discussion

3.1. Textural and Chemical Characteristics of the Synthesized Carbon Xerogels. The N2 adsorption-desorption isotherms of the synthesized carbon xerogels are shown in
Figure 1. The isotherms of the samples synthesized with an initial pH of 6.5 (both conventional and microwave heating) are
a combination of type I and type IV according to the Brunauer, Deming, Deming, and Teller (BDDT) classification,19

(16) Arenillas, A.; Men
endez, J. A.; Zubizarreta, L.; Calvo, E. G.

Patent ES-200930256, 2009.
(17) Dubinnin, M. M. In Progress in Surface and Membrane Science;
Danielli, J. F., Rosenberg, M. D., Cadenhead, D., Eds.; Academic Press: New
York, 1975; Vol. 9, pp 1-70.
(18) Parra, J. B.; de Sousa, J. C.; Bansal, R. C.; Pis, J. J.; Pajares, J. A.
Adsorpt. Sci. Technol. 1995, 12, 5166.

(19) Brunauer, S.; Deming, L. S.; Deming, W. E.; Teller, E. J. Am.

Chem. Soc. 1940, 62, 17231732.

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Energy Fuels 2010, 24, 33343339

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Calvo et al.
Table 2. Chemical Composition of the Synthesized Carbon Xerogels
and the Commercial Activated Carbon, Norit Super DLC-50
elemental analysis (wt %, dry ash-free basis)

Table 1. Textural Properties of the Carbon Xerogels Studied

SBET
(m2 g-1)

Wo-N2a
(cm3 g-1)

Wo-CO2a
(cm3 g-1)

VTb
(cm3 g-1)

dmc
(nm)

C-5.8
C-6.5
MW-5.8
MW-6.5
DLC-50

671
677
648
594
1612

0.26
0.26
0.25
0.22
0.56

0.24
0.22
0.25
0.22
0.28

1.72
0.83
0.91
0.44

38
9
24
9

96.0
96.9
92.7
95.2
92.9

1.3
1.2
1.7
1.4
1.1

2.6
1.7
5.4
3.2
5.4

0.1
0.2
0.2
0.2
0.6

properties of the commercial activated carbon are also

shown in Table 1.
As mentioned above, conventional and microwave heating
generate a similar microporosity. The micropore volumes obtained by applying the Dubinnin-Raduskevich method to the
nitrogen and carbon dioxide adsorption isotherms are very
similar in the C and MW series. In the case of mesoporosity,
conventional heating produces higher mesopore volumes (i.e.,
VT of 1.72 and 0.91 nm for samples C-5.8 and MW-5.8,
respectively). However, it should be kept in mind that the use
of a rapid and simple method for the preparation of carbon
xerogels is a huge advantage, especially from the point of view of
scaling up the process. Moreover, it is necessary to point out that
the microwave method has yet to be fully optimized and, in this
work, is only presented as a very promising synthesis option.
The elemental analysis data (Table 2) indicate that the carbon
materials studied consist mainly of carbon (between 93 and 97%
in the case of the carbon xerogels and 93% for the activated
carbon) and small quantities of oxygen (2-5%). With regard to
the carbon xerogels, the oxygen content is higher in the samples
prepared by microwave heating (i.e., 2.6 and 5.4 wt % for
samples C-5.8 and MW-5.8, respectively), and this is in agreement with previous work.20 The higher oxygen content of the
samples treated in the microwave oven (MW-5.8 and MW-6.5)
can be attributed to secondary reactions that occur during the
synthesis with microwave radiation, which produce higher
cross-linked organic xerogels with more stable oxygen functionalities.21 A deep analysis of the oxygenated surface functionalities of the xerogels was carried out by TPD. The corresponding
CO and CO2 profiles are shown in Figure 2. It is generally
accepted that, as a result of heat treatment, oxygen-containing
functional groups decompose into CO and CO2. Thus, weight
loss can be linked to the chemical functionalities present on the
surface. Evolution of CO2 between 200 and 600 C is due to
decomposition of labile groups (i.e., carboxylic acid), whereas
phenols and other basic groups (quinones and pyrone-like structures) decompose as CO at temperatures higher than 600 C.22
Data shown in Figure 2 indicate that the two synthetic routes
produce analogous kinds of oxygen functionalities. In all cases,
CO evolves in larger amounts than CO2, indicating that most of
the surface functionalities are non-labile groups. Moreover,
according to the decomposition temperatures of the CO desorption profiles (see Figure 2a), they can be assigned mostly to
quinones and phenol-type groups. The CO2 desorption peak
centered at about 200 C is, in all cases, almost negligible,
especially for sample DLC-50.
3.2. Electrochemical Characterization of the Samples. Electrochemical characterization of samples C-6.5, MW-6.5, and
DLC-50 was carried out in a three-electrode configuration. Figure 3 shows the cyclic voltammograms recorded at

Figure 1. Nitrogen adsorption-desorption isotherms of the carbon

xerogels obtained by conventional (C) and microwave heating
(MW) and the commercial activated carbon, Norit Super DLC-50.

sample

sample
C-5.8
C-6.5
MW-5.8
MW-6.5
DLC-50

Obtained by applying the Dubinnin-Raduskevich method to the N2

and CO2 adsorption isotherms. b Total volume of pores estimated by
mercury porosimetry and the Dubinnin-Raduskevich method: VT =
VHg Wo-N2. cAverage mesopore diameter calculated from mercury
porosimetry.

corresponding to micro/mesoporous materials. In contrast,

when the pH of the precursor solution was fixed at 5.8, the
isotherms exhibit a large increase in the volume of nitrogen
adsorbed at relative pressures above 0.8, indicating the
presence of a large volume of mesopores of larger sizes
compared to the xerogels prepared at pH 6.5 and even
macropores. The microporosity is similar in all cases according to the N2 adsorption at low relative pressure, whereas the
mesoporosity differs slightly. The hysteresis loop of the N2
adsorption-desorption isotherms is smaller in the case of the
samples obtained by microwave heating, indicating a lower
volume of mesopores. For comparison purposes, Figure 1
also shows the nitrogen adsorption isotherm of the commercial activated carbon DLC-50. This sample presents a type-I
isotherm, characteristic of a microporous material.
Table 1 summarizes the main textural parameters of the
two series of carbon xerogels (C and MW) evaluated from
the gas adsorption data and mercury porosimetry. As can be
seen from this table, it is possible to control the pore texture
of the carbon xerogels by adjusting the pH of the initial solution. Both the specific surface area and microporosity are
barely affected by the pH of the resorcinol-formaldehyde
aqueous solution, unlike mesoporosity, which is strongly
influenced by it. As the initial pH increases, the total pore
volume and mesopore size decrease, regardless of the heating
mechanism employed (i.e., VT of 1.72 and 0.83 nm for
samples C-5.8 and C-6.5 and VT of 0.91 and 0.44 nm for
samples MW-5.8 and MW-6.5, respectively). The textural

(20) Zubizarreta, L.; Arenillas, A.; Dom nguez, A.; Men
endez, J. A.;
Pis, J. J. J. Non-Cryst. Solids 2008, 354, 817825.
(21) Caddick, S. Tetrahedron 1995, 51, 1040310432.
(22) Otake, Y.; Jenkins, R. G. Carbon 1993, 31, 109121.

3336

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Calvo et al.

Figure 2. (a) CO and (b) CO2 TPD profiles of the carbon materials studied.

Figure 3. Cyclic voltammograms in a three-electrode cell using Hg/Hg2SO4 and graphite as reference and counter electrodes, respectively. Scan
rate = 2 mV s-1.

2 mV s-1 and at two different potential ranges using the carbon

materials as working electrode and Hg/Hg2SO4 and a graphite
rod as reference and counter electrodes, respectively.
When the carbon xerogels are exposed to polarization
between -600 and 200 mV versus Hg/Hg2SO4, a purely
capacitive behavior is observed (reversible charge/discharge
of the double layer), which is confirmed by the quasirectangular shape of the voltammogram. If the potential is
extended to more negative potentials (i.e., -1 V versus Hg/
Hg2SO4), the response is different (Figure 3b). At potentials
below -800 mV versus Hg/Hg2SO4, there is a rapid rise in the
current related to the reduction of water and nascent hydrogen starts to form. For the anodic sweep, the potential was
limited to 300 mV versus Hg/Hg2SO4 because higher
anodic values might cause oxidation of the materials.23
In contrast, the cyclic voltammograms of the commercial
activated carbon deviate from the rectangular shape and
show two wide reversible humps. These are caused by redox
transfer reactions involving the oxygen-containing functionalities in the carbon matrix. This behavior is consistent with

the higher oxygen content of this activated carbon compared

to that of the xerogels obtained at pH 6.5. The appearance of
the humps is even more pronounced when the potential
values are extended from -1000 to 300 mV versus Hg/
Hg2SO4 (Figure 3b). The position of the cathodic and anodic
peaks confirms the existence of the quinone/hydroquinone
pair (reduction potential close to -0.15 V versus Hg/Hg2SO4
for carbons in various environments.23
3.3. Electrochemical Performance of the Materials Studied.
The potential-time curves obtained by galvanostatic
charge/discharge of the electrochemical capacitors constructed using the carbon xerogels and the commercial activated carbon are presented in panels a and b of Figure 4. As
mentioned above, the charge/discharge tests were performed
at several current loads (50-500 mA g-1), in a voltage range
of 0.8 V, but only the curves obtained at 50 and 500 mA g-1
are included in this work. Similar to other authors that have
observed the case of carbon aerogels24 and cryogels,25 the
(24) Li, J.; Wang, X.; Wang, Y.; Huang, Q.; Dai, C.; Gamboa, S.;
Sebastian, P. J. J. Non-Cryst. Solids 2008, 354, 1924.
(25) Seperih, S.; Garc a, B. B.; Zhang, Q.; Cao, G. Carbon 2009, 47,
14361443.

(23) Kinoshita, K. Carbon: Electrochemical and Physicochemical

Properties; Wiley: New York, 1988; p 293.

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Energy Fuels 2010, 24, 33343339

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Calvo et al.

Figure 4. Galvanostatic charge/discharge cycles for carbon materials C-6.5, MW-6.5, and DLC-50 performed at a current load of (a) 50 mA g-1
and (b) 500 mA g-1. Voltage window = 0.8 V.

Figure 5. Specific capacitance, C (F g-1), for the carbon xerogels

and the activated carbon, Norit Super DLC-50, as a function of the
scan rate (mV s-1). The electrolyte used was 1 M H2SO4, and the
voltage range was 0-0.8 V.

Figure 6. Variation of the specific capacitance with the number of

galvanostatic cycles performed for samples C-6.5 and MW-6.5.
Current density, 200 mA g-1; voltage window, 0-0.8 V.

as the xerogels (Table 1). Another fact that stands out is the
variation of specific capacitance with the scan rate that is
lower when the carbon xerogel C-6.5 was used as the
electrode material, which could be related to its higher
narrow mesopore volume compared to the other samples
studied.26,27 As the scan rate increases, the ions of the
electrolyte have a shorter time to spread into the smaller
micropores, so that narrow mesopores acquire a greater role
in the process of charge storage. In summary, the carbon
xerogels prepared appear to have promising electrochemical
properties for their use as electrodes in supercapacitors.
A factor that seriously limits the application in electrochemical devices of high-surface area carbon materials is the
long-term stability of the capacitor.28,29 To confirm the good
performance of the carbon xerogels synthesized in this work,
we tested their stability using galvanostatic long-term cycling. Figure 6 shows the variation of the specific capacitance
values with the number of galvanostatic cycles carried out at
200 mA g-1 in a voltage range of 0.8 V. The carbon xerogels
studied showed excellent cycle durability, because the capacitance fading after 18 000 cycles was very low for both

curves present a quasi-triangular shape, suggesting the absence of pseudo-capacitance. This is in agreement with the
results of the electrochemical characterization of the carbon
xerogels in the three-electrode configuration (Figure 3a).
However, from the electrochemical characterization of the
activated carbon DLC-50, pseudo-capacitance was clearly
observed (see panels a and b of Figure 3). It can also be seen
from Figure 4a that the ohmic drop is relatively limited in all
of the samples, which demonstrates the ability of quick
charge propagation in the synthesized carbon xerogels,
similar to that of a commercial carbon. When the galvanostatic charge/discharge tests were performed at higher current load (Figure 4b), the carbon xerogel C-6.5 shows a
negligible ohmic drop, whereas the samples MW-6.5 and
DLC-50 exhibit a higher ohmic drop than their counterparts
at 50 mA g-1.
To evaluate the degree of dependency of specific capacitance on the scan rate, cyclic voltammetry tests were recorded at several scan rates, between 2 and 100 mV s-1
(Figure 5), using samples C-6.5, MW-6.5, and DLC-50 as
electrode materials. At a low scan rate, the commercial
activated carbon displays a higher specific capacitance (i.e.,
190 F g-1) than the synthesized carbon xerogels (i.e., 155 and
113 F g-1 for samples C-6.5 and MW-6.5, respectively), but it
must be remembered that the activated carbon was compared to non-activated samples. In fact, the activated carbon
has about twice as much surface area and micropore volume

(26) Li, W.; Reichenauer, J.; Fricke, J. Carbon 2002, 40, 29552959.
(27) Pandolfo, A. G.; Hollenkamp, A. F. J. Power Sources 2006, 157,
1127.
(28) Portet, C.; Taberna, P. L.; Simon, P.; Flahaut, E.; LabertyRobert, C. Electrochim. Acta 2005, 50, 41744181.
(29) Khomenko, V.; Raymundo-Pi~
nero, E.; B
eguin, F. J. Power
Sources 2008, 177, 643651.

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Calvo et al.

materials, representing a fall of around 12% in the case of

conventional heating and only 6% in the case of microwave
radiation. Similar results has been reported by other authors
using an activated carbon as the electrode material.28,29

energy (i.e., synthesis time of 3-4 h under microwave radiation compared to several days by conventional heating).
Although it is necessary to optimize this novel method to
obtain carbon xerogels with a better textural development
and electrochemical performance, the use of microwave
radiation to synthesize carbon xerogels leads to promises of
more rapid progress toward their implementation on an
industrial scale.

4. Conclusions
In this work, an ultra-fast and low-cost microwave-assisted
heating method was used to prepare resorcinol-formaldehyde aqueous gels. The textural, structural, and electrochemical properties of the carbon xerogels obtained were compared to those of conventionally synthesized carbon xerogels.
The results show that microwave radiation produces carbon
xerogels with comparable characteristics to those of conventional heating but with an enormous savings of time and

Acknowledgment. The support from the Government of Principado de Asturias PCTI (IB09-00201) and the Ministerio de
Ciencia e Innovaci

on (MAT2008-00217/MAT) is greatly acknowledged. E. G. Calvo also acknowledges a predoctoral
research grant from Fundaci

on para el Fomento en Asturias de
la Investigaci

on Cient fica Aplicada y la Tecnolog a (FICYT).

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