Journal of Colloid and Interface Science 386 (2012) 285–290

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Journal of Colloid and Interface Science

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Effect of exfoliation temperature on carbon dioxide capture of graphene nanoplates

Long-Yue Meng, Soo-Jin Park ⇑
Korea CCS R&D Center, Korea Institute of Energy Research, 152 Gajeongro, Yuseoung-gu, Daejeon 305-343, South Korea
Department of Chemistry, Inha University, 100 Inharo, Nam-gu, Incheon 402-751, South Korea

a r t i c l e i n f o a b s t r a c t

Article history: Thermally exfoliated graphene nanoplates were found to be a novel high efficiency sorbent for the cap-
Received 3 April 2012 ture of CO2. The exfoliated graphene nanoplates were expanded successfully from graphite oxide by a
Accepted 3 July 2012 low-heat treatment at temperatures ranging from 150 to 400 °C under vacuum conditions. The texture
Available online 16 July 2012
was analyzed by N2 full isotherms and XRD. The CO2 capture characteristics of the graphene nanoplates
at 25 °C and 30 bar were examined using a pressure–composition–temperature apparatus. The inter-
Keywords: layer spacing of the graphene layers and pore structure on the CO2 capture capacities were studied as
CO2 capture
a function of the processing conditions. The prepared graphene nanoplates exhibited high capture capac-
Thermally exfoliation
Graphene nanoplates
ities, up to 248 wt.%, at 25 °C and 30 bar. The improved CO2 capture capacity of the graphene nanoplates
was attributed to the larger inter-layer spacing and higher interior void volume.
Crown Copyright Ó 2012 Published by Elsevier Inc. All rights reserved.

1. Introduction relatively moderate strength, easier desorption, and thermal stabil-

Recently, increasing CO2 emission due to industrialization is a
global environmental problem that has attracted increasing atten-
tion [1]. Carbon capture and storage (CCS) (carbon capture and
sequestration) projects refer to technology attempting to prevent
the release of large quantities of CO2 into the atmosphere from fos-
sil fuel use in power generation and other industries [2]. As a re-
sult, current or proposed research into CO2 capture from flue gas
focused on absorption, adsorption (porous materials), cryogenic
distillation, and membrane separation [3–6].
Among those methods, the technology currently considered as
mature is CO2 absorption by amine based liquids [3]. This technol-
ogy, however, is expensive and energy intensive. Therefore, im-
proved technologies for CO2 adsorption are necessary to achieve
low energy consumption [7]. CO2 adsorption is typically performed
at a final polishing step in a hybrid CO2 capture system [8,9]. Pre-
viously, pressure swing adsorption (PSA) is one of the potential
techniques that can be applicable to the removal of CO2 from high
pressure gas streams.
Up to now, different types of adsorbents have been used in CO2
PSA, such as zeolites, activated carbons, silica gel, metal–organic
frameworks (MOFs), and porous organic polymers [10–15]. Acti-
vated carbons generally have higher CO2 adsorption capacity than
zeolite-like materials at pressures greater than atmospheric pres-
sure due to surface hydrophobicity, extended surface area,
⇑ Corresponding author. Address: Department of Chemistry, Inha University, 100
Inharo, Nam-gu, Incheon 402-751, South Korea. Fax: +82 32 860 8438.
E-mail address: sjpark@inha.ac.kr (S.-J. Park).
ity [12]. Up to now, previous studies have focused on the use of
activated carbon, activated carbon fibers, carbon molecular sieves,
carbon nanotubes, and graphene as adsorbents for CO2 capture
[11,16–19].
Graphene is a very important carbon material that has attracted
considerable attention owing to its high aspect ratio, small radius
of curvature, high mechanical strength, unique electrical proper-
ties, and chemical stability [20,21]. In recent years, there has been
increasing interest in graphene-based materials for use as sorbents
in energy and environment-related applications because the highly
ordered pores confined geometry in carbon nanostructures, poros-
ity, and accessible surface area [18,22–26]. On the other hand, few
studies have examined CO2 adsorption on graphene because of its
higher specific surface area than other carbon materials.
Modifications of graphene oxide layers by targeting hydroxy
and epoxy surface functional groups with both organic and inor-
ganic compounds can increase the interlayer spacing of graphene
oxide layers [27]. For example, Srinivas et al. reported the synthesis
of a range of porous graphene oxide frameworks (specific surface
area = 470 m2/g) through the expansion of graphene oxide sheets
with a range of linear boronic acid pillaring units in a solvothermal
reaction [18]. Although the chemical modification and chemical
reduction approach can remove most of the oxygen atoms from
the surface of graphene oxide, some remaining oxygen atoms
and additional functional groups introduced during chemical mod-
ification or reduction might cause the scattering of electrons,
which decreases the structural instability and thermal stability.
In addition, these methods are very expensive and energy intensive
for large-scale preparation.

0021-9797/$ - see front matter Crown Copyright Ó 2012 Published by Elsevier Inc. All rights reserved.
http://dx.doi.org/10.1016/j.jcis.2012.07.025
286 L.-Y. Meng, S.-J. Park / Journal of Colloid and Interface Science 386 (2012) 285–290
Therefore, it is essential to develop a more effective method to
prepare graphene sheets with high gas adsorption capacity. To
date, several methods have been used to obtain a high specific sur-
face area of graphene, including heat treatment at high tempera-
tures and vacuum conditions [26–31]. Ruoff et al. reported the
KOH activation of microwave exfoliated graphene oxide and ther-
mally exfoliated graphene oxide to achieve a specific surface area
up to 3100 m2/g [30,31].
In this study, thermally exfoliated graphene nanoplates were
prepared using a novel high efficiency sorbent for the capture of
CO2. The exfoliated graphene nanoplates were expanded success-
fully from graphite oxide by a low-heat treatment over the temper-
ature range, 150–400 °C, under vacuum conditions.
2. Experimental
2.1. Materials and methods
A 1.0 g sample of pristine graphite flakes and 50 ml of acetic
acid was mixed by ultrasonication for 2 h and then left to stand
for 1 week. The resulting graphite nanoplatelets were washed with
acetone and dried in an oven at 80 °C for 12 h. The obtained graph-
ite nanoplatelets were exfoliated to graphite oxide using Hum-
mer’s method [32–34]. 1.0 g of graphite nanoplatelets and 0.5 g
of NaNO3 were added to 23 ml of concentrated H2SO4 at 0 °C. With
vigorous stirring, 3 g of KMnO4 was added gradually, and the tem-
perature of the mixture was controlled to be less than 20 °C. The
ice bath was then removed, and the temperature of the mixture
was maintained at 35 °C for 0.5 h. Subsequently, 46 ml H2O was
added slowly to the mixture, which made the mixture boil. After
15 min, 140 ml of hot water and an aqueous H2O2 solution was
added to the deeply brown mixture with constant stirring. The
resulting suspension was filtered while still hot. The solid mixture
was washed sequentially with a 5% HCl aqueous solution and ace-
tone. The resulting solid was dried at 60 °C under vacuum. Finally,
the prepared graphite oxide nanoplates were placed in an alumina
boat located to obtain a residual pressure of less than 106 mm Hg
and then heated to a certain temperature (150, 200, 250, 300, and
400 °C, respectively) with the 1 °C/s of heating rate. The samples
were designated GN-150, GN-200, GN-300, and GN-400, respec-
tively. Fig. 1 shows this process. It was observed that, upon vac-
uum-assisted thermal treatment, the grayish GO powder became
graphene nanoplates with a huge volume expansion.
Fig. 1. Schematic diagram of the preparation of graphene nanoplates.
2.2. Characterization
Wide-angle X-ray diffraction (XRD, Rigaku Model D/MAX-III B
with a rotation anode) patterns of the samples were obtained using
Cu Ka radiation (k = 0.15418 nm). The XRD patterns were recorded
over the range, 10–60° 2h. The specific surface area and total pore
volume were determined by N2 adsorption at 77 K using a surface
area analyzer (BEL Japan). Before the measurement, the samples
were degassed at 100 °C for 12 h to obtain a residual pressure of
<106 mm Hg. The N2 adsorbed on the graphene nanoplates was
used to calculate the specific surface area using the BET equation.
The total pore volume was estimated to be the liquid volume of
the N2 at a relative pressure of approximately 0.995, and the mi-
cro- and mesopore structures were analyzed using Horvath–Kawa-
zoe (HK) and Barrett–Joyner–Halenda (BJH) equations,
respectively. TGA data were obtained with a NETZSCH TG 209 F3
analyzer at a heating rate of 10 °C/min from 30 to 850 °C under a
N2 atmosphere. XPS measurements were performed on an ESCA-
LAB220i-XL (VG Scientific, UK) spectrometer with monochroma-
tized Al Ka X-ray radiation as the X-ray source for excitation in
order to confirm the nitrogen contents.
A CO2 adsorption test was conducted under ambient conditions
of 298 K at both low (1 bar) and moderate pressures (30 bar, BEL,
Japan). In each experiment, approximately 0.1 g of the sample
was loaded into a stainless chamber. Before the measurements,
the samples were degassed at 100 °C for 24 h to obtain a residual
pressure of <106 mm Hg. After the chamber was cooled to room
temperature, CO2 was introduced to pressure of 30 bar. Ultrahigh
purity grade (99.9999%) CO2 was used to exclude the effects of
moisture and other impurities. Finally, a volumetric measurement
method was used to determine the CO2 adsorption capacity.
3. Results and discussion
The structural properties of the pristine graphite flakes, graphite
oxide, and graphene nanoplates were characterized by XRD, as
shown in Fig. 2. For the pristine graphite flake, a sharp and intensive
peak at 26.6° corresponding to the graphitic structure (0 0 2) indi-
cated a highly organized layered structure with an interlayer spac-
ing of 0.335 nm (Fig. 2). After oxidation, the graphitic structure
(0 0 2) of the graphite flake powder disappeared and an additional
peak at 11.7° assigned to the (0 0 1) diffraction peak of graphite
oxide was observed [32–35]. According to previous research, the in-
ter-layers of graphite can be intercalated by a variety of molecules
 L.-Y. Meng, S.-J. Park / Journal of Colloid and Interface Science 386 (2012) 285–290
d=0.335 nm
d=0.806 nm
10 20 30 40
2 theta (°)
Fig. 2. XRD patterns of the pristine graphite flake, graphite oxide, and graphene
nanoplates (GN-400).
2
or ions, such as oxygen functional groups, NO 3 and SO4 [34]. The
XRD peak of graphite oxide corresponds to a layered structure with
a basal spacing of 0.806 nm. Therefore, the oxidation process leads
to an increase in d-spacing, which can be attributed to the oxide-in-
duced oxygen containing functional groups.
In contrast, no apparent peaks were detected in the patterns for
GN-400, which might have two explanations: (a) very thin graph-
ene layers due to the high degree of exfoliation; and (b) disordered
structure of graphene caused by the attachment of oxygenated
functional groups. After graphite oxide was exfoliated thermally
at 400 °C, the peak at approximately 11.7° from the GO shifted to
a lower angle. The interlayer spacing of GN-400 was estimated to
be 0.360 nm at 23.5°, which indicates a distorted graphite struc-
ture and suggests the formation of graphene nanoplates. This con-
firms that vacuum-assisted thermal treatment occurred at these
low temperatures, leading to disruption of the periodic layered
structure of graphite oxide plates [28,29].
When the exfoliation temperature was changed, the XRD pat-
terns of the graphene nanoplates obtained showed a typical broad
peak with the obvious disappearance of the characteristic peaks,
which might be due to very thin graphene layers because of the
high degree of exfoliation (Fig. 3). This suggests that the graphene
nanoplates are exfoliated into a few-layers, resulting in a new lat-
tice structure that is significantly different from the pristine graph-
ite flakes and graphite oxide. The interlayer spacing of the
graphene nanoplates (0.358–0.364 nm) was larger than that of nat-
ural graphite (0.335 nm). As the exfoliation temperature was in-
creased, the basal spacing (0 0 2) increased gradually to GN-300
and then decreased at higher temperatures. This is probably due
to the increasing behavior of the graphite peak reflecting the open-
ing of graphite layers after heat treatment.
Fig. 4 shows typical adsorption/desorption isotherms of N2 at
77 K onto the pristine graphite flakes, graphite oxide, and graphene
nanoplates as the function of the heat temperature. Previous
0.358 nm
Intensity (a.u.)
0.364 nm
0.360 nm
20 22 24 26
2 theta (°)
Fig. 3. XRD patterns of the graphene nanoplates as the function of temperature.
287
1200 Graphite
GO
N2 adsorbed (cm3/g, 77 K )
Intensity (a.u.)
GN-150
GN-200
GN-300
GN-400
800
400
Graphite
GO
GN-400 0
0.0 0.2 0.4 0.6 0.8 1.0
P/P0
Fig. 4. N2 full isotherms of the graphene nanoplates as the function of temperature.
studies reported that the graphite and graphite oxide exhibit neg-
ligible specific surface area and porosity for N2 adsorption [36,37].
In contrast, the prepared graphene nanoplates exhibited reason-
ably higher accessible N2 adsorption capacity. The curves of the
graphene nanoplates showed type IV isotherms according to the
IUPAC classification, as well as a hysteresis loop at relative pres-
sures >0.4, indicating the existence of mesopores. This shows that
the treated graphene nanoplates have a broad pore size distribu-
tion. A comparison of the curves of all the samples showed that
the heat temperature promotes the development of porosity in
the samples through the exfoliation of graphene nanoplates at dif-
ferent temperatures.
More recently, Lv et al. [28] and Zhang et al. [29] prepared few-
layered graphene sheets by thermally exfoliating GO under vac-
uum at a significantly low temperature, which is thought to exert
an outward force on the expanding graphene layers and help accel-
erate the expansion of graphene layers [28,29]. However, the sur-
face area (368 m2/g) of Lv and coworker’s graphene sheets was
much lower than that of Zhang and coworker’s graphene sheets
(758 m2/g). They reported that the exfoliation temperature can
be further reduced and the surface area greatly improved under
vacuum condition. Herein, we prepared graphene nanoplates un-
der 106 mm Hg at a lower temperature for synthesis CO2
adsorbents.
Table 1 lists the textural properties of graphite, graphite oxide,
and graphene nanoplates. After heat treatment, the specific surface
area and total pore volume of graphene nanoplates increased up to
300 °C, but decreased at 400 °C. The increase in total pore volume
was accompanied by an increase in mesopore volume. The Lang-
muir surface area and average pore diameter generally decreased
with increasing heat treatment. This suggests that heat treatments
can add to both the specific surface area and pore volume by
exposing the inner graphite layers. The specific surface of the
graphene nanoplates calculated from the BET equation was
480 m2/g for GN-300. This result is lower than that of Zhang’s ther-
mally exfoliated grapheme sheets, but that is higher than that re-
ported by Mishra’s (443 m2/g), Srinivas’ (470 m2/g), and Lv’s
(368 m2/g) [18,25,28]. Recent research works have shown that por-
ous materials with a large population of pores of size 1 nm exhi-
bit a better CO2 adsorption performance than those with narrower
micropores or with a mesoporous pore network [14]. And, the pre-
GN-200
vious work demonstrated that the porous carbons with ultrami-
cropores (<1 nm) are able to capture a large amount of CO2 at
GN-300
1bar [6,17].
GN-400 The pore size distributions were examined for better character-
ization of the changes in the porous structure of the graphene
nanoplates. Fig. 5 shows the micro-(Fig. 5a) and meso-(Fig. 5b)
28 30
pore size distribution of the graphene nanoplates prepared at tem-
peratures ranging from 200 to 400 °C, which were determined
using the HK and BJH method, respectively. According to the
288 L.-Y. Meng, S.-J. Park / Journal of Colloid and Interface Science 386 (2012) 285–290

Table 1
Pore structure parameters and surface group distribution of C1s XPS regions for the pristine graphite flake, graphite oxide, and graphene nanoplates from N2 adsorption
isotherms.

Samples SBETa (m2/g) SLangmirb (m2/g) VTc (cm3/g) Dd (nm) C1s (surface group distributions (%))
CAC; CAH CAOAC C@O COOH; OAC@O
Graphite 3 3 0.005 7.3 95.8 2.2 1.1 0.9
GO 14 20 0.054 15.4 78.7 12.8 3.7 4.8
GN-150 151 134 0.632 16.7 77.1 17.2 2.8 2.9
GN-200 437 313 1.716 15.7 79.9 15.9 2.2 2.0
GN-300 480 247 1.730 14.4 81.4 15.5 1.7 1.4
GN-400 324 245 1.032 12.7 83.8 14.1 1.3 0.8
a
Specific surface area: BET equation.
b
Specific surface area: Langmuir equation.
c
Total pore volume: Vads (P/P0 = 0.995)  0.001547.
d
Average pore diameter: 2  SBET/Vads.

(a) 0.4 Graphite

100
GO
GN-200 80
0.3 GN-300

TG (wt%)
GN-400
60
dV/dd0

0.2
40
GO
0.1
20
0.0
0
1 2 3 4 0 200 400 600 800 1000
d0 (nm) Temperature (oC)

Fig. 6. TG curves of a graphite oxide.

(b)
2.5
Graphite
GO
2.0 GN-200 macro-pores around 900 Å by partial gasification and expansion
GN-300 of the interlayer spacing between the graphene planes.
GN-400
1.5 The heating-driven structural changes of graphite oxide were
dV/dd0

1.0
0.5
0.0
20 40 60 80
d0 (nm)
Fig. 5. Micropore (a) and mesopore (b) size distribution of the pristine graphite
flake, graphite oxide, and graphene nanoplates.
literature, the collision and kinetic diameter (in Å) of a CO2
molecule is 3.9 Å and 3.3 Å, respectively, at room temperature.
Therefore, large CO2 capture by physisorption is obtained with
adsorbents containing a large volume of micropores with a suitable
micropore size (2 nm) [38–41].
The micropore structures were enhanced predominantly by the
heat treatment temperature, and the distributions show that slight
development can be observed around the micro-region compared
to the pristine graphite flake and graphite oxide. Micropore devel-
opment of prepared graphene nanoplates is mainly on the pore re-
gions <12.2 Å in diameter. The graphene nanoplates obtained with
300 °C exhibited exceptional micropore development (supermi-
cropores: 11.7 Å). As shown in Fig. 5b, the prepared graphene
nanoplates showed a broad pore size distribution. The sample ob-
tained at mild temperatures (300 °C) was made up mostly of wider
pores distributed in two well-defined pore systems: one of them
formed by uniform supermicropores (11.7 Å) and the other by
mesopores (20–500 Å). The heat treatment gave a broad meso-/
estimated by TGA, and the results are shown in Fig. 6. The decom-
posing temperature range of graphite oxide is from 100 to 500 °C,
which indicates that the oxygen-containing functional groups
bonded to graphene surfaces are removed in this temperature
range [28,29]. However, such a broad temperature range may drive
oxygen to flee from the planar graphene nanoplates and is not en-
100
ough to fully expand the graphene layers under an atmospheric
pressure [29]. Therefore, the vacuum-assisted thermal treatment
is needed for fast and fully expansion of graphene nanoplates in
this work. Usually, the deconvolution of the C1s spectra yields four
peaks with different binding energy values representing carbon in
the non-oxygenated CAC or CAH (284.5 eV), single CAO bonds
(285.5 eV), double C@O bonds (carbonyl, 287.1 eV), and carboxylic
COOH or OAC@O (288.5 eV) [32]. Table 1 also listed the relative
atomic percentage of CAC increased to 77.1–83.8% for GO and
GN-400, respectively, in comparison with 78.7% of graphite oxide
due to the removal of oxygen functional groups of graphite oxide
by heat treatment. This indicates that the reduction of the heat
treatment deoxygenated sp2 carbon from the epoxides and
hydroxyls. And, some amounts of oxygen functional groups were
still retained on the graphene surfaces, and the GN-400 has fewer
oxygen functional groups than others.
In this work, the aim is that improving the layer space of graph-
ene nanoplates for CO2 adsorption. The CO2 adsorption capacities of
the graphene nanoplates were measured from the CO2 adsorption
isotherms at 25 °C (Fig. 7). The CO2 adsorption capacity of graphene
nanoplates at 25 °C and 1 bar increased from 1 wt.% to 6.36 wt.% at
P/P0 = 1, as shown in Fig. 7a. The adsorbed weights (CO2) of all the
graphene nanoplates were in the following order at the low relative
pressure range (P/P0 6 1): GN-300 > GN-200 > GN-400 > graphite
 L.-Y. Meng, S.-J. Park / Journal of Colloid and Interface Science 386 (2012) 285–290 289

(a)

(wt.%, 298 K)
250 Zeolites
Graphite Activated Carbons
8
CO2 adsorbed (wt.%,1bar)
GO 200 GN-300
GN-150 G-1050
6 GN-200
GN-300 150
GN-400

CO 2 adsorbed
4 100

50
2
0
0
0 5 10 15 20 25 30 35
0.0 0.2 0.4 0.6 0.8 1.0 P/P0
P/P0
Fig. 8. CO2 adsorption isotherms of zeolite-13X, activated carbons, and prepared
graphene nanoplates (GN-300) measured at 30 bar and 25 °C.
(b) 400
CO2 adsorbed (wt.%,35 bar)

GN-200
GN-300 isotherms of these three materials. Zeolite-13 X, activated carbons,
300 GN-400
and conventional graphene nanosheets show maximum CO2
adsorption capacities at 35.1 wt.%, 67.9 wt.%, and 170.1 wt.%,
200 respectively. The advantage of the larger mesopore volumes in
the graphene nanoplates became more evident as the pressure
100 was increased, leading to a higher CO2 capture capacity of GN-
300 compared to that of zeolite-13X and activated carbon under
0 high pressure conditions (P/P0 > 1 bar).

0 10
Fig. 7. CO2 full isotherms of the pristine graphite flake, graphite oxide, and
graphene nanoplates measured at 1 bar (a) and 35 bar (b) and 25 °C.
oxide > graphite. This is because the GN-300 sample had a higher
micropore volume of supermicropores than the other samples
and hence a narrower micropore size distribution, as shown in
Fig. 5a. At the middle and high relative pressure region (P/
P0 > 30), GN-300 also showed maximum CO2 adsorption capacity.
This was attributed to the possible multilayer adsorption of CO2
molecules in the pores at higher pressures.
In the case of CO2 capture, the pore width is a key factor in
developing a carbon adsorbent with high capacity. For post-com-
bustion CO2 capture using solid adsorbents, the mechanism of solid
physisorbents materials can be visualized as follows:
20 30 40
4. Conclusions
P/P0
The CO2 adsorption behavior of exfoliated graphene nanoplates
is related directly to the heat treatment temperature. In this study,
exfoliated graphene nanoplates were expanded successfully from
graphite oxide by a low-heat treatment in the temperature range
of 150–400 °C under vacuum conditions. The heat treatment had
a significant effect on the property development of the graphene
nanoplates studied. The inter-layer spacing of the graphene layers
and pore structure on the CO2 capture capacities were examined as
a function of the processing conditions. The prepared graphene
nanoplates exhibited high capture capacities up to 248 wt.% under
25 °C and 30 bar. The CO2 capture capacities of the graphene nano-
plates were improved by a larger inter-layer spacing and higher
interior void volume.
Acknowledgments

CO2 þ Surface () ðCO2 Þ  ðSurfaceÞ

This work was supported by the Korea CCS R&D Center (KCRC)
grant funded by the Korea government (Ministry of Education, Sci-
where the selective adsorption of CO2 compared to N2 is caused by
ence and Technology) (0031985).
van der Waals attraction between the CO2 molecule and adsorbent
surfaces, as well as by pole-ion and pole-pole interactions between
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