Applied Surface Science 264 (2013) 329–334

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Applied Surface Science

journal homepage: www.elsevier.com/locate/apsusc

Graphene sheets synthesized by ionic-liquid-assisted electrolysis for application

in water purification
Chia-Feng Chang a , Quang Duc Truong b,c,∗ , Jiann-Ruey Chen a
a
Department of Materials Science and Engineering, National Tsing Hua University, Hsinchu 30013, Taiwan
b
Department of Chemistry, Vietnam National University, Hanoi, Viet Nam
c
Institute of Multidisciplinary Research for Advanced Materials, Tohoku University, Sendai 980-8577, Japan

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

D
Article history: A facile and green synthesis of graphene sheets by ionic-liquid-assisted electrolysis was investigated in
Received 22 March 2012 this work. The synthesized graphene sheets have been studied using transmission electron microscopy
Received in revised form 20 July 2012

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(TEM), atomic force microscopy (AFM), X-ray powder diffraction (XRD), Raman spectroscopy (Raman)
Accepted 4 October 2012
and Fourier transform infrared (FTIR) analysis. The obtained graphene was used for the adsorption of
Available online 13 October 2012
Fe2+ whose presence in the drinking water in wide areas of South Asia has been widely known. The result
shows that the graphene could absorb Fe2+ with a capacity of 299.3 mg/g which is 6 times higher than
Keywords:
that of graphite oxide. The adsorption properties of metal ions on graphene and the effects of various
Graphene
factors on the adsorption capacity were also investigated in detail. The research results suggest a novel
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Water purification
Heavy metal material for developing highly efficient water purification materials for the developing economies.
Ionic liquids-assisted electrolysis © 2012 Elsevier B.V. All rights reserved.

1. Introduction most promising approach for the removal of metal ions from water
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owing to its simplicity, cost-effectiveness, and enabling large-scale

Elevated concentrations of geogenic As and related heavy metal application. Therefore, adsorption method is widely used for pro-
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in groundwater raises a threat to the health of tens of millions cesses of the magnitude of municipal water supplies to small
of people living in the large delta areas of South Asia. In the Red domestic water filters, particularly as packed bed filters. For prac-
River delta, Vietnam, an estimated 11 million people who are using tical use, there are several materials which could absorb heavy
groundwater as the major domestic water source for daily life are metals effectively, such as activated carbon, fly ash, prawn shell
at risk [1]. Although it has been found that several geochemical pro- and peanut hull pellet [8–10]. In fact, people in the Red River
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cesses involve in the release of As into groundwater, the reduction delta, Vietnam is currently using hand-made filter containing nat-
of As-containing Fe-oxides with natural organic matter is gener- ural sand and activated carbon for cleaning the domestic water.
ally considered the most important mobilization mechanism [2,3]. The current research has been focused and developed new adsor-
Therefore, the contamination of As always associates with the ele- bents with better absorptive capacity for water purification. To
vated concentration of Fe(II) in the groundwater. The investigation date, the adsorption of metal ions onto carbon nanotubes (CNT)
of As and Fe contaminations in Red River aquifer using random has been investigated extensively. Recently, it has been suggested
monitoring wells in Northern Vietnam showed that the concentra- that graphene oxide and graphite oxide can be practically used for
tion of Fe increases linearly with that of As (Fig. 1). Thus, beside separation of arsenic and heavy metal from water [11,12]. As far as
the task of removing As from groundwater, the removal of Fe in the authors know, the adsorption properties of graphene, a newly
groundwater is still challenging the engineer in the environmental emerging member of carbon materials, for heavy metal ions have
research. not been reported up to now.
Many approaches have been employed to remove metal ions Graphene with hexagonally, sp2 -hybridized and one-atom-
from contaminated water including precipitation, ion-exchange, thick layer structures, has attracted extraordinary research interest
membrane filtration, and adsorption [4–7]. However, adsorption is since Geim and Novoselov, awarded the Nobel Prize in Physics
2010, explored for the first time [13–17]. Theoretical and exper-
imental studies have proved its outstanding mechanics, electricity,
chemicals, thermal stability, specific surface areas, mobility of
∗ Corresponding author at: Institute of Multidisciplinary Research for Advanced
charge carriers, and thermal conductivity [14–17]. Therefore, great
Materials, Tohoku University, Sendai 980-8577 Japan. Tel.: +81 22 2175651;
attention has been devoted on the study the applications of
fax: +81 22 2175651.
E-mail address: tqduc@mail.tagen.tohoku.ac.jp (Q.D. Truong). graphene such as solar cells, sensors, transistors, supercapacitors,

0169-4332/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.apsusc.2012.10.022
330 C.-F. Chang et al. / Applied Surface Science 264 (2013) 329–334

thickness measurement of Graphene sheets was conducted with

tapping mode atom force microscopy (AFM, SPA-400 SPM unit
from Seiko, Japan). 10 mg graphite oxide and graphene sheets were
dispersed in DMF for TEM and AFM measurements. The X-ray pow-
der diffraction (XRD) measurements on a Rigaku D/max-IIB X-ray
diffractometer with Cu K␣ radiation ( = 1.5418 Å) was performed
to identify the crystallite phase of the sample. In order to identify
the graphene material in the synthesized products, Raman mea-
surement with 514 nm excitation wavelength at room temperature
was carried out. The spectra were acquired by a Jasco R-3000 Raman
spectrometer in the backscattering geometry using 514 nm wave-
length and laser power of 90 W for excitation. The incident beam
was focused on the sample through the 100× lenses of microscope
into the spot of 2 ␮m size. The FTIR measurement was carried
out using universal attenuated total reflectance Fourier trans-
form infrared (UATR-FTIR) over the range from 4000 to 650 cm−1 .
For specific surface area determination, 25 mL dye solutions with
20–120 mg L−1 was introduced separately into 25 mL (adsorbent:
Fig. 1. The relationship between Fe(II) and As(III) concentration in groundwater.
0.5 mg mL−1 ) conical flasks and proceeded methylene blue (MB)-
relative surface area measurement.
and composite materials. In comparison with well-known CNTs,
graphene could be soluble in normal solvents or polymers with-
out reducing ideal intrinsic properties by chemical variations. 2.3. Batch adsorption experiments

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Hence, graphene provides many advantages over other carbon
materials. In this study, we focused on studying the removal Batch adsorption experiments were conducted to determine
of high concentration of Fe2+ by using graphene as adsorbent. the Fe(II) adsorption capacity of graphene. Iron stock solution
High concentration of heavy metal such as Fe2+ intake adverse
health effects and long-term exposure to metal can cause acute
gastrointestinal effects [18,19]. Therefore, removal of iron from
ground water is highly desirable, especially, for South Asia
where contamination of As and Fe in groundwater is a serious
TE(1000 mg/L) was prepared by dissolving Fe(NO3 )2 (Merk, Germany)
in deionized water and further diluted to the required concentra-
tions before use. The effect of initial and final pH on metal ion
adsorption by graphene was conducted in a pH range of 5.0–9.0.
The pH of the solution was adjusted to a desired value using appro-
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problem. priate concentrations of HNO3 or NaOH solutions. For the batch
tests, about 20 mg graphite, graphite oxide or graphene sheets
were added to 20 mL solution containing Fe(II) (20 mg L−1 ) while
2. Experimental
the pH of the solution was varied from 5.0 to 9.0. After the sus-
pensions were shaken for 24 h to achieve sorption equilibrium,
2.1. Synthesis of graphite oxide and graphene sheets
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the solid phase was separated from the solution by syringe filtra-
tion. The results of kinetic sorption suggested that Fe(II) sorption
Graphene was synthesized by ionic-liquid-assisted electrol-
on graphite oxide and graphene sheets achieved equilibrium after
ysis according to a procedure reported by Liu et al. [20]. The
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several hours. The concentrations of Fe(II) in the filtrate were deter-

electrolytes consist of ionic liquid, 1-octyl-3-methylimidazolium
mined by atomic absorption spectroscopy (PerkinElmer 3110). All
hexafluorophosphate ([C8mim][PF6 ]), and water. In typical exper-
the experimental data were the average of duplicate determi-
iment, two high-purity graphite oxide rods as the electrodes were
nations, and the relative errors were about 5%. The adsorption
inserted into the solution of ([C8mim][PF6 ])/water (1 g in 15 mL
experiment was also performed with Co(II). The amounts of Fe(II)
water), paralleled with a distance of 4.0 cm. DC voltage of 15 V was
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or Co(II) ions adsorbed on graphite, graphite oxide and graphene

applied to two graphite rods by Keithley 2400 model potentiostat.
sheets (mg/g) were calculated from the initial concentration (C0 )
After electrolyzing for 0.5 h, the anode graphite rod was corroded
and the equilibrium one (Ce ) (qe = (C0 − Ce ) × V/m, where V is the
and black precipitate appeared in the reactor. After electrolyzing for
volume of the suspension, and m is the mass of graphite, graphite
12 h, the precipitate was taken out of the reactor, and was washed
oxide or graphene sheets).
thoroughly with deionized water. Then it was dried at 60 ◦ C in the
electric oven for 6 h. Finally, the mixture of graphene and graphite
oxide was obtained. Since the graphite oxide is more hydrophilic 3. Results and discussion
than graphene, it can be separated from graphene by using polar
and non polar solvent dispersion. Particularly, mixture of toluene 3.1. Characterization of the synthesized materials
(90 vol.%) and H2 O (10 vol.%) was used to separate graphite oxide
and graphene. Typically, mixture of graphite oxide and graphene The XRD pattern of graphite (Fig. 2) presents very sharp diffrac-
was dispersed in water. The precipitation of agglomerated graphite tion peak at 2 = 26.5◦ , which can be indexed to the {0 0 2} peak
oxide sheets was immediately observed in water after the addition of graphitic structure of carbon. This peak only appears in the
of toluene to the aqueous solution. After collecting the aqueous sus- cases of graphene sheets and graphite but not in graphite oxide
pension three times, graphite oxide and graphene could be isolated. sheets. In particular, when graphite was oxidized to graphite oxide,
Finally, graphite oxide and graphene sheets were dried at 60 ◦ C in a new diffraction peak appears at 2 = 10.5◦ , along with the dis-
the electric oven for another 6 h. appearance of the diffraction peak {0 0 2} in the XRD pattern of
the product. In the XRD pattern of graphene, a typical diffraction
2.2. Characterization peak at 2 = 27.5◦ [21,22] was observed which is broaden, indicating
the smaller crystalline size of graphene in single layer or few lay-
The morphology of the obtained structures was examined ers structure. The calculated d-spacing between layers of graphite
using transmission electron microscopy (TEM) of JEM-2100F. The oxide and graphene sheets are 0.84 nm and 0.32 nm respectively.
 C.-F. Chang et al. / Applied Surface Science 264 (2013) 329–334 331

AFM images also reveal that the exfoliation of graphite has been
occurred.
X-ray photoelectron spectroscopy (XPS) was used to verify the
element binding configuration in graphite oxide and graphene
sheets (Fig. 5). The presence of C and O elements from the sur-
vey scan of graphite oxide and graphene sheets is revealed. The
presence of O proves that graphite has been oxidized by hydroxyl
and oxygen radicals at the electrode. The characterization peak of
C O, C O, COOH and the peak area in XPS spectra indicate the
change of composition during the electrolysis (Fig. 5). The relative
peak area of the C 1s to O 1s in graphene is higher than that in
graphite oxide. This evidence indicates that the concentration of
the C C moiety of graphene is higher than that of graphite oxide,
suggesting the smaller amount of oxygenated functional groups in
exfoliated graphene sheets.
The successful exfoliation of graphite into graphene was fur-
ther verified by Raman spectra. In the Raman spectrum of natural
graphite (Fig. 6), there are two peaks at 1580 cm−1 and 2736 cm−1
respectively. The peak at 1580 cm−1 corresponds to an E2g mode
Fig. 2. The XRD patterns of graphite, graphite oxide and graphene sheets. related to the sp2-bonded carbon atom’s vibration in a 2D hexago-
nal lattice. And the peak at 2736 cm−1 arises from the second order
of zone-boundary phonons of graphite. However, the major fea-

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tures, commonly observed in all chemically processed graphene,
The crystalline nature and morphology of graphite oxide are the D band at 1354 cm−1 , G band at 1567 cm−1 , and 2D band
and graphene sheets was investigated using TEM. Fig. 3 shows at 2736 cm−1 . The D band shows the presence of sp3 defects. The

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TEM images and corresponding selected-area electron diffraction presence of the sharp 2D band of graphene at 2723 cm−1 is pre-
(SAED) of the obtained graphite oxide and graphene sheets. The sumably due to two phonon double resonances Raman process.
thinner layers and higher crystalline nature of graphene sheets The shape of the 2D band of graphene is similar to that of previ-
than graphite oxide is revealed. Selected area electron diffraction ously characterized graphene, indicating the presence of few layers
was performed on the graphite oxide and graphene sheets and the for the synthesized graphene. The exfoliated graphite oxide has a
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corresponding SAED patterns are shown as the inset in Fig. 3. The high density of defects as evident from the stronger D peak in the
diffraction rings can be fully indexed to the hexagonal graphitic Raman spectrum in Fig. 6. Due to the presence of oxygenated func-
structure, indicating the crystalline nature of the graphite oxide tional groups, surface defects are formed. It is also suggested that
and graphene sheets. the D band arises from edge defects as well as the larger surface-
The obtained graphite oxide and graphene sheets were fur- to-volume ratio. The extracted graphene has sharp sp2 bonds in 2D
ther analyzed by AFM and the results are shown in Fig. 4. The system and the graphene provides high aspect ratio structure are
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AFM analysis reveals the presence of graphite oxide and graphene evidenced.
sheets with average thickness of 3.0 and 0.98 nm respectively, We observed the different functional groups of graphite,
which are consistent with result of previous report [20]. Particu- graphite oxide and graphene sheets in the FTIR spectra
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larly, the graphene sheet thickness of 0.98 nm is characterized of as shown in Fig. 7. The absorption peaks are observed at
single layer graphene synthesized by ionic-liquid-assisted method 3398–3428 cm−1 ( OH), 1681 cm−1 (C O), 1598–1603 cm−1
[20]. This thickness is thicker than the theoretical value of a single (skeletal vibrations from oxidized graphite domains),
layer (0.34 nm), which may be due to the presence of functionalized 1529–1543 cm−1 ( ph), 1205–1279 cm−1 (C OH stretching
hydrocarbon chains and PF6 − attached to graphene sheets. These vibrations) and 1086 cm−1 (C O stretching vibrations). C O
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Fig. 3. TEM images and SAED of graphite oxide (a) and graphene sheets (b).
332 C.-F. Chang et al. / Applied Surface Science 264 (2013) 329–334

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Fig. 4. AFM images of graphite oxide (a) and graphene sheets (b).
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Fig. 5. XPS spectra of graphite oxide (a, c) and graphene sheets (b, d).
 C.-F. Chang et al. / Applied Surface Science 264 (2013) 329–334 333

Fig. 6. Raman spectra of graphite, graphite oxide and graphene sheets.

group was only found in the spectrum of graphite oxide

structure. From FTIR investigation, it has been proved that

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graphite was transferred to the graphite oxide and graphene
structures.
On the basis of above result, the formation of graphene by elec-
trolysis can be understood as follows. Typically, after applying
voltage, hydroxyl and oxygen radicals were produced inevitably.
These radicals were formed by oxidation of dissociated water. Con-
sequently, the graphite anode was oxidized to produce the graphite
oxide. At the same time, the reduction of the cation from ionic liq-
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uid, leads to the formation of the 1-octyl-3-methylimidazolium
free radical. The radical can combine with one of the electrons
of the p-bond of the graphite [20]. The complicated interactions
between ionic liquid and graphite, including Coulomb interac-
tion and ␲−␲ interactions, could exfoliate graphite into graphene
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sheets. In addition, ionic liquid also provides the anionic ion to Fig. 8. Effect of pH on the sorption (qe ) of Fe(II) (a), and Co(II) (b) on graphite,
open layers between the graphite structures. Thus, the produc- graphite oxide, and graphene sheets.
tion of graphite oxide and graphene occurred through several
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steps as follows: (a) oxidation of water and ionic liquid at anode liquid depolarized and expanded the graphite into graphene
to produce the hydroxyl, oxygen radicals and free radical from sheets; (c) the radicals oxidized the graphite into the graphite
ionic-liquid; (b) the anionic BF6 − and free radical from ionic oxide.

3.2. The adsorption of heavy metals

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The adsorption of Fe2+ and Co2+ on graphite, graphite oxide and

graphene sheets under the different pH values were studied (Fig. 8).
The adsorption capacity is characterized by adsorptions amount
of metal ion/mass of adsorbent (qe , mg/g). It was found that the
adsorption capacity of graphene sheets is 6–7 times higher than
that of graphite oxide sheets. The adsorption capacities of graphene
sheets increased sharply vs. pH value in range of 5.0–8.0 and reach
maximum value of 299.3 and 370 mg/g for Fe(II) and Co(II), respec-
tively. The lower adsorption capacity at pH 9.0 may be due to the
formation of hydroxide Fe(OH)2 and Co(OH)2 , which reduced num-
ber of metal ions adsorbed on the graphene surface. On the other
hand, the adsorption competition of H+ with metal ions for adsorp-
tion sites resulted in low adsorption capacity at low pH condition.
It was reported that the isoelectric point (IEP) of graphene where
the zeta potential equals zero is 4.7 [23]. This indicates that at
pH > IEP, the graphene has negative surface charge, which benefits
for adsorbing cations. Thus, the increase of the adsorption capac-
ity in pH range of 5.0–8.0 may be attributed to the electrostatic
interaction between negatively charged surface of graphene and
metal cation. The highest adsorption of Fe2+ and Co2+ on graphene
Fig. 7. FTIR spectra of graphite, graphite oxide and graphene sheets. sheets at pH 8.0 is presumably due to negatively charged surface of
334 C.-F. Chang et al. / Applied Surface Science 264 (2013) 329–334

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