Journal of Colloid and Interface Science 436 (2014) 41–46

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Journal of Colloid and Interface Science

www.elsevier.com/locate/jcis

Preparation of colloidal graphene in quantity by electrochemical

exfoliation
Kunfeng Chen, Dongfeng Xue ⇑
State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China

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

Article history: We reported the preparation of colloidal graphene in quantity via the anodic exfoliation of graphite in
Received 27 June 2014 (NH4)2SO4 aqueous solution. In the currently designed electrochemical exfoliation route, mass high-
Accepted 27 August 2014 quality graphene was produced within short reaction time, around 1 h. The proposed electrochemical
Available online 6 September 2014
exfoliation mechanism showed that SO2 4 and H2O can be intercalated into those graphite sheets,
monolayer and few-layer graphene were obtained by the formation of gaseous SO2 and O2 within graphite
Keywords: sheets. Stability evaluation showed that our exfoliated colloidal graphene can be perfectly stabilized in
Colloidal graphene
DMF solvent more than 1 week. The colloidal graphene can be used to construct various simple and
Electrochemical exfoliation
Mass production
complex patterns by writing it on A4 paper, which can be applied to flexible printed electronic devices.
Energy storage Furthermore, colloidal graphene can show promising applications in the fabrication of binder- and addi-
Printed electronics tive-free electrodes for supercapacitors and lithium-ion batteries. Our present method shows huge poten-
tial for industrial-scale synthesis of high-quality graphene and further commercialization of graphene
colloid for numerous advanced applications in flexible printed electronics and energy storage devices.
Ó 2014 Elsevier Inc. All rights reserved.

1. Introduction aqueous electrolyte [9,10]. However, the large quantities produc-

Due to its ultrathin, two-dimensional and sp2-bonded carbon
nature and unprecedented properties, graphene has become the
most studied nanomaterials [1,2], which can show potential and
important applications in printed electronics, conductive coatings,
composite fillers, solar cells, sensors, lithium-ion batteries and sup-
ercapacitors [3–5]. The large-scale preparation of colloidal form of
graphene is an important requirement for next-generation printed
electronics [6]. The solar cell, battery and sensor electrodes almost
certainly are produced by solution-coating process and so will
require large quantities of graphene in the form of colloids, liquid
suspensions, inks, or dispersions [1,3]. However, all these applica-
tions require large-scale production of defect-free graphene in a
processable form. The current routes for the preparation of graph-
ene mainly include mechanically exfoliation, epitaxial growth,
chemical vapor deposition (CVD), solvent- and/or surfactant-
assisted liquid-phase exfoliation of graphite, and the thermal/
chemical reduction of graphene oxide [7,8]. Among these methods,
electrochemical exfoliation of graphite has attracted specific atten-
tion due to its easy, fast, and environmentally friendly nature to
produce high-quality graphene [6,9,10]. The electrochemical
exfoliation reaction mainly conducted in ionic liquids or acidic
⇑ Corresponding author.
E-mail address: dongfeng@ciac.ac.cn (D. Xue).
tion of colloidal graphene in mild near neutral solution by electro-
chemical method is rarely reported [6].
Colloids represent a formation stage of crystallization of all
kinds of materials; generally speaking, atoms initially form clusters
in various kinds of solutions or melts, then during nucleation a
colloid is formed which further promotes crystal growth [11,12].
The combination of strongly size- and shape-dependent physical
properties and ease of fabrication and processing makes colloidal
nanocrystals promising building blocks for materials with
designed functions [13]. Recently, we have found that the in-situ
formed colloid during the electrochemical reaction can display
high electrochemical performance as energy storage devices [14–
17]. The as-formed colloids have very large surface area, thus can
effectively utilize their active surfaces to improve electrochemical
performance. Therefore, the colloidal form of graphene can also
produce novel performances compared with other forms of
graphene. In addition, colloidal graphene can be served as versatile
platform to construct devices by the easy solution-route. However,
graphene is prone to aggregate when reducing graphene oxide in
water using reducing agent without additional reagents, where
graphene colloid was produced by the transformation of graphene
oxide colloid. The development of a straightforward process to pre-
pare colloidal graphene from graphite materials is a critical point
for commercial applications.

http://dx.doi.org/10.1016/j.jcis.2014.08.057
0021-9797/Ó 2014 Elsevier Inc. All rights reserved.
42 K. Chen, D. Xue / Journal of Colloid and Interface Science 436 (2014) 41–46

Scheme 1. Schematic drawing shows the large-scale production of graphene sheets by electrochemistry using two graphite electrodes in aqueous (NH4)2SO4 solution. Left,
experimental setup diagram; middle, exfoliation of the graphene sheets from the graphite anode; right, formation of colloidal graphene. The applied direct current (DC) bias
voltage was constant 10 V. The electrochemical exfoliation only occurred at the anodic graphite, while the cathodic graphite kept intact. The electrochemical process was
finished until the fully consumption of anodic graphite.

Scheme 2. Flow chart and the exfoliation mechanism of our designed electrochemical strategy toward high quality colloidal graphene. (a) Flow chart representation of the
reaction processes of graphite anode in aqueous (NH4)2SO4 solution at DC bias voltage of 10 V. (b) Crystal structure of graphite, (c) the intercalation of SO2
4 and H2O within
graphite layers, (d) the evolution of bubbles within the graphite layer due to the electrochemical reactions, (e and f) these gaseous species can exert large forces on the
graphite layers, and separate weakly bonded graphite layers from one another to form graphene sheets. (g) The formation of colloidal graphene with dispersing graphene
sheets in DMF solvent.

Herein, mass colloidal graphene was produced by electrochem-
ical exfoliation of graphite in (NH4)2SO4 aqueous solution within
short reaction time, about 1 h. The exfoliated graphene can be
stable dispersed in DMF solvent to form colloidal solution. Further-
more, colloidal graphene can show potential applications in
printed electronics, fabrication of binder- and additive-free elec-
trodes for supercapacitors and lithium-ion batteries. Our present
results are promising for industrial-scale synthesis of high-quality
graphene and further commercialization of graphene for numerous
advanced applications.
2. Experimental
2.1. Materials preparation
In a typical electrochemical synthesis of graphene, a conven-
tional two-electrode system was used, which consisted of two
graphite flakes as anode and cathode. The electrolyte was 40 mL
aqueous solution containing 0.1 M (NH4)2SO4. The direct current
(DC) bias voltage was set to 10 V and remained until the full
consumption of anodic graphite. When 10 V bias voltage as applied
to electrodes, the bulk graphite expanded quickly and was thor-
oughly consumed within 1 h. Colloidal graphene ink was prepared
by dispersing graphene in N, N-dimethylformamide (DMF) with a
high concentration at sonication conditions.
2.2. Material characterizations
The morphology and structure of the samples were investigated
by field emission scanning electron microscope (Hitachi S4800),
transmission electron microscope (FEI Tecnai G2 F20) and X-ray
diffraction (Bruker D8 Focus). Raman spectra were recorded with
a Renishaw 2000.
2.3. Preparation and electrochemical measurement of supercapacitor
The as-prepared graphene ink was coated on nickel foil to form
binder-free and additive-free working electrode. The electrochemi-
cal measurements were carried out using a classical three-electrode
 K. Chen, D. Xue / Journal of Colloid and Interface Science 436 (2014) 41–46 43

a b

c d

1 μm 5 1/nm

Fig. 1. Characterization of the exfoliated graphene and pristine graphite. (a) SEM images of pristine graphite flakes. (b) SEM image of the exfoliated graphene. (c and d) TEM
image and SAED pattern of the exfoliated graphene. Monolayer graphene can be obtained as evidenced by its electron diffraction pattern.

cell configuration in 2 M KOH. The Pt wire was served as the counter
electrode, and the saturated calomel electrode (SCE) was used as the
reference electrode. The cyclic voltammograms (CV), and galvano-
static charge–discharge measurements were carried out by an
electrochemical workstation (CHI 660D). Specific capacitance val-
ues were calculated from galvanostatic charge–discharge data
according to the following equation:
I Dt
SC ¼
mDE
where I (A) is the current used for charge/discharge, Dt (s) is the
time elapsed for the discharge cycle, m (g) is the mass of the active
electrode material, and DE (V) is the voltage interval.
2.4. Preparation and electrochemical measurement of lithium-ion
battery
The as-prepared graphene ink was directly coated on copper foil
using paintbrush. After drying, the copper foils were cut into disks,
which were directly applied as the working electrode without
using binders and conductive agents. Lithium metal was used as
the counter and reference electrode, Celgard 2400 was used as sep-
arator, and the electrolyte was 1 M LiPF6 in ethylene carbonate/
dimethyl carbonate/diethyl carbonate (EC/DMC/DEC, 1:1:1 vol%).
A galvanostatic cycling test of these assembled half-cells was
conducted on a LAND CT2001A system in the voltage range of
0.01–3.0 V (vs. Li+/Li) at current density of 100 mA/g.
3. Results and discussion
Scheme 1 shows the experimental setup and the procedure of
electrochemical anodic exfoliation of graphite. The exfoliation pro-
cess was performed in a two-electrode system using two graphite
flakes as anode and cathode, and the electrolyte is 0.1 M (NH4)2SO4
aqueous solution. When the direct current voltage of 10 V was
applied to two-electrode setup, vigorous bubbles were produced
at both two electrodes and anodic graphite began to dissociate into
electrolyte (Scheme 1). The voltage was kept constant until com-
pleting the exfoliation process.
The reaction mechanism of electrochemical exfoliation of
graphite is shown in Scheme 2. Graphite has a layered, planar
structure. In each layer, the sp2 carbon atoms are arranged in a
honeycomb lattice and are only weakly bonded to the graphite
sheets above and below. Graphene are essentially single-atom-
ð1Þ thick sheets of graphite, which can be pulled from a crystal of
graphite with something as simple as adhesive tape [18]. Herein,
electrochemical exfoliation of graphite to produce graphene sheets
in aqueous solution was reported. Scheme 2a shows flow chart of
the reaction processes of graphite anode in aqueous (NH4)2SO4
solution at the DC bias voltage of 10 V. The exfoliation mechanism
of our electrochemical strategy toward high quality colloidal
graphene is shown in Scheme 2b–f. Firstly, SO2 4 and H2O were
intercalated into graphite layers by electrochemistry [6]. Then,
the reduction of SO2
4 anions and self-oxidation of water produced
gaseous species such as SO2, O2, and others, which can be evi-
denced by the vigorous gas evolution at anode during the electro-
chemical process. These gaseous species can produce larger forces
beyond the weakly bonded force between the graphite layers [19].
Finally, the weakly bonded graphite layers were exfoliated from
one another to form monolayer graphene sheets. The graphene col-
loid can be formed by dispersing graphene sheets in DMF solvent,
which can be used as ink for printed electronics and energy storage
devices.
The morphology of the exfoliated graphene sheets was investi-
gated by SEM and TEM. Fig. 1a shows SEM image of pristine graph-
ite, which includes many thick graphite flakes. After exfoliated in
(NH4)2SO4 solution, the crumpled and thin sheets can be found,
indicated the formation of graphene sheets (Fig. 1b). The formation
of crumpled sheets is due to the thermodynamic stability of the 2D
graphene resulting in microscopic crumpling via bending or
buckling. Fig. 1c shows TEM image of the exfoliated graphene. A
transparent sheet-like structure can be found and these crumpled
44 K. Chen, D. Xue / Journal of Colloid and Interface Science 436 (2014) 41–46

a a 6

4
Graphene
2
Intensity (a.u.)

Current (A/g)
0

Graphite -2

-4
50mV/s graphene
-6 100mV/s graphene
JCPDS No. 1-640 100mV/s graphite
-8
10 20 30 40 50 60 70 -1.0 -0.8 -0.6 -0.4 -0.2 0.0
2θ (degree) Potential (V vs. SCE)

b 0.0
b
-0.2 1A/g graphene

Potential (V vs. SCE)

Graphite 3A/g graphene
Intensity (a.u.)

G 1A/g graphite
D -0.4

-0.6

-0.8
Graphene
-1.0
1200 1300 1400 1500 1600 1700 1800 0 20 40 60 80 100 120
Wavenumber (cm-1) Time (s)

Fig. 2. (a) XRD patterns and (b) Raman spectra of graphite flakes and the exfoliated
graphene. The graphite exhibits a sharp peak centered at 26.6° and 54.7°
corresponding to the (0 0 2) and (0 0 4) planes. The standard XRD pattern of graphite
crystal with JCPDS No. 1-640 is also shown in graph. Two remarkable peaks in the
Raman spectra are the D band (defects) and the G band (in-plane vibration of sp2
carbon atoms).
Fig. 3. Photographs show the potential applications of colloidal graphene in flexible
printed devices. The graphene words ‘‘CIAC’’ and ‘‘J. Colloid Interface Sci.’’ were
written on A4 paper using a Chinese maobi and graphene colloid ink. The as-
synthesized colloidal graphene can be well stored in DMF and water.
and loose graphene sheets were stacked. The selected area electron
diffraction (SAED) was performed on the graphene sheets and the
corresponding SAED pattern is shown in Fig. 1d. Several diffraction
spots in a hexagonal pattern were identified, suggesting that the
selected graphene sheet is single crystal and the obtained graphene
products include monolayer graphene sheets [20].
Fig. 4. Supercapacitor performance of the exfoliated graphene. (a) CV curves of
graphene electrode at different scan rates and (b) charge–discharge curves at
different current densities. CV and charge–discharge curves of pure graphite are
also shown in a and b for comparison. All data are collected in 2 M KOH electrolyte
at room temperature.
The crystal structure of the pristine graphite and the exfoliated
graphene were analyzed by conducting X-ray diffraction (XRD)
studies (Fig. 2a). The pristine graphite flakes exhibit a sharp peak
centered at 26.6° and 54.7° corresponding to the (0 0 2) and
(0 0 4) planes of graphite crystal. The exfoliated graphene displays
a broad (0 0 2) diffraction peak due to the corrugated structure of
the graphene and the stacked graphene layers. XRD result proved
the successful exfoliation of graphite to producing graphene, which
is in good agreement with the reported value.
Raman spectra of graphite flakes and the exploited graphene
reflect the significant structural changes from graphite to graphene
(Fig. 2b). Two remarkable peaks in the Raman spectrum are the D
band (defects) and the G band (in-plane vibration of sp2 carbon
atoms). The Raman spectrum of the graphite (Fig. 2b) displays a
prominent G peak at 1600 cm1 corresponding to the first-order
scattering of the E2g vibration mode [9]. The Raman spectrum of
the exfoliated graphene shows that the G band is broadened and
the peak of D band is present at 1370 cm1. The ratio of ID/IG cor-
responds to the number of defects in graphene. The intensity of G
band is higher than that of D band for the exfoliated graphene,
thus, the ratio of ID/IG is less than 1, which is much lower than that
of chemically or thermally reduced graphene oxide (1.2–1.5)
[21,22]. The Raman spectrum, XRD and SAED analyses clearly dem-
onstrate the synthesis of high quality graphene by electrochemical
exfoliation methods when compared to chemical methods. Our
present electrochemical exfoliation process shows several advan-
tages, such as simplicity, high productivity, economical viability,
and short processing time when compared to previously reported
techniques and methods [21,22].
 K. Chen, D. Xue / Journal of Colloid and Interface Science 436 (2014) 41–46
a 3.0
2.5
Potential (V vs. Li+/Li)
2.0
1.5
1.0
0.5
0.0
0 50 100 150 200
Capacity (mAh/g)
b 350
300
Charge
Capacity (mAh/g)
Discharge
250
Efficiency
200
150
100
50
0 0
0 10 20 30
Cycle number (n)
Fig. 5. Lithium-ion battery performance of the exfoliated graphene. (a) The initial
three charge–discharge curves and (b) cycling performance of the exfoliated
graphene electrode for lithium-ion battery at a current density of 100 mA/g and the
potential range from 0.01 to 3 V vs. Li+/Li.
In order to find potential applications in flexible printed elec-
tronics, colloidal graphene was firstly prepared and its printed
application was further studied. The graphene colloid was obtained
by dispersing graphene in DMF, water or ethanol (Fig. S1). The as-
synthesized colloidal graphene can be well stored in water and
DMF for long-time. The long-term stability was examined by leav-
ing the suspensions undisturbed for different times. For example,
colloidal graphene in DMF was stable for more than 1 week, while
graphene colloid in water was stable for 24 h. Fig. 3 shows the
potential applications of colloidal graphene. The obtained colloidal
graphene in DMF was served as ink (Fig. S2). Using a Chinese mao-
bi, colloidal graphene can be written on A4 paper. Fig. 3a and b
show the written graphene words ‘‘CIAC’’ and ‘‘J. Colloid Interface
Sci.’’ on A4 paper. With this simple and easy-operating strategy,
various simple and complex graphene patterns can be constructed
on many substrates, such as paper, current collector for flexible
electronic devices. The present results prove that our exfoliated
colloidal graphene ink has promising application in flexible printed
electronic devices.
Large-scale production of graphene is another requirement for
the commercial application of graphene. Among various methods
for synthesizing graphene, electrochemical exfoliation is a promis-
ing route due to its advantages of cost-effective, simple, conve-
nience, and without using complex equipment [20]. In our
designed experiment, two graphite electrodes, one DC power
source, and aqueous electrolyte were only needed to produce mass
graphene within short reaction time. With 1 h reaction time, 0.2 g
of crude graphite was fully exfoliated to produce graphene and the
production rate of graphene was 0.2 g/h. In fact, 80% of literatures
45
had production rate of graphene below 0.04 g/h [1]. Therefore, our
designed electrochemical exfoliation method can show huge
potential in large-scale production of graphene.
1st To further confirm the potential application of the exfoliated
2nd graphene, the performances of supercapacitors and lithium-ion
3rd batteries were evaluated. In this work, the used graphene
electrodes were binder-free and additive-free. The exfoliated col-
loidal graphene ink was directly coated on Ni foam current col-
lector to form supercapacitor electrode, while the graphene ink
coated on copper foil was directly served as anode for lithium
ion battery. The binder-free and additive-free electrode is an
important requirement for high-performance flexible printed
energy storage devices. Fig. 4 shows supercapacitor performance
250 300 350 of the exfoliated graphene. The graphene electrode exhibits a
typical double-layer capacitive behavior with quasi-rectangular
CV curves and linear charge–discharge curves (Fig. 4a and b)
100 [23]. The outline of CV curves at 50 and 100 mV/s, and the profile
of charge–discharge curves at 1 and 3 A/g are similar, indicating
the good capacitive behavior. The specific capacitance of the
80
Efficiency (%) exfoliated graphene is 56.6 F/g at the current density of 1 A/g
according to the discharge curves calculated from Eq. (1). The
60 supercapacitor performance of the pure graphite is also shown
in Fig. 4 for comparison. Pure graphite also shows typical dou-
40 ble-layer capacitive behavior with quasi-rectangular CV curves
and linear charge–discharge curves. However, the specific capac-
20 itance, 0.62 F/g at current density of 1 A/g, is very lower than the
value of the exfoliated graphene. The results proved that the
exploited graphene show significant enhanced specific capaci-
40 50 tance. Furthermore, we studied the lithium-ion battery
performance of the exfoliated graphene. Fig. 5 shows the
charge–discharge curves and cycling performance of the exfoli-
ated graphene electrode for lithium-ion batteries. The first dis-
charge capacity is 342 mA h/g, while the 10th and 20th
discharge capacities are 117.9 and 100.2 mA h/g. High Coulombic
efficiency >91% can be obtained after 10th charge–discharge
cycle. After 50 charge–discharge cycles, the discharge capacity
is 80.1 mA h/g with Coulombic efficiency of 98.4%, indicating that
the exfoliated graphene electrode shows better cycling stability.
The present results prove that the exfoliated colloidal graphene
can be served as effective electrode materials for the develop-
ment of flexible energy storage devices, because that colloidal
graphene can be used to directly fabricate binder-free and addi-
tive-free electrodes.
4. Conclusions
In summary, we reported that mass high-quality colloidal
graphene was produced by electrochemical exfoliation of graphite
in an aqueous (NH4)2SO4 solution within short reaction time, about
1 h. Because SO24 and H2O can be intercalated into graphite sheets,
monolayer and few-layer graphene were formed in the designed
electrochemical exfoliation route. The production rate of graphene
in present work was about 0.2 g/h, which is higher than those val-
ues (below 0.04 g/h) reported in 80% of literatures. The colloidal
graphene can be used to construct various simple and complex
patterns by writing the as-prepared graphene ink on A4 paper,
which can be applied to flexible printed electronic devices. In addi-
tion, colloidal graphene can be directly coated on Ni foam and Cu
current collector to fabricate binder-free and additive-free elec-
trodes for supercapacitors and lithium-ion batteries. We showed
that the electrochemical anodic exfoliation of graphite in aqueous
solution is a promising route for industrial-scale synthesis of high-
quality graphene and the exfoliated colloidal graphene can show
potential applications in printed electronics, binder- and addi-
tive-free electrodes for energy storage devices, solar cells and
sensors.
46 K. Chen, D. Xue / Journal of Colloid and Interface Science 436 (2014) 41–46
Acknowledgments
Financial support from the National Natural Science Foundation
of China (grant nos. 50872016, 20973033 and 51125009) and
National Natural Science Foundation of China for Creative Research
Group (grant no. 21221061), and Hundred Talents Program of
Chinese Academy of Science are acknowledged.
Appendix A. Supplementary material
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.jcis.2014.08.057.
References
[1] K.R. Paton, E. Varrla, C. Backes, R.J. Smith, U. Khan, A. O’Neill1, C. Boland, et al.,
Nat. Mater. 13 (2014) 624.
[2] K.S. Novoselov, A.K. Geim, S.V. Morozov, D. Jiang, Y. Zhang, S.V. Dubonos, I.V.
Grigorieva, A.A. Firsov, Science 306 (2004) 666.
[3] K.S. Novoselov, V.I. Fal’ko, L. Colombo, P.R. Gellert, M.G. Schwab, K. Kim, Nature
490 (2012) 192.
[4] F. Liu, S. Song, D. Xue, H. Zhang, Adv. Mater. 24 (2012) 1089.
[5] F. Liu, D. Xue, Chem. Eur. J. 19 (2013) 10716.
[6] K. Parvez, Z. Wu, R. Li, X. Liu, R. Graf, X. Feng, K. Müllen, J. Am. Chem. Soc. 136
(2014) 6083.
[7] C.J. Shih, A. Vijayaraghavan, R. Krishnan, R. Sharma, J.H. Han, M.H. Ham, Z. Jin,
S.C. Lin, G.L.C. Paulus, N.F. Reuel, Q.H. Wang, D. Blankschtein, M.S. Strano, Nat.
Nanotechnol. 6 (2011) 439.
[8] P.W. Sutter, J.I. Flege, E.A. Sutter, Nat. Mater. 7 (2008) 406.
[9] V.V. Singh, G. Gupta, A. Batra, A.K. Nigam, M. Boopathi, P.K. Gutch, B.K. Tripathi,
A. Srivastava, M. Samuel, G.S. Agarwal, B. Singh, R. Vijayaraghavan, Adv. Funct.
Mater. 22 (2012) 2352.
[10] C.Y. Su, A.Y. Lu, Y.P. Xu, F.R. Chen, A.N. Khlobystov, L.J. Li, ACS Nano 5 (2011)
2332.
[11] D. Nykypanchuk, M.M. Maye, D. van der Lelie, O. Gang, Nature 451 (2008) 549.
[12] K. Chen, D. Xue, CrystEngComm 16 (2014) 4610.
[13] Y. Yin, A.P. Alivisatos, Nature 437 (2005) 664.
[14] K. Chen, D. Xue, Colloids Interface Sci. Commun. 1 (2014) 39.
[15] K. Chen, D. Xue, J. Colloid Interface Sci. 424 (2014) 84.
[16] K. Chen, D. Xue, J. Colloid Interface Sci. 416 (2014) 172.
[17] K. Chen, D. Xue, J. Colloid Interface Sci. 430 (2014) 265.
[18] K.S. Novoselov, D. Jiang, F. Schedin, T.J. Booth, V.V. Khotkevich, S.V. Morozov,
A.K. Geim, Proc. Natl. Acad. Sci. USA 102 (2005) 10451.
[19] F. Beck, J. Jiang, H. Krohn, J. Electroanal. Chem. 389 (1995) 161.
[20] K. Parvez, R.J. Li, S.R. Puniredd, Y. Hernandez, F. Hinkel, S.H. Wang, X.L. Feng, K.
Müllen, ACS Nano 7 (2013) 3598.
[21] C. Mattevi, G. Eda, S. Agnoli, S. Miller, K.A. Mkhoyan, O. Celik, D.
Mastrogiovanni, G. Granozzi, E. Garfunkel, M. Chhowalla, Adv. Funct. Mater.
19 (2009) 2577.
[22] V. López, R.S. Sundaram, C.G. Navarro, D. Olea, M. Burghard, J.G. Herrero, F.
Zamora, K. Kern, Adv. Mater. 21 (2009) 4683.
[23] M.F. El-Kady, V. Strong, S. Dubin, R.B. Kaner, Science 335 (2012) 1326.