Journal of Science: Advanced Materials and Devices 1 (2016) 454e460

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Journal of Science: Advanced Materials and Devices

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

Original Article

Graphene-zinc oxide (G-ZnO) nanocomposite for electrochemical

supercapacitor applications
Murugan Saranya a, *, Rajendran Ramachandran b, **, Fei Wang b, ***
a
Platinum Retail Ltd, Chorleywood Road, Rickmansworth, United Kingdom
b
Department of Electronic and Electrical Engineering, Southern University of Science and Technology, Shenzhen 518005, China

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

Article history: Graphene-ZnO nanocomposites (G-ZnO) were prepared by a facile solvothermal approach. Well, crys-
Received 12 September 2016 talline ZnO nanoparticles with size in the range of 30e70 nm are uniformly deposited on the graphene
Accepted 6 October 2016 sheets, as evidenced by different techniques. The electrochemical properties of the prepared nano-
Available online 13 October 2016
composites were examined by measuring the specific capacitance in 6 M KOH solution using cyclic
voltammetry and galvanostatic chargeedischarge techniques. G-ZnO nanocomposites showed a good
Keywords:
capacitive behavior with a specific capacitance of 122.4 F/g as compared to graphene oxide (2.13 F/g) and
Solvothermal
rGO (102.5 F/g) at 5 mV/s scan rate. Results demonstrated that such hybrid materials are promising
Graphene-ZnO
Graphene oxide
electrode materials for high-performance supercapacitor applications.
Cyclic voltammetry Crown Copyright © 2016 Publishing services by Elsevier B.V. on behalf of Vietnam National University,
Specific capacitance Hanoi. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/
4.0/).

1. Introduction has been the most encouraging material for energy storage appli-
cations due to its high electrical conductivity, thermal conductivity,
Supercapacitors are charge storage devices of tremendous in- superior chemical stability, unique mechanical strength and a large
terest in view of its high power density, fast charging/discharging surface to volume ratio than other carbon materials [3]. Disorder in
rate, long cycle life, a wide operating temperature range and envi- the atomic configuration of graphene can have dramatic effects on
ronmentally benign. Still, the low energy density of these super- its electronic, thermal, magnetic and other properties [4,5]. Super-
capacitors has forced huge difficulties in utilizing them as essential capacitors are categorized into two types based on the charge
energy sources to replace batteries [1]. Hence continuous effort has storage mechanism viz. electric double layer capacitors (EDLCs) and
been embraced to use nanostructured materials with enhanced pseudocapacitor. The latter stores charge faradically, which allows
specific capacitance. Most research is focused on the development them to achieve higher capacitance properties and enhanced en-
of different electrode materials like carbon, conducting polymers, ergy densities than EDLCs. Polymers and metal oxides like NiO [6],
metal oxides and out of which carbon-based materials like activated RuO2 [7], MnO2 [8], Co3O4 [9], and V2O5 [10] exhibit this type of
carbon, carbon nanotube, and carbon aerogels is paid more atten- capacitance called pseudocapacitance which involves redox re-
tion for energy storage devices [2]. Activated carbon and carbon actions and often the pseudocapacitance of such polymers and
nanotube shows good electrical double layer capacitance because of metal oxides show higher specific capacitance than EDLCs. How-
their excellent conductivity and high surface area, where the stor- ever, the relatively low conductivity and poor stability of such
age process is non-Faradaic and the storage of energy is electro- materials usually require the addition of conductive phases e.g.
static. The key to achieving high capacitance increases the surface carbon-based to enhance the charge transfer. In this way, these two
area and electrical conductivity of the material. As of late graphene could be merged together for the fabrication of a hybrid capacitor,
where both faradaic and non-faradaic processes can be used for
charge storage and enhanced electrochemical properties. It has
* Corresponding author. been accounted that the combination of carbon material with
** Corresponding author. polymer/metal oxides or both exhibit higher specific capacitance
*** Corresponding author. due to the combination of the redox reaction of metal oxide and
E-mail addresses: [email protected] (M. Saranya), ramnano2009@gmail. high surface area/conductivity of graphene than their individual
com (R. Ramachandran), [email protected] (F. Wang).
form due to a positive synergistic effect [11]. In the most recent
Peer review under responsibility of Vietnam National University, Hanoi.

http://dx.doi.org/10.1016/j.jsamd.2016.10.001
2468-2179/Crown Copyright © 2016 Publishing services by Elsevier B.V. on behalf of Vietnam National University, Hanoi. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/).
 M. Saranya et al. / Journal of Science: Advanced Materials and Devices 1 (2016) 454e460 455

Fig. 1. Schematic digram of G-ZnO nanocomposite synthesis.

couple of years, graphene-based composites are being examined for property. Because of the superior electrical conductivity of ZnO, it is
supercapacitor applications. In general, the specific capacitance of widely used in many applications ranging from optoelectronics [13],
graphene is lesser than the expected value due to restacking of the gas sensors [14], energy storage and solar cells [15]. Lu et al. re-
graphene sheets which could be improved by making it as a com- ported the maximum specific capacitance of 61.7 F/g for graphe-
posite with other materials. Wu et al. have reported a maximum neezinc oxide thin film which prepared by ultrasonic spray
specific capacitance of 210 F/g for grapheneepolyaniline composite pyrolysis method [16] and another report showed the maximum
[12]. Among the metal oxides, RuO2 exhibits higher specific specific capacitance of 146 F/g for G-ZnO nanocomposite [17]. Here,
capacitance yet its usage is limited due to its high cost and toxicity. we report a facile approach to synthesize ZnO/Graphene nano-
Thus, the fabrication of supercapacitor electrode materials with composites by the solvothermal process. These composites were
low-cost production is challenging in the field of energy storage utilized to fabricate supercapacitor electrodes to probe their elec-
devices and hence it is imperative to explore more desirable ma- trochemical properties and results revealed that the nanocomposite
terials for supercapacitor applications. Zinc oxide (ZnO) is a po- materials had a good electrochemical performance as electrode
tential semiconductor material with amazing optical and electrical materials with a specific capacitance of 122.4 F/g.

Fig. 2. XRD pattern of G-ZnO composite and graphene oxide (Inset picture).
456 M. Saranya et al. / Journal of Science: Advanced Materials and Devices 1 (2016) 454e460

Fig. 3. (a) DRS UV spectrum of G-ZnO composite and (b) optical band gap diagram of G-ZnO.

was centrifuged (Eppendorf centrifuge 5430, 460W, Germany) at

7500 rpm with deionized water and dried at 60
C for 24 h.

2.3. Synthesis of G-ZnO nanocomposites

Graphene-ZnO nanocomposites were prepared by our previ-

ously reported solvothermal method as described in the literature
[19]. In brief, GO (5 mg) was dissolved in 20 ml of ethylene glycol
and sonicated for 1 h. Then 20 mg of zinc acetate dissolved in 20 ml
of ethylene glycol was added to the above GO dispersed solution
under continuous stirring. Later, 0.1 M NaOH in 5 ml of distilled
water was added to the mixture. After 30 min of stirring, the
mixture was transferred into the Teflon-lined stainless steel auto-
clave and maintained at 160
C for 48 h. The obtained final mixture
was centrifuged and washed with de-ionized water and ethanol
several times, and dried at 60
C for 24 h. The weight of graphene in
the G-ZnO composite is 2 weight%.

2.4. Electrochemical measurements

Fig. 4. FTIR spectrum (a) G-ZnO composite (b) Graphene Oxide.

Cyclic Voltammetry and chronopotentiometry experiments

were investigated by using a CHI 600C electrochemical workstation
2. Materials and experimental in a three electrode system. Glassy carbon electrode, Ag/AgCl, and
platinum wire electrode were used as working, reference and
2.1. Materials counter electrodes respectively. Experiments were carried out at
room temperature in 6 M KOH electrolyte in the potential range
Graphite powder, sodium nitrate, potassium permanganate, from 0 to 0.8 V.
hydrogen peroxide, sodium hydroxide, potassium hydroxide,
ethylene glycol, and zinc acetate were purchased from Sigma- 2.5. Electrode preparation
eAldrich. All the materials were used as received without any
further purification. The fabrication of the modified working electrode, glassy carbon
was polished with 0.03 mm alumina powder, rinsed thoroughly
with de-ionized water, sonicated with ethanol and deionized water
2.2. Preparation of graphene oxide for 5 min. After a few minutes, 0.5 mg of the active material (G-ZnO,
GO, rGO) in 2 mL Nafion solution was coated on the GC electrode
Graphene oxide was prepared through modified Hummer's (geometric surface area of the electrode is 0.0706 cm2) and allowed
method as described in the literature [18]. Graphite powder (1 g) to dry at room temperature for few hours.
and sodium nitrate (1 g) were mixed with 46 ml of concentrated
sulfuric acid. The mixture was kept in an ice bath for four hours 2.6. Characterization
under continuous stirring. To it, potassium permanganate (6 g) was
added and the reaction was then allowed at 35
C for two hours and The X-ray diffraction system (BRUKER, D8 Advance, Germany)
diluted with 92 ml de-ionized water. Then the temperature was was used for the X-ray analysis with Cu-Ka radiation (l ¼ 1. 540 Å).
raised to 98
C and maintained for two hours. The solution was Step scanning was used with 2q intervals from 8
to 60
. Scanning
further diluted with 200 ml warm water and 20 ml hydrogen Electron Microscope images were taken from the system (FEI
peroxide and further stirred for another one hour. After the reac- Quanta FEG 200). The electrochemical performance was done by
tion, the color of the solution turned into yellowish brown, which the system CHI 600C work station, Version 5.01.
 M. Saranya et al. / Journal of Science: Advanced Materials and Devices 1 (2016) 454e460 457

Fig. 5. HRTEM images of G-ZnO nanocomposite at various magnifications and EDS spectrum of G-ZnO nanocomposite (Inset picture of b).

3. Results and discussion intercalation of oxygen functional groups during the oxidation
process. The major diffraction peaks in G-ZnO composite were
3.1. Structural analysis observed at 2q value 31.8
, 34.4
, 36.2
, 47.5
, 56.5
, 62.7
, 66.3
,
68.0
, 69.1
and 76.9
which correspond to (100), (002), (101), (102)
The schematic diagram of G-ZnO nanocomposites synthesis is (110), (103), (200), (112), (201) and (202) crystalline plane of ZnO
given in Fig. 1. The XRD pattern of graphene oxide and G-ZnO respectively. These crystalline planes are indexed to the wurtzite
composites is shown in Fig. 2. The inset picture showed the XRD structure of ZnO particles matched with the JCPDS No. 36-1451
pattern of GO and the peak was observed at 2q ¼ 10
suggesting [21]. The average ZnO crystalline size as calculated from Scherrer
that the perfect oxidation and the interlayer distance of graphene formula was 14 nm. It could be seen that there is no diffraction peak
are 8.8 Å [20]. The increased interlayer distance is due to the of carbon in the composite. Due to the good crystallinity of ZnO

Fig. 6. Cyclic voltammetry performance (a) Graphene Oxide (b) G-ZnO composite at different scan rates.
458 M. Saranya et al. / Journal of Science: Advanced Materials and Devices 1 (2016) 454e460

peak at 398 nm due to ZnO particles in graphene sheets [17]. The

optical band gap is obtained by the following equation, with the
help of absorption spectra.


ðahnÞn ¼ A hn  Eg

where ‘a’ is the absorption coefficient, ‘h’ is the Planck constant, ‘y’
is the light frequency, ‘Eg’ is the band gap, ‘n’ is either ½ for an in-
direct transition or 2 for a direct transition and A is a constant.
According to the above equation, the band gap of the as-obtained
ZnO-Graphene nanocomposites is 3.12 eV, which is shown in
Fig. 3(b).
The FTIR spectrum of GO and G-ZnO composite is shown in
Fig. 4. It is observed that the oxygen functional groups of GO are
revealed by the peaks at 1726, 1217 and 1055 cm1 corresponding
to C]O stretching, CeO is stretching and CeO bending [24]
respectively. These oxygen functional groups are generated dur-
ing the oxidation process of the graphite by Hummer's method
Fig. 7. Comparison Cyclic voltammetry response of GO, rGO and G-ZnO composite at [25]. In the case of G-ZnO composite, it could be observed that the
100 mV/s scan rate. oxygen functional groups were almost reduced, which is indicating
the reduction of GO during the hydrothermal process. The absor-
bance peak at 1581 and 450 cm1 indicated the skeletal vibration of
graphene sheets and stretching vibration of ZneO [26]. Thus, these
results indicate, the formation of ZnO on graphene matrix. To
further know the morphology of these nanostructures, HRTEM
analysis was recorded and the corresponding images are given in
Fig. 5. It can be seen that the wrinkled structure of graphene sheets
is well decorated with ZnO nanoparticles with particle size in the
range from 30 to 70 nm. The uniform distribution of ZnO nano-
particles on the graphene sheets which contributes to an excellent
electrical conductivity of the composite. The presence of carbon,
zinc and oxygen were further confirmed from EDS spectrum given
in the inset picture of Fig. 5(b).

3.2. Electrochemical measurements

The capacitive performances of the materials were further

evaluated by cyclic voltammetry (CV) and galvanostatic charge/
discharge techniques in 6 M KOH electrolyte. The CV was run at
different scan rates in the potential ranging from 0 to 0.8 V in 6 M
Fig. 8. Plot of scan rate verse specific capacitance for GO, rGO, and G-ZnO
nanocomposite.
KOH electrolyte (Fig. 6). The shapes of the CV loop in our experi-
ment exhibit quasi-rectangular shape indicating the capacitive
behavior of the capacitor [27]. As seen from the Fig, though the
nanoparticles in composite, the diffraction of carbon atoms in curve is partially rectangular, it shows deviation from an ideal
graphene is weakened. The ZnO nanoparticles covering the gra- rectangular shape with some redox peaks due to Faradaic reaction
phene sheets in the composite and gave strong diffraction peaks. of ZnO, which indicates the pseudocapacitive nature of the mate-
Hence, the carbon diffraction peak is disappeared in the composite rial. Also, could be observed from this figure is that as compared to
[22]. GO, the addition of ZnO to the graphene gives a better and a
The electronic structure of the G-ZnO nanocomposites was symmetric curve. From the Fig. 7, it can be seen that the current
measured by UV diffusive reflectance spectroscopy, as shown in level and area of CV curves is higher for G-ZnO nanocomposite than
Fig. 3(a). It is observed that the graphene-ZnO composite spectrum rGO and GO, which indicates more capacitive nature of electrode.
showed low absorption in the visible and infrared region; however, The possible faradic process can be explained as follows:
high absorption in the ultraviolet region, which is in good agree-
ment with the literature by other workers [23]. Also, it exhibited a ZnO þ OH 4ZnOOH þ e

Table 1
ZnO based electrode materials with specific capacitance values.

Electrode material [SC] (F/g) [SR] (mV/s) [EL] [R] Electrode preparation

Carbon aerogel/ZnO 25 10 6 M KOH [29] Active material coated on Ni foam electrode

Functionalized CNT/ZnO 59 5 0.1 M TBAPC/DMF [30] Two symmetric electrodes separated by thin
polypropylene separator
Activated graphene/ZnO 84 e 6 M KOH [31] Active material coated on stainless steel electrode
Graphene/ZnO 61.7 50 1 M KCl [16] ZnO deposited on graphene by USP method
Graphene/ZnO 122.4 5 6 M KOH This work Active material coated on carbon paper electrode

[SC] e Specific capacitance, [SR] e Scan Rate, [EL] e Electrolyte, [R] e Reference.
 M. Saranya et al. / Journal of Science: Advanced Materials and Devices 1 (2016) 454e460 459

The galvanostatic charge/discharge is a reliable technique to

evaluate the electrochemical capacitance of materials under
controlled current conditions. Fig. 9 demonstrates the char-
geedischarge behavior of GO and G-ZnO composite at a constant
current of 0.1 A/g. Both curves exhibited a nearly triangular shape
and typical features of potential charge/discharge viz. linear
response to time with asymmetric capacitive behavior during the
discharge process. The sudden drop in current at the starting of
discharge is due to the internal resistance of electrode material
[32]. It can be seen that the IR drop of GO is much higher than G-
ZnO, which indicates the larger electrode/electrolyte interfacial
resistance in the former. Low internal resistances are important for
energy storage devices and less energy will be wasted to produce
unwanted heat during charge/discharge processes. A discharge
time of 130 s has been noticed for G-ZnO electrode which is higher
than GO discharge time 7.5 s. A high discharge time is a clear evi-
dence for the high specific capacitance of G-ZnO electrode. These
results are in accordance with the CV measurements.
Electrochemical impedance analysis is an informative technique
Fig. 9. Charge/Discharge behavior of GO and G-ZnO electrodes at current density of 0.1
A/g.
to evaluate the properties of conductivity and charge transport in
the electrode/electrolyte interface. Fig. 10 shows the Nyquist plot
and equivalent fitting circuit of GO and G-ZnO electrodes. In the
As the scan rate increases, the total peak current also increases low-frequency region, the impedance plot is increased sharply and
demonstrating the good rate properties and capacitance behavior. tends to become vertical which is due to the capacitive nature of
The specific capacitance of the composite is calculated from the electrode. The 45
straight line can be observed in Fig. 9(b) shows
following equation [28] the pure capacitance behavior of G-ZnO. The intercept of higher
frequency on X axis yields the electrolyte resistance (Rs) and the
ðIþ  I Þ diameter of semicircle yields the charge transfer resistance (Rct)
C¼
mn [32]. A small electrolyte resistance of 12.2 U was observed for G-
ZnO which is due to the excellent conductivity of graphene sheets
where Iþ is maximum current in the positive scan (A), I is in ZnO. The Warburg impedance can be observed in G-ZnO elec-
maximum current in the negative scan (A), m is the mass of the trode related to the diffusional impedance of the electrochemical
active material (g) and y is the scan rate (V/s). The specific capaci- systems. Thus, the EIS analysis clearly demonstrated that the
tance is proportional to the area under the CV curve, which is larger graphene-ZnO composite provides easier access to charge between
for G-ZnO than GO and rGO. A maximum specific capacitance of electrode and electrolyte and hence a maximum specific capaci-
122.4 F/g was obtained at a scan rate 5 mV/s for G-ZnO which is tance have been achieved. These results suggested that the G-ZnO
higher than that of rGO (102.5 F/g) and GO (2.13 F/g) respectively. electrode could be used for high-performance supercapacitor
The high specific capacitance achieved in the G-ZnO may be due to applications.
effective electrical and ionic conductivity. Fig. 8 shows the plot of
scan rate versus specific capacitance and from the graph, it is
evident that the specific capacitance decreases at higher scan rates, 4. Conclusion
which could be due to the presence of inner active sites that cannot
sustain the redox transitions. Also, this decrement indicates that In summary, XRD evolution demonstrates wurtzite structure of
the parts of the surface of the electrode are inaccessible at high ZnO and a particle size of ~150 nm as observed from SEM investi-
charging/discharging rates. It shows that the G-ZnO composites gation. The electrochemical behavior of composite was studied by
could be used for high-performance supercapacitor applications. A cyclic voltammetry and electrochemical impedance spectroscopy.
comparison has been given in Table 1 on the specific capacitance of Cyclic voltammetry results show a maximum specific capacitance
the present work with other reported materials. of 122.4 F/g for G-ZnO composite electrode at 5 mV scan rate. The

Fig. 10. Nyquist plot and an equivalent circuit of GO (a) and G-ZnO (b).
460 M. Saranya et al. / Journal of Science: Advanced Materials and Devices 1 (2016) 454e460

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