Journal of Experimental Nanoscience

ISSN: 1745-8080 (Print) 1745-8099 (Online) Journal homepage: https://www.tandfonline.com/loi/tjen20

A one-step facile route synthesis of copper oxide/

reduced graphene oxide nanocomposite for
supercapacitor applications

Suresh Sagadevan, Zaira Zaman Chowdhury, Mohd. Rafie Bin Johan, Fauziah
Abdul Aziz, Emee Marina Salleh, Anil Hawa & Rahman F. Rafique

To cite this article: Suresh Sagadevan, Zaira Zaman Chowdhury, Mohd. Rafie Bin Johan, Fauziah
Abdul Aziz, Emee Marina Salleh, Anil Hawa & Rahman F. Rafique (2018) A one-step facile route
synthesis of copper oxide/reduced graphene oxide nanocomposite for supercapacitor applications,
Journal of Experimental Nanoscience, 13:1, 284-296, DOI: 10.1080/17458080.2018.1542512

To link to this article: https://doi.org/10.1080/17458080.2018.1542512

© 2018 The Author(s). Published by Informa Published online: 07 Dec 2018.

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JOURNAL OF EXPERIMENTAL NANOSCIENCE
2018, VOL. 13, NO. 1, 284–295
https://doi.org/10.1080/17458080.2018.1542512

A one-step facile route synthesis of copper oxide/reduced

graphene oxide nanocomposite for supercapacitor
applications
Suresh Sagadevana,b, Zaira Zaman Chowdhuryc, Mohd. Rafie Bin Johanc,
Fauziah Abdul Aziza, Emee Marina Salleha, Anil Hawaa and Rahman F. Rafiqued
a
Department of Physics, Center for Defence Foundation Studies, Universiti Pertahanan Nasional
Malaysia, Kuala Lumpur, Malaysia; bCentre for Nanotechnology, AMET University, Chennai, India;
c
Nanotechnology & Catalysis Research Centre, University of Malaya, Kuala Lumpur, Malaysia;
d
Department of Environmental Sciences, The State University of New Jersey, New Brunswick,
NJ, USA

ABSTRACT ARTICLE HISTORY

In this research, a one step, facile route has been undertaken to Received 13 July 2018
synthesise copper oxide/reduced graphene oxide (CuO/rGO) Accepted 25 October 2018
nanocomposites. X-ray powder diffraction analysis (XRD) was car-
KEYWORDS
ried out to identity the crystalline structure and phase of the syn-
Nanocomposite; CuO/rGO;
thesised sample. Elemental analysis and surface morphological Raman spectroscopy and
features were analysed using EDX and FESEM Images. Particle size electrochemical properties
as well as the shape of the as prepared composite was observed
from HR-TEM images. Raman spectra illustrated the peak of the
individual composite materials. The electrochemical properties of
the prepared nanocomposite were investigated. The dielectric
behaviour of the sample including dielectric constant, dielectric
loss and AC conductivity was measured at various frequency lev-
els. Temperature was varied accordingly to observe the effect of
temperature on the dielectric properties of the sample.

1. Introduction
Graphene is a comparatively new form of nano carbon where monolayers of carbon
atoms are arranged in a honeycomb lattice. It has attracted huge attention in recent years
among the experimental and theoretical scientific communities [1]. Graphene oxide (GO)
is one of the most important derivatives of graphene. GO exhibit layered structure where
oxygen functional groups are present on its basal planes and edges [2]. Since it has special
surface properties and layered structure, it can be considered as potential nanoscale build-
ing blocks for novel materials with improved properties [3]. The two-dimensional (2D)
graphene nano-sheets can act as an ideal atom-thick substrate which can be hybridised
easily with nanoparticles to obtain three-dimensional (3D) architectures having unique
chemical, physical and structural properties [4–6]. Recently, hybrid nano-composites

CONTACT Zaira Zaman Chowdhury [email protected]

ß 2018 The Author(s). Published by Informa UK Limited, trading as Taylor & Francis Group.
This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/
licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 285

fabrication by integrating graphene nano sheets with other inorganic materials gained lot
of interests among the researchers [7–10]. The aggregation of inorganic nanoparticles can
be effectively stabilised using graphene sheets. The functional properties of the nanopar-
ticles also can be improved due to incorporation of graphene sheets inside the composite
matrix [11–15]. Recently, various literature has reported regarding the doping of metal,
metal oxide, semiconducting, and magnetic nanoparticles including Pd [16], Pt [17],
Au [18], TiO2 [19] and Fe3O4 [20] over the surface of GO nano-sheets. Nanoparticles can
prevent the agglomeration of GO nano-sheets. It can provide space between GO nano-
sheets not only to reduce the agglomeration but also can allow these active nanoblocks
with high surface energy to function properly. Thus, the surface area and pore volume of
GO- sheets become high which make them suitable candidate for applications including
adsorption processes and electro-catalysis. The nanocomposite synthesised using GO
nano-sheets with metal/metal oxide nanoparticles doped inside it usually demonstrates
superior properties and amended functionalities. Due to the synergetic effects between
GO nano-sheets and the nanoparticles, they can be used as efficient electro-catalysts [11, 21].
Nevertheless, limited amount of research has been conducted to evaluate their catalytic
activity for transformation of organic compounds.
CuO is considered as a cheap substitute compared to other expensive noble metal or
metal oxide nanoparticles. It has broad potential application as heterogeneous catalysts,
active anode materials, superconductors, sensors and heterogeneous catalysts. Its’ abun-
dant availability, reduced cost, promising pseudo-capacitive features with environmental
compatibility enable it to be considered as eco-friendly candidate for nanocomposite syn-
thesis [22, 23]. Incorporation of nanoparticles over Graphene nano-sheets has gained lot
of attention recently and has become an active arena of research due to their promising
application in versatile fields. Hydrothermal method assisted by ammonia solution has
been used by other researchers to synthesise CuO–Graphene nanocomposites for applica-
tion in supercapacitors [24]. In lithium ion batteries, CuO-deposited graphene nanocom-
posites are extensively used as these types of composites can show superior performance
as anodic materials [24, 25]. In its’ presence, the anode can exhibit high capacity and cap-
acity retention. In this research, 2 D graphene sheets were acting as a conductive platform
which can be easily doped by CuO nanoparticles. The synthesis strategy adopted here was
chemically assisted, simple, one step and economically feasible. Scanning electron micros-
copy (SEM) with energy dispersion spectroscopy analysis and high-resolution transmis-
sion electron microscopy (HR-TEM) analysis was carried out to study the surface
morphological features of the synthesised sample. The phase of the synthesised sample
with crystallites size was measured from X-ray diffraction (XRD) analysis. Surface func-
tional groups were identified using FT-IR analysis. Raman spectroscopy and dielectric
studies had been conducted to illustrate the electrochemical properties fabricated
nanocomposite.

2. Experimental procedure
2.1 Synthesis of the CuO/rGO nanocomposite
For a typical preparation of CuO/reduced graphene oxide composite, graphite oxide
(5 mg) was first exfoliated in a mixed solvent of distilled water (6 mL) and N, N-dimethyl-
formamide (DMF) (50 mL) with ultrasonic treatment to form a stable graphene oxide
(GO) nano-sheets suspension. Then, 0.02 g cuprous chloride was dissolved in 1 ml ammo-
nia solution (3%) with flow of N2 in a round-bottomed flask. Finally, the above graphene
286 S. SAGADEVAN ET AL.

Figure 1. X-Ray diffraction patterns of CuO/rGO nanocomposite.

oxide nano-sheets (GO) suspension was quickly mixed with the solution containing
cuprous chloride and ammonia solution. The reduction reaction was carried out in one
step under reflux at 80 C for 2 h under vigorous stirring. The solid product (CuO/rGO)
䊊

was separated by centrifugation (5000 rpm) and washed using deionised water and anhyd-
rous ethanol several times to remove other ions. The final product was collected and dried
in vacuum at 70 C for 5 h.
䊊

2.2 Characterisations techniques

The XRD diffraction pattern for the synthesised sample of CuO/rGO nanocomposite was
analysed using an X-ray diffractometer (Schimadzu model: XRD 6000) where the data
have been recorded for CuKa (k ¼ 0.154 nm) radiation with a diffraction angle between
10 and 80 . The surface morphological features were observed using scanning electron
microscopic (SEM) analysis (JEOL, JSM- 67001). To avoid the charging effect, the syn-
thesised samples were coated with gold prior the SEM analysis. The particle size and
shape were observed using the high-resolution transmission electron microscope
(HRTEM) analysis. The image was taken using a JEOL 3010 with a UHR pole piece oper-
ating at an accelerating voltage of 300 kV. Raman spectroscopic analysis was carried out
using a Bruker RFS 27; stand-alone model Raman spectrometer. Aqueous 2 M KOH solu-
tion was used as the supporting electrolyte. CVs in the potential at various current den-
sities and electrochemical impedance spectra (EIS) over the frequency were carried out by
using the VSP biologic electrochemical system. The frequency range was varied from
50 Hz to 5MHz to determine the dielectric properties of the CuO/rGO nanocomposite
(HIOKI 3532-50 LCR HITESTER).

3. Results and discussion

Figure 1 illustrates the X-ray diffraction patterns of the synthesised CuO/rGO nanocom-
posite and the prepared rGO and GO here. The positions of the diffraction peaks
observed here for the composite samples accorded well with the standard CuO and rGO
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 287

Figure 2. (a, b) TEM Images of CuO/rGO nanocomposite (c,d) HR TEM Images of CuO/rGO nanocomposite.

samples. The peaks (110), (-111), (111), (-202), (020), (202), (-113), (-311), (220) were
consistent with the standard XRD pattern for the CuO monoclinic phase. Some extra
peaks around (002) and (100) were observed which could be attributed to the reduced
graphene oxide. Since GO was reduced successfully to RGO during the synthesis process,
redox reaction took place and the characteristic peak of GO at (001) disappeared from
the XRD pattern of the composite material. However, the intensity observed for the two
characteristic reflection peaks of rGO in the composite material became much weaker
than those of the as-prepared reduced graphene oxide. This happened due to the presence
of less agglomerated, disordered stacking of the rGO sheets inside the composite matrix.
The TEM pictures of the synthesised sample are shown in Figure 2. The TEM images
gave the information regarding the size and morphology of the CuO/rGO as well as their
agglomeration tendencies. From Figure 2(a), it was observed that the pure CuO nanopar-
ticles were agglomerated. The particle size obtained was in the range of 60–65 nm. The
288 S. SAGADEVAN ET AL.

Figure 3. SEM images and EDX spectrum of CuO/rGO Nanocomposite.

composite prepared here is highly crystalline in nature (Figure 2b). This type of interac-
tions can ensure high mechanical flexibility of the reduced graphene nano-sheets and will
prevent its’ agglomeration to large particles.
The SEM images of CuO nanoparticles are shown in Figure 3. The spherical shape of
the particles is clearly visible from the images. The surface texture was rough and uneven.
However, the particle size determined was within the nano range. The SEM images con-
firmed the presence of stacked graphene sheets inside the composite matrix. The peaks
observed from EDX spectrum showed the presence of all three elements (Cu, O and C)
which confirmed the formation of CuO/rGO nanocomposite (Figure 3d).
The FTIR spectrum of CuO/rGO nanocomposite is illustrated in Figure 4. The vibra-
tion of the Cu–O bond was confirmed by the presence of the peak at 526 cm1. This
showed that the cuprous ions were oxidised to CuO by GO during the synthesis process.
In addition, the OH stretching vibration occurred at 3433 cm1. The results clearly dem-
onstrated that the samples obtained here were partially reduced in presence of cuprous
ions. Figure 5 shows the Raman spectrum of CuO/rGO composite. The D and G bands at
1330 and 1594 cm1, respectively, were observed from the Raman spectrum of CuO/rGO
composite. In general, it is accepted that the Raman ID/IG ratio (where ID and IG are the
D- and G-peak Raman intensities, respectively) is related to the density of defects in gra-
phene-based materials, and the graphitisation degree of carbonaceous materials.
The cyclic voltammetry process was carried out to observe the electrochemical per-
formance of the synthesised CuO/rGO nanocomposite for supercapacitor. This showed
that the electrodes were consecutively charged and discharged over the whole voltammet-
ric cycle. The capacitance behaviour of the nanocomposite was observed by the presence
of anodic and cathodic peaks. This further confirmed that the surface redox reactions had
been taken place. Figure 6 displays the CV profiles of the nanocomposite at different scan
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 289

Figure 4. FTIR spectrum of CuO/rGO nanocomposite.

Figure 5. Raman spectrum of CuO/rGO nanocomposite.

rates. A lower specific capacitance was observed using higher scan rate due to reduced
charge storage capacity. This is expected for a higher scan rate as the electrolyte ions
could not enter inside the interior part the electrode materials. The minimum area of the
electrode was used by the electrolyte ions to years through at lower scan rate. This
resulted in superior values for specific capacitance. Moreover, the electrochemical capaci-
tive behaviour depends on the rate of charge exchange. This depends on the diffusion of
anions and cations towards the electrode/electrolyte interfaces. CuO can diffuse on the
surface of graphene and ensure more ions diffusion due to increase in interface zone
between the electrode and electrolyte.
Figure 7 illustrated the EIS measurements on pure CuO nanoparticles. The behaviour
of the electrodes was evaluated for three charge/discharge cycles. The intercept impedance
on the Z-real axis reflects the electrolyte solution resistance, while the semicircle in the
high middle frequency range and the oblique line at low frequencies represents the
charge-transfer process and the lithium ion diffusion process (Warburg), respectively.
Nyquist plots contain two parts – one is semicircle and another on is the straight line.
290 S. SAGADEVAN ET AL.

Figure 6. C–V characteristics of CuO/rGO-nanocomposite.

Figure 7. Nyquist plots of CuO/rGO nanocomposite.

At the high middle frequency region, the semicircle portion reflects the change transfer
process around electrode/electrolyte interface. The straight line at lower frequency
region illustrates the Warburg impedance process. The smaller diameter of the semi-
circle represents the reduced charge transfer resistance. Enhanced electron transfer
with less resistance properties were observed using highly conductive reduced graphene
nano-sheets. The polarisation rate was depressed due to reduced charge trans-
fer resistance.
The specific capacitance values are inversely proportional with the scan rate. At a lower
scan rate, positive ions (Kþ) can simply diffuse inside the every accessible site of materi-
als. This initiates satisfactory insertion pathways for reaction. However, at higher scan
rate, positive ions can approach only outer surface of the electrode. The constituent mate-
rials found inside the inward space has minor role to the capacitance behaviour. This ini-
tiates a slight deviation from ideality and less capacitance values. The highest reversible
capacities with the best cycling stability were observed for the CuO/rGO nanocomposite
electrode. Under various current densities, the specific capacity for the synthesised
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 291

Figure 8. The rate capabilities of the CuO/rGO nanocomposite.

nanostructures was measured to improve the capacity of anodes and the results are plot-
ted in Figure 8. The nanoparticles of CuO were distributed homogenously over the rGO
nanosheets. The particle aggregation was reduced by rGO nanosheets, thus electrochem-
ical cycling problem was able to reduce the pulverisation of the electrode. It was noticed
that rGO nano-sheets can conduct electricity. It can initial the internal resistance of the
electrode-specific capacities. The ion transport path length was shortened due to CuO
incorporation inside the rGO nano-sheets. Thus, electrode/electrolyte contact area was
enhanced. The higher storage capacities with columbic efficiencies and cycling stabilities
were observed. The electrochemical performance of the electrode was enhanced by the
synergetic effect rGO nano-sheets and CuO nanoparticles. The nanocomposite electrode
delivered a discharge capacity of the first cycle and maintained stable capacities from the
second cycle with an excellent capacity retention.
Figures 9 and 10 illustrate the dielectric properties of the synthesised sample at differ-
ent temperatures. A step-like decrease in dielectric constant with increasing frequency fol-
lowed by Debye-like dipolar relaxations, i.e. dielectric loss peaks (Figure 10) of the CuO/
rGO NC. At particular frequency range, the Debye-like dipolar relaxations was observed.
This happened due to large dielectric response. Maxwell–Wagner–Sillars (MWS) inter-
facial polarisation effect was observed due to step like reduction in dielectric constant
with different frequency levels [26]. When the nanoparticles were under the interfaces of
an electric field the space charge was accumulated at the interfaces of the electrode and
nanoparticles, it was also present at the interfaces between the neighbouring grains at
lower frequency level. The short range dipole interactions were observed at the interface
between the neighbouring grains [27]. This was attributed to the large interface to volume
ratios. At lower frequency range, large MWS interfacial polarisation effect leads to range
dielectric constant. At higher frequency level, the change carriers were confined, takes
relatively Longley time was required for the accumulation and movement process. At vari-
ous temperatures, the dielectric loss is illustrated as a function of frequency in Figure 10.
Both the values for dielectric loss and dielectric constant were reduced at an increased fre-
quency level. The dielectric loss was professional with increasing temperatures. It is high
292 S. SAGADEVAN ET AL.

Figure 9. Dielectric constant of the CuO/rGO nanocomposite.

Figure 10. Dielectric loss of the CuO/rGO nanocomposite.

at lower frequency level, but with enhanced temperatures it dropped significantly [28, 29].
The magnitude of dielectric loss was increased with increasing temperature. This was evi-
dent and was further confirmed the thermally activated characteristics of the dielectric
relaxation of the composite system [30].
Figure 11 illustrates the behaviour of ac conductivities with frequency changes for
the CuO/rGO nanocomposites. The conductivity of the CuO/rGO NC may be split into
two regions: (i) the low-frequency region, where the conductivity is mostly influenced
by dc conductivity and (ii) the high-frequency region, which is mainly distinguished by
frequency-dependent conductivity which confirms the ac conductivity due to MWS
interfacial polarisation effects and dielectric relaxations [31]. Thus, due to MWS
 JOURNAL OF EXPERIMENTAL NANOSCIENCE 293

Figure 11. AC conductivity of the CuO/rGO nanocomposite.

interfacial polarisation, the ac conductivities have increased with frequency for the
CuO/rGO NC.

4 Conclusion
A simple and cost-effective strategy has been developed to obtain CuO/rGO nanocompo-
sites. Homogenous dispersion of CuO having monoclinic phase was observed over the
surface of rGO. The XRD spectra confirmed the formation of CuO and rGO. Surface
functional groups present over CuO and rGO were confirmed using FTIR and Raman
analysis. Surface morphological features with particle size and shape were confirmed by
FESEM and TEM analysis. The electrochemical performance of the CuO/rGO nanocom-
posite was enhanced due to the presence of graphene inside its matrix. The surface area
of graphene sheets is greatly reduced by its aggregation intensities. This is attributed to its
enhanced specific capacitance, better stability as well as increased wettability of the elec-
trode materials. Hence, the electrochemical results suggest that CuO/rGO nanocomposite
is a prominent candidate for high-performance supercapacitor devices. The dielectric con-
stant, dielectric loss and AC conductivity were determined and the values were estimated
at different frequencies and temperature level. The magnitude of dielectric constant and
dielectric loss values were inversely proportional with increase in temperature and fre-
quency. The conductivity behaviour revealed that the sample was here thermally activated.
The AC conductivity values were dependent on the frequency level at higher temperature.
At higher temperature, the values were increasing significantly. The AC conductivity was
temperature dependent and with elevated temperature – it was increasing also.

Acknowledgements
This work has been made possible because of the generous grants RP044C-17AET and RP044D-17AET
from the University Malaya, Malaysia. One of the authors (Suresh Sagadevan) acknowledges the honour,
namely the “Visiting fellow” at the Department of Physics, Center for Defence Foundation Studies,
Universiti Pertahanan Nasional Malaysia, Kem Sg. Besi, 57000 Kuala Lumpur, Malaysia. The author
wishes to place on record his heartfelt thanks that are due to the authorities concerned.
294 S. SAGADEVAN ET AL.

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