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One-pot synthesis of CuO nanoflowerdecorated reduced graphene oxide and its

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DOI: 10.1039/C1CY00374G

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One-pot synthesis of CuO nanoower-decorated reduced graphene oxide

and its application to photocatalytic degradation of dyesw
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Sen Liu,a Jingqi Tian,ab Lei Wang,a Yonglan Luoa and Xuping Sun*a
Received 17th September 2011, Accepted 13th October 2011
DOI: 10.1039/c1cy00374g
In this paper, we demonstrate our recent nding that CuO nanoower-decorated reduced
graphene oxide (CuONF/rGO) nanocomposites can be successfully prepared by heating the
mixture of Cu salts and GO in the presence of poly[(2-ethyldimethylammonioethyl methacrylate
ethyl sulfate)-co-(1-vinylpyrrolidone)] (PQ11) and urea for the rst time. Several analytical
techniques, including UV-vis spectroscopy, Raman spectroscopy, X-ray diraction (XRD),
transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) have been
used to characterize the resulting CuONF/rGO nanocomposites. We further demonstrated that
such CuONF/rGO nanocomposites can serve as an eective photocatalyst for degradation of
rhodamine B (RhB) under UV irradiation. It also suggests that these CuONF/rGO
nanocomposites exhibit a higher photocatalytic activity toward degradation of RhB than CuO
nanoparticles or rGO samples.

Introduction
Graphene, a monolayer of sp2-bonded carbon atoms tightly
packed into a two-dimensional (2D) honeycomb lattice, and
characterized as the thinnest material in our universe, has
recently received considerable attention.1 Because of its high
surface area (B2600 m2 g 1), high chemical stability, and
unique electronic, mechanical properties, graphene has great
promise for potential applications in nanoelectronics, composites,
Li ion batteries, sensors etc.2 Compared to other methods for
production of graphene, the strategy based on chemical
reduction of graphene oxide (GO) has great advantages of
low cost and bulk quantity production and reduced graphene
oxide (rGO) thus formed has been widely used for preparation
of graphene-based nanocomposites.3 Particularly, metal or
metal oxide/rGO composites have attracted considerable interest
because of the combination of remarkable unusual properties
of metal or metal oxide with graphene and hence their synthesis
and application have become of scientic and technological
importance.4 Recent research has shown that graphene is a
promising candidate for preparation of graphene-based hybrids
for adsorption and separation of dyes and photocatalytic
degradation of dyes due to its high surface area and p-rich
structure.5 Indeed, graphene has been successfully decorated with
a

State Key Lab of Electroanalytical Chemistry, Changchun Institute

of Applied Chemistry, Chinese Academy of Sciences, Changchun
130022, Jilin, P. R. China. E-mail: sunxp@ciac.jl.cn;
Fax: +86-431-85262065; Tel: +86-431-85262065
b
Graduate School of the Chinese Academy of Sciences,
Beijing 100039, China
w Electronic supplementary information (ESI) available. See DOI:
10.1039/c1cy00374g

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numerous inorganic materials including gold, Ag@AgCl, ZnO,

TiO2, Cu salts by various methods, leading to nanocomposites
with photocatalytic activity for degradation of dyes.6
CuO as a p-type semiconducting material has received
considerable attention due to its wide applications in many
important elds such as gas sensors, magnetic phase transitions,
superconductors and photocatalysts.7 Inspired by enhancement
of the properties of nanoparticles through anchoring them
onto graphene sheets, researchers have attempted to prepare
CuO nanoparticle decorated graphene sheets. Up to now,
however, only very limited methods have been developed,
including heating an aqueous solution of Cu salts in the
presence of graphene synthesized by an arc discharge method,8a
solvothermal synthesis of CuO/GO and the subsequent
reduction of GO by hydrazine vapor,8b and chemical reduction
of Cu salts in an aqueous solution in the presence of hydrogen
induced exfoliated graphene (HEG).8c Unfortunately, all these
above-mentioned methods suer from more or less drawbacks
such as the involvement of two steps in the preparation and
thus complex and time-consuming, high cost and poor dispersing
ability of resulting nanocomposites, which limit their wide
applications. Accordingly, developing simple and economical
methods for preparation of CuO/graphene nanocomposites is
highly desired.
In this study, we developed a facile strategy for one-step
preparation of well-stable aqueous dispersion of CuO nanoower-decorated rGO (CuONF/rGO) nanocomposites, carried
out by heating the mixture of Cu salts and GO in the presence
of poly[(2-ethyldimethylammonioethyl methacrylate ethyl
sulfate)-co-(1-vinylpyrrolidone)] (PQ11) and urea. It suggests
that the resulting CuONF/rGO nanocomposites can serve as an
Catal. Sci. Technol., 2012, 2, 339344

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eective photocatalyst for degradation of rhodamine B (RhB)

under UV irradiation and their photocatalytic activity is
higher than that of CuO nanoparticles or rGO samples.

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Experimental section
PQ11, graphite powder, Cu(OAc)2
H2O, urea, and H2O2
(30%) were purchased from Aladin Ltd. (Shanghai, China).
NaNO3, RhB, H2SO4 (98%), and KMnO4 were purchased
from Beijing Chemical Corp. All chemicals were used as
received without further purication. The water used throughout all experiments was puried through a Millipore system.
UV-vis spectra were obtained on a UV5800 spectrophotometer. Raman spectra were obtained on a J-Y T64000 Raman
spectrometer with 514.5 nm wavelength incident laser light.
Powder X-ray diraction (XRD) datum was recorded on a
RigakuD/MAX 2550 diractometer with Cu Ka radiation
(l = 1.5418 A). X-Ray photoelectron spectroscopy (XPS)
analysis was measured on an ESCALABMK II X-ray photoelectron spectrometer using Mg as the exciting source. Transmission electron microscopy (TEM) measurements were made
on a Hitachi H-8100 electron microscope (Hitachi, Tokyo,
Japan) with an accelerating voltage of 200 kV. The sample for
TEM characterization was prepared by placing a drop of
colloidal solution on a carbon-coated copper grid and drying
at room temperature.
GO was prepared from natural graphite powder through a
modied Hummers method.9 In a typical synthesis, 1 g of
graphite was added into 23 mL of H2SO4, followed by stirring
at room temperature over a period of 24 h. After that, 100 mg of
NaNO3 was introduced into the mixture and stirred for 30 min.
Subsequently, the mixture was kept below 5 1C using an ice bath,
and 3 g of KMnO4 was slowly added into the mixture. After
being heated to 3540 1C, the mixture was stirred for another
30 min. After that, 46 mL of water was added into the above
mixture during a period of 25 min. Finally, 140 mL of water and
10 mL of 30% H2O2 were added into the mixture to stop the
reaction. After the unexploited graphite in the resulting mixture
was removed by centrifugation, as-synthesized GO was dispersed
into individual sheets in distilled water at a concentration of
0.5 mg mL 1 with the aid of ultrasound for further use.
CuONF/rGO nanocomposites were prepared by heating the
mixture of Cu(OAc)2
H2O and GO in the presence of PQ11
and urea. In a typical synthesis, 26 mg of Cu(OAc)2
H2O and
16 mg of urea were added into 10 mL of ethanol, followed by
addition of 1 mL of 0.67 M PQ11 aqueous solution and 1 mL
of GO (0.5 mg mL 1) solution. After sonication at room
temperature for 20 min, the solution was transferred into an
autoclave and then heated at 180 1C for 40 min. The solid
products were obtained by centrifugation, washed by water and
ethanol, and dispersed into water for further characterization
and use. The rGO and CuO nanoparticles were also prepared
in a similar method without adding Cu(OAc)2
H2O and GO,
respectively.
The photocatalytic activity of the CuONF/rGO nanocomposites, CuO nanoparticles, and rGO was evaluated by
the degradation of a model pollutant RhB. For the degradation
of RhB, the reactor was placed in a sealed black box with
an open top and was irradiated by a UV light source with a
340

Catal. Sci. Technol., 2012, 2, 339344

150 W xenon lamp. In a typical run, 100 mL of catalyst dispersion

was added into 3 mL of H2O, followed by addition of 100 mL of
H2O2 and 10 mL of RhB solution (2 mg mL 1 in ethanol). The
concentration of RhB in the solution was determined using a
UV5800 spectrophotometer by collecting the absorbance of RhB
at 553 nm.

Results and discussion

Fig. 1 shows the Raman spectra of GO and the products
obtained by heating the mixture of Cu(OAc)2
H2O and GO in
the presence of PQ11 and urea. It is well-known that graphene
obtained by chemical reduction of GO exhibits two characteristic
main peaks: the D band at B1350 cm 1, arising from a
breathing mode of k-point photons of A1g symmetry; the G
band at 1575 cm 1, arising from the rst order scattering
of the E2g phonon of sp2 C atoms.10 In our present study, it
is seen that both GO and the products exhibit a D band at
1347 cm 1 and a G band at 1604 cm 1. It is also found that the
products show relatively higher intensity of D to G band (0.96)
than that of GO (0.77). These observations conrm the
formation of new graphitic domains after the heat treatment
process. Fig. 1 inset shows the photographs of aqueous
dispersion of GO (left) and the products thus obtained (right),
revealing a distinct color change from pale-yellow to black
after heat treatment. Such observation provides another piece
of evidence to support the formation of rGO.
The XRD pattern of products thus obtained as shown in
Fig. 2 exhibits that three diraction peaks at 2y of 35.8, 39.2
and 62.01 are observed, which are assigned to the (002), (200)
and ( 113) planes of monoclinic CuO (JCPDS 45-0397),
respectively.11 Note that except for these CuO peaks, no other
peaks corresponding to Cu or Cu2O are observed. All these
observations indicate that CuO samples were successfully
prepared by heat treatment of Cu(OAc)2 solution in the
presence of PQ11 and urea.
The surface composition and element analysis for the overall
composition of the resulting products were characterized by an
XPS technique. Fig. 3 shows the XPS spectrum of products,
revealing three peaks at 285.5, 400.9 and 531.0 eV, which are
attributed to C1s, N1s, and O1s, respectively.12 Other two peaks

Fig. 1 Raman spectra of GO (a) and products thus obtained (b). Inset:
photographs of GO (left) and products (right) in aqueous solution.

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Fig. 2

XRD pattern of products thus obtained.

at 933.3 and 77.0 eV associated with Cu2p and Cu3p, respectively, are also observed.13 XPS results show that products
thus obtained are formed from Cu(OAc)2 and GO, while
the observation of N element in the XPS spectrum indicates
the presence of PQ11 on the surface of such products. It is
also found that the O1s intensity of products is signicantly
decreased compared with that of GO, suggesting the loss of
oxygen in GO after the heat treatment.14
Fig. 4 shows the C1s spectra of GO and the products,
respectively. The C1s spectra of GO and the products could
be deconvoluted into three peaks at 284.5, 286.6, and 288.4 eV,
which are associated with CC, CO, and CQO, respectively.
It is obviously seen that the peak intensity of CO and CQO is
strong in GO (Fig. 4a); in contrast, after heat treatment, the
peak intensity of CO and CQO in the products tremendously
reduced (Fig. 4b). In addition, it is also seen that a new peak at
286 eV attributed to the CN band is observed, further
conrming the presence of PQ11. All the observations suggest
that the most oxygen-containing functional groups are successfully
removed after heat treatment.15
Fig. 5 shows the Cu2p spectrum of products thus obtained.
It is seen that the Cu2p spectrum exhibits a copper 2p1/2 peak
at 953.3 eV and a 2p3/2 peak at 933.7 eV, which are 1.3  0.2 eV
higher than the peak positions for Cu(0) metal and are attributed
to oxidized Cu(II).16 Strong shake-up satellite peaks are also

Fig. 3 XPS spectra of GO (a) and products thus obtained (b).

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Fig. 4 C1s spectra of GO (a) and products thus obtained (b).

observed at B942.0 eV and an overlapping series at B962.1 eV,

further conrming the presence of Cu(II) on the surface.16 All
these observations further conrm the formation of CuO.
Fig. 6a shows the low magnication TEM image of the
products, indicating the formation of CuO nanoparticle-decorated
rGO. The high magnication TEM image (Fig. 6b) further
reveals that such nanoparticle consists of smaller nanoparticles
and is ower in shape, suggesting the formation of CuONF/
rGO. It is worthwhile mentioning that the dispersion of the

Fig. 5

Cu2p spectrum of products thus obtained.

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Fig. 6 TEM images of CuONF/rGO nanocomposites.

resulting CuONF/rGO can be well-stable for several weeks

without the observation of any oating or precipitate particles,
owing to the presence of PQ11 which has been used as an
eective stabilizing agent for rGO and metal nanoparticles in
our previous studies.17
It should be noted that GO has been successfully reduced by
heating the mixture of GO and Cu salts in the presence of
PQ11 and urea at 180 1C for 40 min. The production of rGO
from GO can be attributed to the various factors in the present
study, including the high temperature used,18 the heat treatment
of GO by alcohol,19 the treatment of GO by alkaline formed
by hydrolysis of urea20 as well as the reduction of GO by the
reducing agent PQ11.11b,c All the above factors play an
important role in reduction of GO, and thus, a short time is
required to complete reduction of GO. We have found that
CuO nanoparticles with diameter of 24 nm were obtained
by heating the mixture of Cu salts in the presence of PQ11,
but the products prepared in the absence of PQ11 are nanoparticle aggregates about 50100 nm in size,21 indicating that

Scheme 1
method.

342

PQ11 serves as an eective stabilizing agent. Furthermore, our

previous report also suggests that PQ11 is a good stabilizing
agent for formation of rGO.11a It is also found in our present
study that heat treatment of the mixture of Cu salts and GO in
the absence of PQ11 results in the formation of aggregates of
rGO and CuO (Fig. S1, ESIw). All the above observations
suggest that PQ11 plays an important role in the formation of
CuONF/rGO, serving as an eective stabilizing agent for
formation of CuO nanoparticles and a good reducing and
stabilizing agent for formation of stable rGO dispersion. Due
to the strong interaction between PQ11 and CuO nanoparticles as well as rGO, an assembly process occurs, resulting
in the formation of a CuO nanoower on the surface of rGO.
The possible formation mechanism is proposed as follows:
CuO nanoparticles and rGO are formed from Cu salts and GO
in the presence of PQ11 and then CuO nanoparticles thus
formed are subsequently assembled into CuONF on rGO with
the aid of PQ11. Scheme 1 presents a scheme (not to scale) to
illustrate the formation of CuONF/rGO nanocomposites from

A scheme (not to scale) to illustrate the formation of CuONF/rGO nanocomposites from GO and Cu salts by a one-pot heat treatment

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that the color of RhB solutions becomes less intense, and the
intensity of absorption spectra decreases gradually with increasing
irradiation time, indicating that a strong oxidation of RhB has
occurred in the presence of CuONF/rGO under UV irradiation.
All these observations indicate that CuONF/rGO nanocomposites exhibit excellent performance for degradation of RhB.
According to the previous report,7e the possible mechanism
for degradation of RhB may be proposed as follows: the
photodecomposition of H2O2 to form a certain amount of
OH
in the presence of CuO nanoower rst, and then these
OH species oxidize degradation of RhB into CO2, H2O and
other mineralization through a series of redox reactions.

Conclusions
In summary, CuONF/rGO nanocomposites have been successfully prepared by heating the mixture of Cu salts and GO in
the presence of PQ11 by a one-pot route. The photocatalytic
degradation of RhB by CuONF/rGO nanocomposites in the
presence of H2O2 has also been demonstrated and it revealed
that the CuO nanoowers contained therein exhibit notable
catalytic activity toward the degradation of RhB. Our present
ndings provide us a simple approach to the facile production
of metal oxide decorated rGO on a large scale for photocatalytic
applications.

Acknowledgements
This work was supported by National Basic Research Program
of China (No. 2011CB935800) and the National Natural Science
Foundation of China (No. 21175129).
Fig. 7 Photodegradation of RhB (a) over CuONF/rGO (), without
catalyst (K), over CuO nanoparticles (m), and rGO (.) (b) under UV
light irradiation.

GO and Cu salts in the presence of PQ11 by a one-pot heat

treatment route.
As a demonstration of application of such CuONF/rGO,
RhB was chosen as a representative organic dyestu to
evaluate the photocatalytic performance. Fig. 7a shows the
photocatalytic performance of various catalysts for degradation
of RhB in the presence of H2O2. In the absence of a photocatalyst, RhB was degraded slowly by H2O2. It is seen that the
degradation of RhB was greatly enhanced in the presence of
CuONF/rGO, indicating the excellent photocatalytic activity
of CuONF/rGO. However, CuONF/rGO exhibits no obvious
photocatalytic activity in the absence of H2O2 (Fig. S2, ESIw).
Furthermore, the degradation of RhB was slightly enhanced in
the presence of CuO nanoparticles or rGO, which is attributed
to the catalytic oxidation of RhB by CuO and adsorption of
RhB by rGO, respectively. It should be noted that the high
photocatalytic activity of CuONF/rGO can be attributed to
the fast adsorption of RhB by pp stacking interactions
between RhB and the p-conjugation system of CuONF/rGO
as well as the two-dimensional planar structure of CuONF/
rGO, leading to the fast degradation of RhB.6e Fig. 7b shows
the typical time-dependent UV-vis absorption spectra of RhB
solution during the photodegradation in the presence of
CuONF/rGO with the aid of H2O2. It is seen that RhB
exhibits a maximum absorption peak at around 553 nm. Note
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results.

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The Royal Society of Chemistry 2012