Applied Surface Science 311 (2014) 602–608

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Applied Surface Science

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

Controllable fabrication of CuO nanostructure by hydrothermal

method and its properties
Tingting Jiang, Yongqian Wang ∗ , Dawei Meng, Xiuling Wu, Junxia Wang, Jieyu Chen
Faculty of Material Science and Chemistry, China University of Geoscience, Wuhan 430074, China

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

Article history: The copper oxide (CuO) nanostructures of varying shape were synthesized by a simple hydrothermal
Received 23 March 2014 method without using any template and surfactants. The influences of reactant concentration, hydro-
Received in revised form 6 May 2014 thermal temperature and time on the growth of nanostructure were investigated. And the samples were
Accepted 18 May 2014
characterized by means of scanning electron microscope (FESEM) and X-ray powder diffraction (XRD).
Available online 26 May 2014
At the same time, photo-decomposition test and UV–vis spectroscopy were done. The results shows that
the CuO nanostructure has monoclinic structure with single crystalline phase. However, the structure
Keywords:
and morphology of CuO nanocrystal can be controlled by changing reactant concentration. Its photo-
CuO nanostructure
Hydrothermal method
degradation rate to methylene blue can reach 92.1%. And the optical band gap calculated of nanosheets is
Photo-decomposition found about 5.89 eV. Moreover, the plausible growth mechanism for the formation of CuO nanostructure
Growth mechanism is proposed.
© 2014 Elsevier B.V. All rights reserved.

1. Introduction tadpole-shaped [14] and other unique morphology have been

Copper oxide (CuO) is an important p-type metal oxide semi-
conductor with narrow band gap (1.2 eV) [1]. At the same time, it is
a good Mott Insulator (transition metal oxides) and the basic com-
ponent unit of high temperature superconductor. The electronic
structure of CuO cannot be simply explained by traditional band
theory [2]. It possesses unique physical properties and great poten-
tial for diverse electronic and photonic applications that require
superconductivity, colossal magnetoresistivity, and piezoelectric-
ity, which has received considerable attention due to its potential
applications in many fields, such as solar energy conversion, bat-
teries, magnetic storage media, gas sensing, catalysis, and field
emission [3–5].
When the dimension of CuO decreases to nanoscale, such
nanostructure exhibits unique structural characteristics and size
confinement effects along with novel physical properties [6].
Nanoscale CuO with different shapes and dimensions, such as nano-
tubes [7], nanowires [8], nanosheets [9] and nanoneedles [10] have
been synthesized by using numerous methodologies. Of course, the
great diversity of applications needs the distinct morphological and
functional CuO nanostructures. Several complex nanostructures
including nanoflowers [11], spherical-like [12], urchin-like [13],
∗ Corresponding author. Tel.: +86 13871379285; fax: +86 02767885162.
E-mail addresses: cugwyq@126.com, wyq@cug.edu.cn (Y. Wang).
explored. Studies on the preparation and properties of nanostruc-
tured materials are one of the most important topics at present. Up
to now, various approaches have been used to fabricate the CuO
nanostructure, such as solid state reaction process [15], sol–gel
method [16], hydrothermal method [3,12,14], thermal oxidation
method [17], electrochemical method [18], template methods
using carbon nanotubes [19], sonochemical method [20] and so on.
Among these methods, hydrothermal synthesis is of great interest
in fabrication of CuO nanostructures due to its easy manipula-
tion, scalable production, well-defined size and shape, and low cost
[21].
Recently, the research on the shape control of various nanostruc-
tures has been widely developed because physical and chemical
properties are strongly dependent on the sizes, shapes, compo-
sitions, and structures of the nanocrystals. CuO nanostructures
are extensively used in various other applications, including
photodetectors [22], field emissions, gas sensors [14], energetic
materials (EMs), bio-sensors [23], supercapacitors [24], nanofluid
[25], photocatalysis [26], and magnetic storage media. In this arti-
cle, we report the synthesis of CuO nanostructures by a simple and
convenient surfactant-free hydrothermal method in the presence
of sodium hydroxide (NaOH). The influences of concentration of
reactants, hydrothermal temperature and time on the growth of
crystals were investigated, and the formation mechanism of CuO
nanostructure and its fundamental properties was proposed and
discussed.

http://dx.doi.org/10.1016/j.apsusc.2014.05.116
0169-4332/© 2014 Elsevier B.V. All rights reserved.
 T. Jiang et al. / Applied Surface Science 311 (2014) 602–608
2. Experiment
2.1. Chemicals
All chemical reagents were analytical grad and purchased with-
out any further purification including absolute ethyl alcohol, copper
acetate and sodium hydroxide.
2.2. Preparation of copper oxide nanostructures
The CuO nanostructure was obtained by hydrothermal pro-
cess without the use of surfactants. The experimental procedures
were simply described as follows: First, 4 g Cu(CH3 COO)2 ·H2 O
was dissolved in 50 mL water under stirring until completely dis-
solved. Next, 40 mL sodium hydroxide aqueous solution (1 M/L)
was introduced into above aqueous solution with the drop-wise
addition under continuous stirring. Then, the total 90 mL solution
was transferred into a Teflon lined stainless steel autoclave, which
was sealed and maintained at 110 ◦ C for 2 h. Last, the autoclave was
took out and cooled to room temperature naturally. After terminat-
ing the reaction, black precipitate was obtained which was washed
with deionized water and ethanol and finally dried at 90 ◦ C in air.
2.3. Property characterization
The general morphologies of the synthesized CuO nanostruc-
tures were examined by using field emission scanning electron
microscopy (FESEM, U8100, HITACHI). The SEM samples were pre-
pared with a thin amorphous gold on their surface. And the crystal
phase of the product was characterized by X-ray diffraction (XRD,
D8 Advanced XRD, Bruker AXS).
In the test of photo-decomposition, the methyl blue solution
of 12 mg/L was poured into three beakers. One was mixed with
CuO nanocrystal and another was mixed with CuO powder. And
the rest was used as reference. All of them were illuminated by
a high pressure mercury lamp (160 W) at 15 cm vertical distance.
The absorbance of methyl blue solution was measured by a UV–vis
spectrophotometer (UV-2550, Shimadzu, Japan).
3. Results and discussion
Hydrothermal reaction is an effective method to obtain desir-
able crystals, such as mild conditions, controllable morphology, low
aggregation and high crystallinity. During the hydrothermal reac-
tion process, the temperature and pressure of system and other
conditions have obvious effect on the microstructure of the product.
In order to get the influence of hydrothermal reaction conditions on
the product, we explore the impact of four factors on the CuO mor-
phology and its structure including copper acetate concentration,
precipitant, reaction temperature and reaction time.
3.1. The influence of preparation parameters on the CuO
nanostructure
3.1.1. Influence of copper acetate concentration
Fig. 1 shows the XRD patterns of the samples prepared by the
hydrothermal processing at 110 ◦ C for 2 h with different concentra-
tion of copper acetate. All of the diffraction peaks can be indexed as
the monoclinic phase of CuO with the lattice constants a = 4.68 Å,
b = 3.43 Å, c = 5.13 Å and ˇ=99.26◦ or 99.47◦ , which are consistent
with the values in the standard card (JCPDS 80-0076 or JCPDS
05-0661), as previously reported [27]. No other impurities were
detected by XRD analysis, indicating the phase purity of CuO nano-
structures. And the major peaks located at 2=35.5◦ and 38.7◦
are indexed as (0 0 2) and (1 1 1) crystal planes, respectively. The
broadening of all recorded peaks in the spectrum indicates the
603
Fig. 1. XRD patterns of CuO nanostructure fabricated by hydrothermal approach at
different concentration of copper acetate: (a) 0.02 M/L, (b) 0.08 M/L, (c) 0.1 M/L, (d)
0.2 M/L, (e) 0.3 M/L, (f) 0.4 M/L, (g) 0.5 M/L, (h) 0.6 M/L, (i) 0.7 M/L.
presence of nanoscale crystallites. Moreover, with the increase of
Cu(CH3 COO)2 concentration from 0.06 M/L to 0.7 M/L (from pat-
tern 1a to pattern 1i), the diffraction peaks become the highest
and the narrowest when the concentration of copper acetate is
0.2 M/L, which illustrates that the crystallization and size of CuO
nanostructure are enhance to maximum.
The general morphologies of the synthesized CuO products pre-
pared by hydrothermal route at different reactant concentration
were analyzed by FESEM and results are shown in Fig. 2. With
the increase of the Cu(CH3 COO)2 concentration, the morphology of
CuO nanostructure has a large change. The morphology of flower-
like CuO nanostructures is obtained at 0.4 M/L, as shown in Fig. 2a,
which indicates that the flower-like CuO nanostructures are com-
posted of the irregular nanosheets with about 70 nm in width
and 1.7 ␮m in length. With the reactant concentration increas-
ing, the morphology of flower-like CuO nanostructures disappeared
and dispersed plume-like nanosheets formed, as shown in Fig. 2b.
The size of nanoplates is about 400 nm in width and 900 nm in
length. When the reactant concentration is equivalent to 0.6 M/L,
the morphology transformed into spindle-like nanostructure. So,
the morphology of CuO nanocrystals can be controlled by changing
reactant concentration.
3.1.2. Influence of sodium hydroxide
In order to explore the influence of NaOH on the formation of
CuO nanostructure, we keep the same reaction conditions at 110 ◦ C
for 2 h by using Cu(CH3 COO)2 concentration of 0.4 M/L. The powder
XRD patterns of CuO nanostructure prepared with NaOH or not are
shown in Fig. 3. The products are well indexed to monoclinic phase
according to standard card JCPDS 05-0661. Compared to Fig. 3a, it
is clear that the characteristics peaks in Fig. 3b are sharper and nar-
rower, indicating that the sample synthesized with NaOH has better
crystallinity. No characteristic peaks such as Cu (OH)2 or CuO2 were
detected in both of products.
Fig. 4 shows the morphology of nanostructure grown with NaOH
or not under the same conditions. When the synthesis process was
carried out without NaOH, hericium erinaceus-like morphology of
CuO was obtained, as shown in Fig. 4(a). However, with the concen-
tration of NaOH increasing to 1 M/L, distinct change has taken place
in morphology and layered structure of CuO nanostructure occurs,
which we can conclude from Fig. 4(b). That is to say, NaOH plays
604 T. Jiang et al. / Applied Surface Science 311 (2014) 602–608

Fig. 2. The FESEM images of CuO nanostructure prepared under different concentration of copper acetate at 110 ◦ C for 2 h: (a) 0.06 M/L, (b) 0.4 M/L, (c) 0.6 M/L.

Fig. 3. XRD patterns of CuO nanostructure fabricated by hydrothermal approach Fig. 5. XRD patterns of CuO nanostructure fabricated by hydrothermal approach at
under 0.4 M/L copper acetate at 110 ◦ C for 2 h: (a) without NaOH, (b) 1.0 M/L NaOH. different reaction temperature: (a) 110 ◦ C, (b) 140 ◦ C, (c) 170 ◦ C.

an important role to decide the morphology of CuO nanostruc-
tures because OH− is mightily related to the reaction that forms
nanocrystals.
3.1.3. Influence of reaction temperature
In this work, the concentration of Cu(CH3 COO)2 and NaOH was
set to 0.4 M/L and 1 M/L severally. At the same time, the hydro-
thermal time was kept at 2 h. To check the influence of reaction
temperature on crystal phases and crystallinity of the synthesized
nanostructures, XRD pattern was done and presented in Fig. 5.
All reflection peaks in the XRD patterns of the as-synthesized
products are well-matched to monoclinic CuO (JCPDS 05-0661),
respectively. Except CuO, no other peaks were observed in the
pattern, which verified that the synthesized nanostructures were
pure CuO. However, with the temperature increasing from 110 ◦ C
to 170 ◦ C, the diffraction peaks become higher and narrower.
The increase of crystallization expounds larger grains. Therefore,
raising the temperature in a certain temperature range can improve
the crystallinity of nanocrystalline.
Fig. 6 shows the FESEM images of the as-synthesized CuO
nanostructure prepared by hydrothermal route at different tem-
peratures. It can be seen that each of them is lamellar nanostructure.
With the increase of the temperature, the morphology of CuO nano-
structure has a slight change that the length of the nanosheets
become shorter, as shown in Fig. 6a–c. From Fig. 6d, we can see
that when the hydrothermal temperature is up to 170 ◦ C, the CuO
nanosheets are about 600 nm in length and 200 nm in width.
3.1.4. Influence of reaction time
Fig. 7 shows the XRD patterns of the samples prepared by
the hydrothermal method with 0.4 M/L copper acetate and 1 M/L
sodium hydroxide at different reaction time. The hydrothermal
time was varied from 2, 4, 8, 12, 24, 48 to 72 h while the hydro-
thermal temperature was kept at 110 ◦ C. The synthesized powder is

Fig. 4. The FESEM images of CuO nanostructure prepared with 0.4 M/L copper acetate at 110 ◦ C for 2 h: (a) without NaOH, (b) 1.0 M/L NaOH.
 T. Jiang et al. / Applied Surface Science 311 (2014) 602–608
Fig. 6. The FESEM images of CuO nanostructure prepared under different reaction temperature: (a) 110 ◦ C, (b) 140 ◦ C, low magnified (c) and high magnified (d) images at
170 ◦ C.
composed of JCPDS (05-0661) data of CuO with monoclinic phase.
No impurity peaks such as Cu(OH)2 or Cu2 O are found, suggest-
ing the pure phase of the products. On the other hand, along with
the extending of reaction time, the higher and narrower diffraction
peaks indicates that the reaction time also has some influences on
the products to some degree, but the impact is just a little. This phe-
nomenon may be due to in the condition of excess alkali solution,
the reducing activity of acetic acid from hydrolysis reaction could
not play out.
The morphology of as-synthesized CuO products under different
reaction time was observed by using FESEM analysis and is shown
in Fig. 8 of a low magnification FESEM image of CuO nanosheets.
Compared to the morphology of CuO nanosheets at 2 h, the lamel-
lar nanostructure of CuO at 12 h has become clearer and possesses
smaller size. It is obvious that the reaction time has little influence
on the morphology and structure of the products.
Fig. 7. XRD patterns of CuO nanostructures fabricated by hydrothermal approach
at different reaction time: (a) 2 h, (b) 4 h, (c) 8 h, (d) 12 h, (e) 24 h, (f) 48 h, (g) 72 h.
605
3.2. Growth mechanism of nanostructure
As a physical phenomenon, the Ostwald ripening process has
been universally known to explain the formation of a crystal, whose
process means the growth of larger crystals from smaller crystals
because the smaller has higher solubility than the larger [28].
Fig. 9 shows a schematic representation of the formation mecha-
nism of CuO nanosheets by using the hydrothermal method. Fig. 9a
indicates the primary stage from the synthesis of CuO nanosheets.
First, the dissolution of Cu(CH3 COO)2 ·H2 O and NaOH in water
at room temperature promotes the hydrolysis reaction on these
chemical reagents. Thus, this process leads to the formation of
Cu(OH)2 and solvation of (CH3 COO)− and Na+ ions. After several
seconds, the first precipitates of Cu(OH)2 were formed. Accord-
ing to the document account, the (0 1 0) plane of this hydroxide
is a corrugated sheet structure and a sheet of distorted [Cu(OH)6 ]
octahedra is formed by edge sharing [29]. The 2D layers of these
sheets parallel to the (0 1 0) plane are connected through H-bonds
[30]. Fig. 9b shows a diagrammatic sketch of the formation pro-
cedure of CuO nanosheets by hydrothermal method. The heating
make the interplanar H-bonds break and accordingly speeds up the
dehydration rate. As a result, this mechanism contributes to rapidly
transform Cu(OH)2 (orthorhombic structure) into CuO nanoplates
(monoclinic structure). On the other hand, the heating is able to pro-
mote an increase of the effective collisions between CuO particles.
Consequently, it promotes a growth process on the crystallographic
planes of high atomic densities and more favorable thermodynami-
cally [31]. Fig. 9c and d shows an Ostwald-ripening mechanism that
is identified to be the chief formation mechanism involved in early
stage. And then under the force of van der Waals, the aggregation of
plates surface takes place. In fact, it is reported that at the foremost
stage of the hydrothermal process to form CuO nanosheets, no mat-
ter the small nanosheets or the large nanoplates would be emerged
in non-equilibrium solution of autoclave. And then, the solvated
H-ions generated from the small nanosheets by degrees in the solu-
tion could spontaneously transfer onto the surface of some large
ones. As a consequence, large CuO crystals would be provided as
the seeds for the growth of nanosheets at the cost of the small ones
by Ostwald ripening [32]. Ostwald-ripening mechanism, that is dis-
solution/recrystallization, is usually used to interpret the growth of
nanocrystals during the hydrothermal processing. So, owing to the
606 T. Jiang et al. / Applied Surface Science 311 (2014) 602–608

Fig. 8. The FESEM images of CuO nanostructure prepared under different reaction time. (a) 2 h, (b) 12 h.

larger nanocrystals are more energetically favored than the smaller,
the thermodynamically-driven spontaneous process could be able
to happen. Meanwhile, the heating can strengthen the aggregation
of plates surface through the force of van der Waals along the pref-
erential growth directions of [1 0 0] and [0 1 0]. Eventually, due to
the fast nucleation from the first seeds and collision between small
sheets, the formation of irregular and agglomerate CuO nanosheets
is done. And the vast quantities of CuO nanoplates would be longer,
wider and thicker in size [29,33].
The differences observed in these morphologies can be related to
the variations in the electron density of the ligands by steric imped-
iment. And precipitant such as NaOH would have great influence on
the crystallographic orientation. When the concentrations of Cu2+
or OH− is not enough to spontaneously form more fine CuO nuclei
in the aqueous complex solution, CuO nanocrystals would growth
along with the surface of first seeds to use less energy, which forms
tufted structure rather than scattered crystals.
3.3. UV–vis studies of CuO nanosheets
Fig. 10 shows the UV–vis spectra of CuO nanosheets and the
(˛h)2 vs. h plot for the sample along with the fitted portion of
the curve. Its broad absorption peak is observed at 265 nm. The
optical band-gap of the CuO nanostructure is obtained by using the
Tauc’s relation [34], as shown below.
n
 
(˛hv) = B hv − Eg (1)
In which, ˛ is the absorption coefficient which is calculated
by the relation: ˛=2.303A/t, where A is absorbance and t is the
thickness of the samples. Besides, hv is the photon energy of
radiation, superscript n represents the nature of transition, Eg is
the optical band-gap of the materials and B is constant related to
the material and matrix element of the transition. It is worth saying
explicitly that when the values of 1/2, 2, 3/2 and 3 are taken for n,
these numbers, respectively, correspond to allowed direct, allowed

Fig. 9. Schematic representation of the synthesis and growth process of CuO plates. (a) Initial stage from the chemical synthesis for the formation of Cu(OH)2 and small
plates. (b) Increase of the effective collision rates between small plates by the heating, promoting the dehydration process and the rapid formation process of CuO plates. (c)
Growth process of CuO plates along the [1 0 0] and [0 1 0] directions. (d) Growth of the CuO like-plates.
 T. Jiang et al. / Applied Surface Science 311 (2014) 602–608
Fig. 10. (a) Absorption spectra of CuO nanosheets, (b) (˛h)2 vs. photon energy (h) plot for CuO nanosheets.
non-direct, forbidden direct or forbidden non-direct transitions.
The value of band gap of CuO nanoparticles is found to be 5.89 eV.
Because of the quantum size effect, the value of calculated band
gaps is higher than that of CuO with normal size. The smaller
particle size is, the lager surface area per unit volume will be.
As a consequence, surface atom has lower atomic interaction
and coordination number. Band gap energies increase due to the
increase of the highest valance band energy and decrease of the
lowest unoccupied conduction band energy.
3.4. Photocatalytic test of CuO nanosheets
In this experiment, using CuO nanosheets as catalyst and
methylene blue solution as target pollutants to simulate organic
wastewater, catalytic properties of CuO nanosheets to degrade
methylene blue under the irradiation of UV can be measured. Fig. 11
shows the result of the photo-degradation rate of methyl blue. From
the curve, it is obvious that the photo-degradation rate with CuO
nanocrystal is higher than that of copper oxide with general size.
When the time reaches 180 min, the photo-degradation rate of CuO
nanocrystal is up to 91.9%, almost two times than that of CuO whose
photo-degradation rate is just about 56.2%. 92.1% as the maximum
value of photo-degradation rate with CuO nanomaterial occurs at
the time of 210 min. Therefore, it is concluded that CuO nanosheets
possess good photocatalytic properties compared to CuO powder.
[10] Y.L. Liu, L. Lei, J.C. Li, C.X. Pan, From copper nanocrystalline to one-dimensional
Fig. 11. The photo-degradation rate of CuO nanosheets and CuO powder.
607
4. Conclusions
In summary, well-crystalline CuO nanosheets were synthesized
at low-temperature in large quantity via hydrothermal method.
The morphology with flower-like, plume-like, spindle-like and
size of CuO nanoparticles can be tuned by adjusting the reaction
parameters including reactant concentration, precipitant, reaction
temperature and reaction time. By detailed structural and optical
characterizations, it is confirmed that the synthesized nanocrystals
are monoclinic phase in high purity and possessing good opti-
cal properties. Moreover, a growth mechanism was proposed to
explain the formation of CuO nanoplates by the hydrothermal
method with Ostwald-ripening mechanism. The optical band gap
calculated of nanosheets is found about 5.89 eV. What’s more, its
photo-degradation rate of methylene blue can reach 92.1% which
is almost two times than that of CuO powder.
Acknowledgments
This work was supported by the National Natural Science Foun-
dation of China (21203170, 41102025). The financial support was
gratefully appreciated.
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