J Mater Sci: Mater Electron (2014) 25:974–980

DOI 10.1007/s10854-013-1674-4

Octahedral cuprous oxide synthesized by hydrothermal method

in ethanolamine/distilled water mixed solution
Shufang Wu • Tianmo Liu • Wen Zeng • Shixiu Cao •

Kangguan Pan • Shiyang Li • Yongsong Yan •

Jiejun He • Bin Miao • Xianghe Peng

Received: 13 August 2013 / Accepted: 17 October 2013 / Published online: 3 January 2014
Ó Springer Science+Business Media New York 2013

Abstract Octahedral cuprous oxide has been synthesized nature, it has attracted a great attention to the researchers
by a simple hydrothermal method using copper sulphate and been widely applied in photocatalysis [7], sensors [8],
and sodium hydroxide as raw materials in ethanol amine/ negative electrode materials for lithium-ion batteries [9],
distilled water mixed solution. The synthesized cuprous electrochromism [10], and antibacterials [11]. The funda-
oxide powders were characterized by X-ray diffraction mental properties of micro/nanostructured semiconductors
(XRD) and field emission scanning electron microscopy. are found to be dependent greatly on surface chemistry, their
XRD pattern exhibited that the nanocrystalline nature with architectures, shape, geometry, morphology, and hierar-
cubic structure for the synthesized nanostructures. Analysis chical structures [12]. Therefore, great efforts have been
results reveal that pH value of solution plays an important devoted to artificially control the morphology of cuprous
role in the formation of octahedron shape for cuprous oxide micro/nanocrystals in the past several years [13–28].
oxide. A probable formation mechanism of octahedral So far, cuprous oxide crystals with different shapes have
cuprous oxide is also proposed. been synthesized, such as cube, truncated cubes, cubocata-
hedra, truncated octahedron, octahedron, short hexapods,
extended hexapods [29], dodecahedra [30], nanocages [7],
1 Introduction nanowires [31], nanorods [32], nanotube [32], nanospheres
[33], hierarchical [34] and hollow structures [35].
Cuprous oxide is a p-type semiconductor with a small band Recently, the preparations of different polyhedron
gap of about 2 eV, which makes it a promising material in morphology cuprous oxide have been reported by several
the application of solar energy conversion [1–3]. Due to its researchers. Liang et al. [30] reported that oleic acid, as a
unique optical, electrical, and magnetic properties [4–6] face selective adsorption additive, can subtly determine the
while low cost and simple preparation along with nontoxic morphology of the final products. Various concentrations
of oleic acid can result in a series of morphologies of
cuprous oxide, such as cube, octahedron, {110} truncated
S. Wu  T. Liu (&)  S. Cao  K. Pan  S. Li  Y. Yan  J. He  octahedron and microhombic dodecahedron with {110}
B. Miao
surfaces. Zhang et al. [36] synthesized porous cuprous
College of Materials Science and Engineering, Chongqing
University, Chongqing 400044, People’s Republic of China oxide octahedron with a mean diameter of 1 lm with high
e-mail: [email protected] yield via a hydrothermal reduction at low temperature of
120 °C. They indicated that both citric acid and PVP
T. Liu  W. Zeng
played a crucial role in the growth of octahedral cuprous
National Engineering Research Center for Magnesium Alloys,
Chongqing University, Chongqing 400044, People’s Republic of oxide. Heng et al. [37] reported that Zn-doped cuprous
China oxide polyhedrons with various crystal morphologies, from
50-facet and 26-facet to 8-facet, were synthesized via a
X. Peng
mild, low-temperature process based on the hydrothermal
Department of Engineering Mechanics, State Key Laboratory of
Coal Mine Disaster Dynamics and Control, Chongqing method. Zhang et al. [38] reported that octahedral cuprous
University, Chongqing 400044, People’s Republic of China oxide could be controlled by adding different kinds of

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surfactants such as SDBS, SDS, CTAB, BTM, CPC, PEG, purchased from Chengdu Kelong chemical reagent plant
PVP and Tween 80 into solution through a wet reduction and distilled water was used throughout.
process. Ma and Zhu [39] successfully prepared cuprous
oxide polyhedrons by a hydrothermal method at 200 °C for 2.2 Sample preparation
2 h using Cu(CH3COO)2H2O, glycine (C2H5NO2) and
NaOH. They found that the morphology of cuprous oxide In this work, mixed liquid of distilled water and organic
was significantly influenced by the concentration of gly- solvent ethanolamine were designed as solvent of sodium
cine. When the quantity of glycine was decreased to hydroxide solution and copper sulphate solution. The vol-
0.120 g, individual needles were formed as a major mor- ume of distilled water and organic solvent ethanolamine in
phology. Only a small number of assembly of needles were both sodium hydroxide solution and copper sulphate
observed along with. When the quantity of glycine was solution is 54.9 and 0.1 ml, respectively. Octahedral
further decreased to 0.105 g, a mixture of morphologies cuprous oxide were synthesized by the following process:
including polyhedrons, and an assembly of needles was firstly, 0.45 g white copper sulphate powder was dissolved
observed. When the quantity of glycine was decreased to in 59.5 ml distilled water, then the solution was stirred by
0.090 g, the polyhedrons were formed as a major mor- fine glass rod until all the copper sulphate powder dis-
phology. Al-Ghamdi et al. [40] reported that a novel and solved and the solution became sky blue, followed by the
efficient synthesis of cuprous oxide nano-octahedron was addition of 0.1 ml ethanolamine, next the solution was
successfully prepared via a green chemical approach uti- stirred by magnetic stirring reactor for 30 min. The colour
lized a microwave hydrothermal route at low growth of the copper sulphate solution becomes light blue. Thus
temperature without the presence of any surfactant. 50 mmol/l copper sulphate solution was prepared. Parall-
However, most of the methods mentioned above utilize elly 0.23 g sodium hydroxide block was added to 54.9 ml
surfactant to control the morphology of cuprous oxide, and distilled water, then the solution was also stirred by the fine
one method employed microwave irradiation. In this work, we glass rod, less than 10 min later all the sodium hydroxide
reported the synthesis of octahedral cuprous oxide via the block dissolves quickly and the solution became transpar-
reduction of copper sulphate by hydrazine hydrate ent, followed by the addition of 0.1 ml organic solvent
(N2H4H2O) under alkaline condition by means of employing ethanol amine, then the solution was also stirred by the
SDS as {111} crystallographic induction surfactant by magnetic stirring reactor for 30 min. Hence 100 mmol/l
hydrothermal method and its characterization by X-ray dif- sodium hydroxide solution was prepared. Secondly, put the
fraction (XRD). The morphology of octahedral cuprous oxide sodium hydroxide solution into the copper sulphate solu-
nanostructures was observed by field emission scanning tion slowly. The mixed liquid of sodium hydroxide solution
electron microscopy (FESEM). Furthermore, the probable and copper sulphate solution almost remained sky blue, and
formation mechanism was discussed. In this paper, the main floc deposition produced. The mixture was stirred by the
purpose is to investigate the synthesis process of octahedral magnetic stirring reactor for 30 min until all sodium
cuprous oxide and formation process mechanism of octahe- hydroxide interacted with copper sulphate and cupric
dral cuprous oxide in alkaline solution under hydrothermal hydroxide precipitated completely. Thirdly, 0.1007 g SDS
condition. Compared with the previous literature on formation powder was added to the solution, and 6.875 ml 100 mmol/
mechanism of octahedral cuprous oxide, we come up with l hydrazine hydrate (N2H4H2O) was added dropwise to the
perspective decrease of {111} surface energy promoted the solution. The cupric hydroxide was reduced gradually and
growth of {111} crystallographic plane and finally obtained the solution became slight brick red form sky blue. This
cuprous oxide octahedron, this is the novelty of the paper. reduction reaction lased for 5 h at room temperature under
stirring condition by magnetic stirring reactor. The pH
value of the solution is about 10 when the reduction
2 Experimental reaction completed. Fourthly, 110 ml the above mixture
was transferred into two 60 ml autoclaves. The autoclaves
2.1 Chemicals were sealed, shook right and left, and maintained at 120 °C
for 24 h in heater furnace, then cooled to room temperature
All of the chemical reagents in this experiment were naturally. The solution after hydrothermal reaction was put
directly used without further purification. Analytical grade into 5 ml plastic centrifugation tubes and the samples were
sodium hydroxide, distilled water and ethanolamine were centrifuged at 6,000 rpm for 3 min (TG high speed cen-
purchased from chemical reagent plant, Chongqing Chu- trifuge) and the top solution was withdrawn. The precipi-
andong Chemical (Group) Co., Ltd. Copper sulphate tates were centrifuged three times by distilled water and
(CuSO4) and hydrazine hydrate (N2H4H2O) were ethanol respectively to remove the unreacted chemicals.

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observed belonging to impurities indicating that all the

products were phase-pure.
In addition to the general confirmation of cuprous oxide
phase, the XRD patterns also provide information on
crystal orientations. From the XRD pattern of Fig. 1, the
h111i reflection of the samples obtained is comparatively
strong, which is probably due to the orientation of the
nano-crystallines.

3.2 The morphology of product and probable formation

mechanism

The morphology of the prepared cuprous oxide sample was

analyzed by the FESEM, as shown in Fig. 2. Figure 2a
shows a panoramic view of the as prepared product, the
Fig. 1 XRD pattern of octahedral cuprous oxide synthesized at
120 °C for 24 h
lower magnification image in Fig. 2a indicates that the
product consists of a large amount of particles with narrow
size distribution. While the higher magnification image in
And the slight brick red powder was dried at vacuum oven Fig. 2b clearly reveals that the particles are composed of
at 60 °C for 8 h. regular polyhedra. Further magnified images (Fig. 2c, d)
indicate that these polyhedral particles are perfect octahe-
2.3 Instrumentation dra, The measured average edge length of these octahedral
is about 2.63–3.20 lm, and the octahedron is bounded by
X-ray diffraction test was conducted on a Rigaku D/Max- eight perfect {111} triangle planes.
3C X-ray diffractometer with Cu Ka radiation The formation mechanisms of the octahedral cuprous
(k = 0.1542 nm) with accelerating voltage of 40 kV and a oxide were explained in a different perspective under dif-
current of 25 mA at room temperature. A scan rate of ferent preparation conditions. According to references, As
0.02°/s was applied to record the powder patterns for 2h Liang [30] reported that the concentration of oleic acid
between 20° and 75°. Field emission scanning electron molecules can affect the shapes of cuprous oxide crystals
microscopy (FESEM) images was obtained by the FEI because of their preferentially selective adsorption on the
Nova 400 FEG-SEM. {100}, {111} and {110} surfaces. As reported, the shapes
of the cubic crystals, such as cuprous oxide, are determined
by the growth ratio R of the growth rate along the h100i
3 Results and discussion directions to the h111i directions [41]. When the amount of
oleic acid is 1 ml, firstly it interacts with the {100} planes
3.1 The structure of cuprous oxide of cuprous oxide crystal and then preferential adsorption on
the {100} face confines crystal growth along h100i direc-
The structure and chemical composition of the sample were tions, therefore microcubic cuprous oxide form, with a
confirmed by an XRD. The typical XRD patterns of the corresponding R of 0.58. As the concentration of oleic acid
samples synthesized via hydrothermal method at 120 °C for increases, not only is the {100} surface completely cov-
24 h are shown in Fig. 1. In the XRD pattern, there are ered, but also the {111} face begins to adsorb oleic acid.
eight peaks with 2h values of 29.42°, 36.28°, 42.24°, 52.36°, Continuous adsorption of oleic acid on the {111} faces
61.24°, 69.70°, and 73.38° corresponding to h110i; confines the growth of {111} planes. When the amount of
h111i; h200i; h211i; h220i; h310i, and h311i crystal oleic acid reaches 1.5 ml, {111} truncated cubes appear.
planes of pure cuprous oxide, respectively. These results are The amount of oleic acid continues to increase, and
in good agreement with the cuprous oxide powder obtained cuprous oxide irregular micro-octahedra are obtained at
from the International Center of Diffraction Data Card 2 ml of oleic acid. When the value of R increases from 0.58
reflections (JCPDS, 05–667). The peaks located at 2h values to 1.73, micro-octahedral cuprous oxide are obtained at the
of 20–75° can be indexed to the characteristic diffractions of oleic acid amount of 2.5 ml. When the concentration of
cubic phase cuprous oxide (a = b = c = 4.27 Å). The peak oleic acid continues to increase, both {100} and {111}
intensities and widths clearly indicated that the sample was crystal planes show saturated surface coverage, and oleic
highly crystalline in nature. Compared with the standard acid begins to be adsorbed on the {110} crystal planes,
diffraction patterns, there are no other characteristic peaks resulting in the formation of {110} truncated octahedra

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(a) (b)

2 µm
10 µ m

(c) (d)

1µm 1 µm

Fig. 2 FESEM of octahedral cuprous oxide prepared at 120 °C for 24 h in ethanol amine/distilled water mixed solution

with the exposure of {110} and {111} surfaces. As the rate along the h111i direction and enhance the growth rate
oleic acid concentration increases, the area of {110} sur- along the h100i direction. So in their present experiment,
face continuously increases, and {111} faces gradually the most stable (111) faces preferentially appear and the
disappear. Finally, the rhombic dodecahedra with complete perfect cuprous oxide octahedra are obtained. Al-Ghamdi
{110} coverage are obtained. Based on the above experi- et al. [40] analyzed that based on the crystal growth con-
mental results and analysis, there should be a strong cept, the morphology and size of crystals is mostly gov-
interaction between the surface of cuprous oxide particles erned by the relative growth rate (i.e. kinetic control) of
and oleic acid molecules, although the nature of selectivity different crystal faces and coordination’s during their for-
of oleic acid with different crystal planes is still to be mation. For cuprous oxide monocrystal, when face (100)
studied further. Zhang et al. [36] found that citric acid grows relatively fast, it tends to octahedron-like morphol-
played a crucial role on the porous cuprous oxide octahedra ogy. It is known that particles usually have the specific
growth. They think the citric acid was used as an assistant shape because a single-crystal particle has to be enclosed
vesicant, reacting with acetate and releasing many gases by crystallographic facets that have lower surface energy.
with the temperature increasing, resulting in the porous Therefore, it is believed that the formation of cuprous
structure. In the reaction mixture, PVP was another oxide octahedrons during the microwave hydrothermal
important factor in determining the morphology of the final process proceeds in a way with much faster growth rate
product. With the assistance of PVP, these cuprous oxide along (100) than along (111) due to the highest surface
nanoparticles were able to grow into octahedral-shaped energy and area of the (100) surfaces, thereof different
structures. It could be believed that the surfactant PVP was shapes of cuprous oxide crystal can be obtained via con-
to kinetically control the growth rates of various faces. trolling the Cu? atoms which determines the growth of
When PVP is introduced, it is believed that the selective face (111) and face (100). Xu et al. [42] reported that
interaction between PVP and various crystallographic octahedral cuprous oxide crystals with tunable edge length
planes of cuprous oxide could greatly reduce the growth were synthesized by reducing copper hydroxide with

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(a) (b) (c) (d) (e)

300 nm 3 µm 1 µm 200 nm 500 nm

Fig. 3 FESEM results showing different morphologies of cuprous oxide prepared at 120 °C under different hydrothermal time in ethanol amine/
distilled water mixed solution

hydrazine without using any surfactant. Systematic exper- experienced a shape evolution from cubooctahedron
iments were carried out to investigate the factors which (Fig. 3c) to vertex-truncated octahedrons (Fig. 3d) and at
impact on the morphology and size of the products. The reaction time 24 h, vertex-truncated octahedrons finally
molar ratio of the reagents (NH3:Cu2?and OH-:Cu2?) became high symmetry octahedrons (Fig. 3e), corre-
determined the morphology and size of the corresponding sponding to a progressive shrinkage of {100} and
products via affecting the coordination between NH3:Cu2?. enlargement of {111} as illustrated by Fig. 3a–e.
It is demonstrated that the ratio of growth rate along h111i In our work, we reported the synthesis of octahedron
versus h100i was varied by adjusting the molar ration of cuprous oxide synthesized by hydrothermal method in eth-
NH3 to Cu2?, thus cuprous oxide crystals with different anol amine/distilled water mixed solution. It is reported that
morphologies such as spheres, cube-like, and octahedra a series of shape evolutions of cuprous oxide particles from
were obtained. the species such as cubic crystals to eight-pod particles have
It is believed that the reduction in surface energy is the been synthesized via a kinetically controlled process by
primary driving force for simple particle growth, the fur- adjusting pH of the solution [44]. When the cuprous oxide
ther reduction in surface energy due to the minimization of particles sample was prepared at pH 6.5, all the particles are
high surface energy faces will drive the morphology evo- well monodispersed and have a regular cubic shape. When
lution. Recent studies showed that the selective adsorption pH value of the solution was increased to 6.7, the mor-
of molecules and ions in solution on different crystal faces phology of the product sustained to be cubic. It reveals there
will also make the nanoparticles grow into various shapes are some pinholes on its surface. When the pH of the solu-
by controlling the growth rates along different crystal tion is adjusted to 7.5, most of cuprous oxide particles are
directions [43]. In our experiments, the octahedral cuprous still cube-shaped, but a few of them have tendency of
oxide bound by {111} surfaces were formed owing to the transforming into four-horn shaped particles. Almost each
effect of OH- ion decreasing the surface energy of {111} panel has pinhole, and the pinholes become bigger than
crystal plane. cuprous oxide particles synthesized at pH 6.7, few of them
On purpose to explore the formation for cuprous oxide even take up the whole panel. With increase in pH of the
octahedron, the whole process was carried out at different solution to about 8.0, the cube-shaped ones are replaced by
reaction times as 4, 8, 12 and 24 h at 120 °C. The mor- four-horn-shaped ones. It is clearly shown that the four horn
phologies of cuprous oxide under different hydrothermal shaped particles are three dimensional eight-pod particles,
time evolved from cube through truncated cube, cubooc- and that these eight-pod particles are incompletely grown of
tahendron, truncated octahedron and finally to octahedron. cuprous oxide cube-shaped ones. Here, we think that pH
The broad views of the different shaped cuprous oxide are value of solution played an important role in the formation
shown in Fig. 3. Under 4 h conditions, cube-shaped parti- of octahedron shape cuprous oxide.
cles, the thermodynamically stable form of the cuprite It has previously reported that the preferential adsorp-
oxide were observed in the products (Fig. 3a), with edge tion of SDS on {111} facets of cuprous oxide crystals can
length of about 860 nm, the exposed surfaces of the cubes be utilized to obtain octahedral crystal shapes. In this work
are made of six {100} facets. When the reaction time was we use SDS to induce the growth of {111} facets. From the
increased to 8 h, {111}-corner-truncated cubes (Fig. 3b) morphology shown in Fig. 3a, we analyzed that cuprous
were produced, eight triangles were cut in each vertices of oxide tends to form cubes initially due to the orientational
the cubes. With the hydrothermal time further increasing, crystallization mechanism. Copper sulphate could be dis-
the {111} triangle continue to grow, and {100} began to solved in water and forms a uniform ionic solution. When
shrink, two {111} intersected at one point on the edge of sodium hydroxide is added in the solution, the Cu2? ions
the cube (Fig. 3c), this product is called cubooctahedron. reacts with OH- and forms blue insoluble cupric hydroxide
As the reaction time increases to 12 h, the products precipitate. While cupric hydroxide suspension reacts with

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order of surface energies. The fastest crystal growth will

occur in the direction perpendicular to the face with the
highest surface energy. This results in the elimination of
higher energy surfaces while the lower energy surfaces
increase in area. This preferential adsorption lowers the
surface energy of the bound plane and hinders the crystal
growth perpendicular to the plane, resulting in a change in
the final morphology.
In this work the pH value of the solution is about 10, after
the sample was heated and the pH value was measured about
8.5. The decrease in pH was assumed to be because of the
consumption OH- ions during the reaction process.
Regarding the crystal growth, it is believed that the reduc-
tion of surface energy is the primary impetus for the mor-
phology evolution. The crystal growth rate perpendicular to
Fig. 4 The unit cell of cuprous oxide a plane is proportional to its surface energy. For cuprite
structured Cu2O, each ‘O’ atom is surrounded by a tetra-
hedron of ‘Cu’ atom and each ‘Cu’ atom, has two ‘O’
hydrazine hydrate, cupric hydroxide will be reduced into neighboring atoms as illustrated by its unit cell model
reddish cuprous oxide nanoparticles. The formation pro- (Fig. 4). From the crystal structure of cuprite oxide, it can be
cess of Cu2O particle composes the following two con- seen that three copper atoms distributed on {111} crystal
secutive reactions: plane, the three copper atoms have a positive charge.
CuSO4 þ 2NaOH ! CuðOHÞ2 þNa2 SO4 ð1Þ As to our experiments, according to the growth mech-
anism theory mentioned above, we speculate that abundant
4 CuðOHÞ2 þN2 H4 ! 2Cu2 O þ 6H2 O þ N2 ð2Þ
OH- ions could be preferentially absorbed on {111}
From the chemical reaction above, the cupric hydroxide crystallographic plane of cuprous oxide. Studies showed
can be considered as a precursor for the formation of that the selective adsorption of molecules and ions in
cuprous oxide in this work. solution on different crystal faces will also make the
It is well-known that the shape of a crystal is determined nanoparticles grow into various shapes by controlling the
by the crystallographic planes that form the surface. In growth rates along different crystal directions. So,
general, one specific shape of a crystal forms either in order absorption of OH- ions on {111} crystallographic plane of
to minimize the surface energy or because of the kinetics of cuprous oxide nanocrystals will lower the surface energy of
growth [45]. The fast growing faces have smaller surface the {111} crystallographic plane and hinder the crystal
areas, and the slow growing faces therefore dominate the growth perpendicular to {111} crystallographic plane, slow
morphology of the crystal. It is commonly accepted that the the growth rates along the h111i direction, and promote the
geometrical shape of cubic phase crystal is mainly deter- growth of {111} facet, thus resulting in the final mor-
mined by the ratio (R) of the growth rate along the h100i phology. From morphology of the cuprous oxide octahedron
versus h111i direction [46]. When R = 1.73, it is favorable at different hydrothermal time we can deduce that the for-
to form octahedron or tetrahedron bounded by {111} fac- mation process of cuprous oxide octahedron may be divided
ets. When inorganic crystals are formed under equilibrium into five stages as following: stage one: the production of
conditions then crystal habit is determined by the relative cuprous oxide cube (Fig. 5a). Cubic cuprous oxide initially

Fig. 5 Schematic illustration of probable formation process of octahedral cuprous oxide

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980 J Mater Sci: Mater Electron (2014) 25:974–980

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