Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Short communication

One-pot low-temperature sonochemical synthesis of CuO

nanostructures and their electrochemical properties
Da-Sol Kim a,1, Jae-Chan Kim a,1, Byung-Kook Kim b, Dong-Wan Kim a,n
a
School of Civil, Environmental and Architectural Engineering, Korea University, Seoul, 136-713 Republic of Korea
b
High-Temperature Energy Materials Research Center, Korea Institute of Science and Technology, Seoul, 136-791 Republic of Korea

art ic l e i nf o a b s t r a c t

Article history: We report a low-temperature sonochemical method for the synthesis of CuO nanostructure. CuO na-
Received 17 August 2016 nowires and ellipsoidal CuO nanostructures were fabricated using 20 kHz ultrasonic irradiation. The
Received in revised form ultrasonic irradiation led to the efficient precipitation of crystalline CuO nanoparticles at 10 °C without
2 September 2016
additional dehydration or heat treatment. The formation mechanism of the CuO nanostructures was
Accepted 6 September 2016
investigated by X-ray diffraction, field emission scanning electron microscopy, and transmission electron
microscopy with respect to the exposure time and amount of surfactant. The optimized CuO nano-
Keywords: particles (SW-CTAB1) have an ideal one-dimensional CuO nanostructure with a high Brunauer-Emmett-
A. Powders: chemical preparation Teller surface area of 62.15 m2 g
1. Furthermore, the SW-CTAB1 electrodes exhibited a good lithium
B. Electron microscopy
activity.
B. X-ray methods
& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
D. Transition metal oxides
E. Batteries

1. Introduction which prevents nuclear growth and secondary nucleation. Com-

pared to hydrothermal and precipitation processes, the sono-
CuO is a typical p-type transition metal oxide semiconductor chemical method was proven to be a promising technique for
with a bandgap range of 1.8 eV. It is a promising candidate for preparing nanomaterials with various structures at relatively low
catalysis, photoelectrochemistry, solar-energy transformation, and temperature. Low frequency ultrasound irradiation causes acoustic
biosensor applications because of its abundance, low cost, che- cavitation, which can provide extreme temperature and pressure.
mical stability, non-toxicity, and easy production [1]. Of these This high energy can generate highly reactive radicals (H, OH,
applications, significant efforts have been devoted to study the O2
, and HO2) from water molecules, and these radicals fabri-
applicability of CuO in lithium-ion batteries because it can attain a cate metal oxide nanostructures within a short time [6]. Azadeh
much higher reversible capacity than commercial graphite-based et al. reported that nanocrystalline transition metal oxide (Co3O4
electrodes through conversion reactions (CuO þ2e
þ2Li þ 2Cu and Mn3O4) powders can be prepared by sonication at ambient
° þLi2O) and a low reaction potential (  1.5 V). Despite the high temperature of 25 °C, and Dengsong et al. reported polycrystalline
storage capacity of the conversion reaction, it would not be suffi- CeO2 nanorods synthesized by ultrasonication at ambient tem-
cient for practical applications because of the volume expansion perature [7,8]. However, none of these experiments is without
associated with sustainable cycling. heat treatment. Thus, it is still unclear whether the phase forma-
To improve the cycling performance limitation, transition metal tion/transformation was actually due to the heat treatment. Ad-
oxides have been fabricated by designing nanostructures [2]. Na- ditional studies are needed to prepare nanomaterials without any
nostructured materials have outstanding features, such as high thermal treatment.
surface area, narrow size distribution, and high surface reactivity. In this work, we describe a fast, green, and facile ultrasonic
It has been reported that the CuO nanowires, nanorods, and na- irradiation route to synthesize CuO nanostructures by the hydro-
nofibers provide enhanced electrochemical performances [3–5]. lysis of a copper acetate monohydrate solution at low temperature
Among lots of synthetic processes for nanostructures, the so- of 10 °C. The formation mechanism of the CuO nanostructures was
nochemical method provides a high dispersibility of nanoparticles, investigated by controlling the reaction time of the ultrasonic ir-
radiation. The cetyltrimethylammonium bromide (CTAB) was ad-
n ded as a surfactant for morphological control. The electrochemical
Corresponding author.
E-mail address: [email protected] (D.-W. Kim). properties of the CuO nanostructures were characterized by cyclic
1
These authors contributed equally to this article. voltammetry and galvanostatic cycling tests for lithium-ion

http://dx.doi.org/10.1016/j.ceramint.2016.09.044
0272-8842/& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i
2 D.-S. Kim et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎

battery applications. ethanol and dried for a day by a freeze-drying process. Finally, the
products were obtained and labeled as SW-nm (n ¼the reaction
time). For comparison, additional CuO powders were synthesized
2. Experimental procedure using the same experimental procedure but without the ultrasonic
irradiation (Stirr-nm). We were obtained CuO nanorods by ad-
Cu(CH3COO)2  H2O (0.55 g, Sigma-Aldrich) was dissolved in justing different CTAB amounts (0.5 g, 1 g, and 3 g), which was
175 mL of deionized water and 75 mL of ethanol for 5 min. Then, prepared according to the method described above. The system
the 20 kHz ultrasonic waves were directly irradiated into the so- was irradiated by 20 kHz ultrasonic waves at an output power of
lution by a high intensity ultrasonic probe (VC750, Sonics & Ma- 49% at 10 °C for 60 min. The resulting materials were named SW-
terials, USA), and 8 mL of aqueous NaOH (1 M) was simultaneously CTABm.
dropped into the solution at a rate of 1 mL min
1. The reaction The morphology and crystal structure of the prepared CuO
temperature was maintained at 10 °C. Afterward, the dark colloid products were characterized by field emission scanning electron
was washed several times with distilled water and absolute microscopy (FE-SEM, Quanta 250 FEG, Hitachi, Japan), high-

Fig. 1. (a) XRD patterns of Stirr-30m and SW-30m. High- and low-magnification SEM images of (b, c) Stirr-30m and (d, e) SW-30m.

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i
 D.-S. Kim et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎ 3

resolution transmission electron microscopy (HRTEM, Tecnai G2 crystals without any pores on the surface of the particles (Fig. 1c).
F30ST, FEI Co., USA), and X-ray diffraction (XRD, SmartLab, Rigaku, Fig. 1d and e show the morphologies of SW-30m. The SW-30m
Japan). The Brunauer-Emmett-Teller surface area of the CuO pro- particles have a uniform 3D ellipsoidal-shape with an average
ducts was determined (BET, ASAP2020, Micromeritics, USA). The length of 600 nm and a thickness of tens of nanometers. According
electrochemical performance of the CuO electrode was measured to the high-magnification images in Fig. 1e, the ellipsoidal shape of
in a voltage range of 0.01–3 V vs. Li þ /Li using an automatic battery the SW-30m particles had a rough surface, and the ellipsoidal CuO
cycler (WBCS 3000, WonATech, Korea). The CuO electrodes were particles were formed by assembled small nanoparticles as
prepared using a slurry consisting of 70 wt% active materials, building blocks. From these results, the ultrasonic irradiation in-
15 wt% super P, and 15 wt% PVDF-HFP binder on a copper foil. The duced the precipitation of CuO nanoparticles, and they were self-
galvanostatic half-cells were assembled with lithium metal and assembled to an ellipsoidal shape.
1 M LiPF6 EC/DMC electrolyte. Cyclic voltammetry tests were also To clarify the formation process of the ellipsoidal CuO structure,
performed at a slow scan rate of 0.1 mV s
1 in a potential range of SW-10m and 30m were prepared at different ultrasonic irradiation
0.01–3 V. times. The crystal structure and morphologies were demonstrated
by XRD, FE-SEM, and TEM analyses with respect to the reaction
time variation. Fig. 2a shows the XRD patterns of SW-10m and
3. Results and discussion 30m. In the case of SW-10m, most peaks corresponded to the
monoclinic CuO phase, but weak peaks were also detected at 16.7°
To determine the effect of the ultrasonic irradiation, the crystal and 23.8°, which were matched to the orthorhombic Cu(OH)2
structure change was examined by comparing the samples pre- (020) and (021) planes, respectively. The XRD results show that Cu
pared with and without the sonication process. The XRD patterns (OH)2 was not fully converted into crystalline CuO because of the
of Stirr-30m and SW-30m are shown in Fig. 1a. The peaks at 16.7°, lack of reaction time. However, the XRD pattern of SW-30m re-
23.8°, 34.2°, 39.7°, and 53.5° in the XRD pattern of Stirr-30m cor- vealed a high-purity CuO phase without Cu(OH)2 or other im-
respond to orthorhombic Cu(OH)2 (JCPDS card No. 13-0420). The purities as the results in Fig. 1.
XRD peaks of Stirr-30m were broad and weak because the low To better understand the sonochemical reaction, the
reaction temperature of 10 °C led to a low degree of crystallinity morphologies of SW-10 and 30m were identified using the FE-SEM
for Cu(OH)2. The peaks at 32.5°, 35.4°, 35.5°, 38.7°, 38.9°, 48.7°, and and TEM images in Fig. 2. Fig. 2c and d show the FE-SEM and TEM
53.5° for SW-30m were well indexed to the monoclinic CuO (110), images of SW-10m. The FE-SEM image of SW-10m presented two
(002), (
111), (111), (200), (
202), and (020) lattice planes, re- morphologies of bundles and small particles. Bundles are up to
spectively (JCPDS card No. 80-1268). The crystal structure of SW- 5 mm long and several hundred nanometers thick. More accurate
30m was clearly the CuO phase without any Cu(OH)2 or other information can be obtained from the TEM image in Fig. 2d. The
impurities despite its synthesis at a low temperature, 10 °C. The bundles were composed of nanorods with an average diameter of
following sonochemical phenomena could be a possible explana- 15 nm. The nanorods originated from the precipitation of Cu(OH)2.
tion for the formation of the CuO phase at low temperature. First, They aggregated with each other and formed nanorod-bundles to
the sonochemical irradiation occurred in a high energy collapsing reduce their high surface energy [4]. The selected area electron
bubble. Then, the collapsing bubble generated a reactive radical. diffraction (SAED) pattern or d-spacing information of nanorod-
These reactive radicals played a role in the formation of CuO at low bundles cannot be measured by HR-TEM because they are rapidly
heat energies. damaged by the high-energy electron beam. Similar morphologies
Many researchers have already reported on CuO nanostructures for Cu(OH)2 were previously reported [9,10,13]. Fig. 2c and d show
using various approaches [9–11]. It is hard to form the CuO phase that the particles have an average diameter of 10–100 nm. As the
at 10 °C because the dehydration and oxidation reactions usually reaction proceeds, the nanorod-bundles decomposed to irregular
occur over 60 °C. However, the crystalline CuO can be synthesized particles, and Cu(OH)2 transformed to the CuO phase through a
at 10 °C with our sonochemical approach. The formation me- dehydration reaction. However, the nanorod-bundles were not
chanism of CuO can be expressed as follows: fully converted to particles because 10 min was not sufficient time.
When the sonication time was prolonged to 30 min, numerous
Cu2 þ þ 2OH
-Cu(OH)2 (1) nanoparticles were built up to the secondary ellipsoidal archi-
tecture. Fig. 2e shows TEM images of SW-30m particles, which had
Cu(OH)2 þ2OH
-[Cu(OH)4]2
(2) an ellipsoidal shape and were 250 nm and 500 nm in width and
length, respectively. The CuO nanoparticles have average dia-
[Cu(OH)4]2
-CuO þ 2OH
þH2O (3) meters of 8.2 nm with a high crystallinity. From a thermodynamic
point of view, small nanoparticles tend to decrease the total sur-
2þ
In the reaction system, [Cu(H2O)6] ions formed as a light blue face area to maintain the lowest surface energy, thus neighboring
solution when the Cu salt and water mixed together. When the nanoparticles were agglomerated [14]. The sonication time is a key
NaOH solution was dropped into this solution, copper hydroxide parameter to control the morphological evolution and the for-
precipitated because of the reaction between the Cu ion and OH mation of the ellipsoidal shape. For the formation of CuO phase, an
radical. With the excess of hydroxyl ions, the color of the sus- ultrasound exposure time of over 30 min is required. Fig. 2f and
pension changed to deep blue, which showed that Cu(OH)2 and the inset show a high-resolution TEM image and SAED patterns of
[Cu(OH)4]2
were formed. During decomposition in the highly SW-30m. The SEAD patterns of SW-30m revealed ring patterns
basic media, [Cu(OH)4]2
ions initially coordinated with the CuO that indicate polycrystalline materials. Each ring was well indexed
primary nanoparticles that were formed under incessant ultra- to the CuO (110), (002), (111), (202), and (220) planes. This result
sonic irradiation [12]. matched the XRD results in Fig. 2a.
The morphologies of Stirr-30m and SW-30m were observed by Based on our TEM results, we suggest a possible growth me-
FE-SEM images to examine the microstructure change caused by chanism for ellipsoidal CuO as in the schematic illustration in
ultrasonic irradiation. As shown in Fig. 1b, the low magnification Fig. 2b. In the initial stage, the formed Cu(OH)2 nanorod-bundles
image of Stirr-30m revealed irregular shaped particles with a large consisted of parallel nanorods that aligned by oriented assembly.
size variation from a few nanometers to over ten micrometers. The Primary CuO particles were generated from the Cu(OH)2 bundles.
stirring process at low temperature precipitated large and bulk The coexistence of CuO particles and Cu(OH)2 nanorods indicated

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i
4 D.-S. Kim et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎

Fig. 2. (a) XRD patterns of the synthesized samples at different ultrasonic exposure times of 10 min and 30 min (SW-10m and SW-30m, respectively). (b) Schematic il-
lustration of the morphology evolution steps for the CuO nanostructures. (c) FE-SEM and (d) TEM images of SW-10m. (e) TEM and (f) HR-TEM images of SW-30m and SAED
pattern of ellipsoidal CuO (inset in (f)).

that the formation of CuO is supported by the dissolution of the Cu of the so-called “oriented attachment.” Penn et al. reported that
(OH)2 nanorod-bundles [9]. The primary CuO particles were in- anisotropic growth occurred along [010] because of the lowest
terconnected to adjacent particles in the next step so that they density of Cu atoms on the (010) plane based on their theoretical
were agglomerated into an ellipsoidal shape by an ultrasonic ir- study. Based on additional TEM images and SAED patterns of SW-
radiation route. This process is related to the proposed mechanism 30m (Fig. S1), it is also confirmed that the preferential growth

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i
 D.-S. Kim et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎ 5

Fig. 3. FE-SEM images of (a) SW-CTAB0.5, (b) SW-CTAB1, and (c) SW-CTAB3. (d) Nitrogen adsorption/desorption curves of the SW-CTAB samples. (e) XRD patterns and HR-
TEM image of SW-CTAB1.

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i
6 D.-S. Kim et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎

orientation of SW-30m is along [010]. This formation mechanism monoclinic CuO, respectively (Fig. 3e). SW-CTAB1 has a unique
is commonly followed by oriented attachment [15,16]. mixed structure of crystalline CuO and the amorphous phase. The
A morphological evolution was conducted with an extended nanowire growth mechanism is not clear. We believe that the
amount of CTAB. Fig. 3a–c show the FE-SEM images of SW- CTAB effect the nanocrystals to adhere each other following a
CTAB0.5, 1, and 3, respectively. There were many ellipsoidal preferential direction driven by the low surface energy [20].
structures and a small number of nanorods. The ellipsoidal shapes For the confirmation of the Li-activity of the CuO nanos-
were 320 nm in average length, which was smaller than the tructure, the electrochemical performance of the SW-CTAB1
morphologies for SW-30m. The FE-SEM images in Fig. 3b and c electrodes was characterized by cyclic voltammetry (CV) and gal-
indicate that CuO nanowires were synthesized instead of ellip- vanostatic discharge-charge measurements in Fig. 4. The CV was
soidal shapes in accordance with the surfactant increase. When 1 g measured between 0.01 and 3 V at a scan rate of 0.1 mV s
1. The
of CTAB was used, CuO nanowires with diameters of 5 nm were five cathodic peaks in the first cycle were observed near 1.98, 1.3,
formed and intertwined with a few ellipsoidal shapes (Fig. 2b). 1.18, 0.75, and 0.58 V (Fig. 4a). This multistep reaction corresponds
Fig. 3c exhibits the morphology of SW-CTAB3. An excessive to reaction of CuO with lithium, which is the reduction of CuO to
amount of surfactant (3 g CTAB) provided short nanorods or na- metallic Cu. The peaks at 1.18 and 0.58 V disappeared after the
noparticle-shaped CuO. Relative to 1 g of CTAB, 0.5 g of CTAB could second cycle, which was caused by an irreversible reaction, such as
not inhibit the ellipsoidal-shaped growth, and 3 g of CTAB sup- the formation of a solid-electrolyte interface (SEI) layer [21,22].
pressed the growth of nanowires to become shorter rods or During the anodic process in Fig. 4a, two oxidation peaks were
particles. observed at 1.5 and 2.5 V, which indicates that Li ions were ex-
For the pore characteristic, N2 adsorption/desorption mea- tracted from CuO electrodes [3]. In the subsequent cycles, the
surements were conducted to SW-CTABm samples. As shown in peaks maintained their position and intensity, suggesting the re-
Fig. 3d, the nitrogen adsorption-desorption isotherms can be as- versibility of the SW-CTAB1 electrodes.
signed as type III. The BET surface areas of SW-CTAB0.5, CTAB1, Galvanostatic cycling was performed in the voltage window of
and CTAB3 were 39.97, 62.15, and 69.41 m2 g
1, respectively 0.01–3.0 V at a current density of 67 mA g
1. Fig. 4b shows the
(Fig. 3d), which are higher than that for similar CuO materials first and second step charge-discharge of SW-CTAB1. The first
[13,17]. SW-CTAB0.5, CTAB1, and CTAB3 had total pore volumes of discharge of SW-CTAB1 was 1091 mA h g
1, and the irreversible
0.1968, 0.5381, and 0.3998 cm3 g
1, respectively. SW-CTAB1 had capacity of SW-CTAB1 reached 565 mA h g
1. The SW-CTAB1
the large BET surface area and total pore volume of SW-CTAB1 was electrodes exhibited high Li activity due to the advantage of the
the highest among CuO nanostructures. The CTAB can play a sig- one-dimensional nanostructure, such as a larger surface area and
nificant role in preventing aggregation by providing a stabilization effective electron conduction pathway [23]. The capacity retention
effect at the surface and anisotropic nanoparticle growth with a and low Coulombic efficiency need to be improved by further
high surface area [18,19]. Moreover, one dimensional nanos- research.
tructure of SW-CTAB1 can offer better electrochemical perfor-
mance because of its unique advantages such as large surface area
and efficient electrical pathways. 4. Conclusions
SW-CTAB1 was subjected to further crystal structure analyses
by XRD and HR-TEM. Fig. 3e shows the XRD pattern of SW-CTAB1. We successfully synthesized CuO ellipsoidal nanostructures
All peaks were well indexed to the monoclinic CuO phase, but the and CuO nanowires by a sonochemical method at a low tem-
crystallinity significantly decreased compared to SW-30m. This perature of 10 °C. The sonochemical reaction required enough
phenomenon was also confirmed by the HR-TEM image. The CuO energy to fully transform to the CuO phase (20 kHz of ultrasonic
nanowires were composed of nanoparticles that had a low crys- irradiation for more than 30 min). The ultrasonic irradiation led to
tallinity and were smaller than 5 nm. The lattice fringes of the the precipitation of CuO nanoparticles, and they self-assembled to
nanowires were measured to be 0.252 and 0.230 nm, which is in an ellipsoidal shape without heat treatment. Through the addition
good agreement with the (
111) and (111) planes of the of CTAB as a surfactant, the nanowires and ellipsoidal-shaped CuO

Fig. 4. (a) Cyclic voltammetry curves of the SW-CTAB1 electrodes at a rate of 0.1 mV s
1 and (b) galvanostatic charge-discharge curves of SW-CTAB1 electrodes at 0.1 C.
Electrochemical tests were performed between 0.01 and 3 V.

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i
 D.-S. Kim et al. / Ceramics International ∎ (∎∎∎∎) ∎∎∎–∎∎∎ 7

were fabricated following an oriented-attachment growth me- cycleability, J. Phys. Chem. C 116 (2012) 18087–18092.
chanism. The optimized amount of 1 g CTAB provided an ideal [6] T. Gao, Q. Li, T. Wang, Sonochemical synthesis, optical properties, and electrical
properties of core/shell-type ZnO nanorod/CdS nanoparticle composites,
one-dimensional nanostructure of CuO with a high BET surface Chem. Mater. 17 (2005) 887–892.
area of 62.15 m2 g
1. The electrochemical test using SW-CTAB1 [7] A. Askarinejad, A. Morsali, Direct ultrasonic-assisted synthesis of sphere-like
anodes presented a high Li activity with initial specific capacities nanocrystals of spinel Co3O4 and Mn3O4, Ultrason. Sonochem. 16 (2009)
of 1091 and 565 mA h g
1 for discharge and charge, respectively. 124–131.
[8] D. Zhang, H. Fu, L. Shi, C. Pan, Q. Li, Y. Chu, W. Yu, Synthesis of CeO2 nanorods
The sonochemical method can be expected to apply diverse metal via ultrasonication assisted by polyethylene glycol, Inorg. Chem. 46 (2007)
oxide nanostructures to large-scale productions because of its 2446–2451.
economic and environmental advantages. [9] C. Lu, L. Qi, J. Yang, D. Zhang, N. Wu, J. Ma, Simple template-free solution route
for the controlled synthesis of Cu(OH)2 and CuO nanostructures, J. Phys. Chem.
B 108 (2004) 17825–17831.
[10] J.Y. Xiang, J.P. Tu, L. Zhang, Y. Zhou, X.L. Wang, S.J. Shi, Self-assembled synthesis
Acknowledgment of hierarchical nanostructured CuO with various morphologies and their ap-
plication as anode for lithium ion batteries, J. Power Sources 195 (2010)
313–319.
This work was supported by the National Research Foundation [11] M. Vaseem, A. Umar, S.H. Kim, Y.B. Hahn, Low-temperature synthesis of
of Korea (NRF) Grant funded by the Ministry of Science, ICT, and flower-shaped CuO nanostructures by solution process: formation mechanism
Future Planning, South Korea (Nos. 2016R1A2B2012728 and and structural properties, J. Phys. Chem. C 112 (2008) 5729–5735.
[12] V.K. Patel, S. Bhattacharya, High-performance nanothermite composites based
2016M3A7B4909318) and by the institutional research program of on aloe-vera-directed CuO nanorods, ACS Appl. Mater. Interfaces 5 (2013)
the Korea Institute of Science and Technology, South Korea 13364–13374.
(2E26081-16-054). [13] L. Wang, K. Zhang, Z. Hu, W. Duan, F. Cheng, J. Chen, Porous CuO nanowires as
the anode of rechargeable Na-ion batteries, Nano Res. 7 (2014) 199–208.
[14] J. Huang, X. Xu, C. Gu, M. Yang, M. Yang, J. Liu, Large-scale synthesis of hy-
drated tungsten oxide 3D architectures by a simple chemical solution route
Appendix A. Supporting information and their gas-sensing properties, J. Mater. Chem. 21 (2011) 13283–13289.
[15] R.L. Penn, J.F. Banfield, Imperfect oriented attachment: dislocation generation
in defect-free nanocrystals, Science 281 (1998) 969–971.
Supplementary data associated with this article can be found in [16] J.F. Banfield, S.A. Welch, H. Zhang, T.T. Ebert, R.L. Penn, Aggregation-based
the online version at doi:10.1016/j.ceramint.2016.09.044. crystal growth and microstructure development in natural iron oxyhydroxide
biomineralization products, Science 289 (2000) 751–754.
[17] G. Xiao, P. Gao, L. Wang, Y. Chen, Y. Wang, G. Zhang, Ultrasonochemical-as-
sisted synthesis of CuO nanorods with high hydrogen storage ability, J. Na-
References nomater. (2011) 1–6.
[18] J. Zhu, H. Chen, H. Liu, X. Yang, L. Lu, X. Wang, Needle-shaped nanocrystalline
[1] L. Wang, H. Gong, C. Wang, D. Wang, K. Tang, Y. Qian, Facile synthesis of novel CuO prepared by liquid hydrolysis of Cu(OAc)2, Mater. Sci. Eng. A-Struct. Mater.
tunable highly porous CuO nanorods for high rate lithium battery anodes with Prop. Microstruct. Process. 384 (2004) 172–176.
realized long cycle life and high reversible capacity, Nanoscale 4 (2012) [19] E.J.H. Lee, C. Ribeiro, E. Longo, E.R. Leite, Oriented attachment: an effective
6850–6855. mechanism in the formation of anisotropic nanocrystals, J. Phys. Chem. B 109
[2] P.L. Taberna, S. Mitra, P. Poizot, P. Simon, J.M. Tarascon, High rate capabilities (2005) 20842–20846.
Fe3O4-based Cu nano-architectured electrodes for lithium-ion battery appli- [20] C. Pan, D. Zhang, L. Shi, CTAB assisted hydrothermal synthesis, controlled
cations, Nat. Mater. 5 (2006) 567–573. conversion and CO oxidation properties of CeO2 nanoplates, nanotubes, and
[3] F. Wang, W. Tao, M. Zhao, M. Xu, S. Yang, Z. Sun, L. Wang, X. Song, Controlled nanorods, J. Solid State Chem. 181 (2008) 1298–1306.
synthesis of uniform ultrafine CuO nanowires as anode material for lithium- [21] K.S. Park, S.D. Seo, Y.H. Jin, S.H. Lee, H.W. Shim, D.H. Lee, D.W. Kim, Synthesis of
ion batteries, J. Alloy. Compd. 509 (2011) 9798–9803. cuprous oxide nanocomposite electrodes by room-temperature chemical
[4] X.P. Gao, J.L. Bao, G.L. Pan, H.Y. Zhu, P.X. Huang, F. Wu, D.Y. Song, Preparation partial reduction, Dalton Trans. 40 (2011) 9498–9503.
and electrochemical performance of polycrystalline and single crystalline CuO [22] F. Cao, X.H. Xia, G.X. Pan, J. Chen, Y.J. Zhang, Construction of carbon nanoflakes
nanorods as anode materials for Li ion battery, J. Phys. Chem. B 108 (2004) shell on CuO nanowires core as enhanced core/shell arrays anode of lithium
5547–5551. ion batteries, Electrochim. Acta 178 (2015) 574–579.
[5] R. Sahay, P.S. Kumar, V. Aravindan, J. Sundaramurthy, W.C. Ling, S. [23] X.H. Huang, J.P. Tu, X.H. Xia, X.L. Wang, J.Y. Xiang, L. Zhang, Y. Zhou, Mor-
G. Mhaisalkar, S. Ramakrishna, S. Madhavi, High aspect ratio electrospun CuO phology effect on the electrochemical performance of NiO films as anodes for
nanofibers as anode material for lithium-ion batteries with superior lithium ion batteries, J. Power Sources 188 (2009) 588–591.

Please cite this article as: D.-S. Kim, et al., One-pot low-temperature sonochemical synthesis of CuO nanostructures and their
electrochemical properties, Ceramics International (2016), http://dx.doi.org/10.1016/j.ceramint.2016.09.044i