Nano Energy (2015) 11, 719–727

Available online at www.sciencedirect.com

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

RAPID COMMUNICATION

High output piezoelectric nanocomposite

generators composed of oriented BaTiO3
NPs@PVDF
Yingli Zhaoa,1, Qingliang Liaoa,1, Guangjie Zhanga, Zheng Zhanga,
Qijie Lianga, Xinqin Liaob, Yue Zhanga,b,n

a
State Key Laboratory for Advanced Metals and Materials, School of Materials Science and Engineering,
University of Science and Technology Beijing, Beijing 100083, China
b
Key Laboratory of New Energy Materials and Technologies, University of Science and Technology Beijing,
Beijing 100083, China

Received 11 September 2014; received in revised form 11 November 2014; accepted 27 November 2014
Available online 8 December 2014

KEYWORDS Abstract
BaTiO3 NPs; Piezoelectric nanocomposites (p-NC) composed of piezoelectric nanoparticles (NPs) and flexible
PVDF; polymer have emerged as outstanding applications for flexible nanogenerators (NGs). In this
p-NC; article, we proposed a p-NC NG by combining the barium titanate nanoparticles (BaTiO3 NPs)
NGs with the poly-vinylidene fluoride (PVDF). By a facile and scalable solvent evaporation process,
the BaTiO3 NPs and PVDF composite (BaTiO3 NPs @ PVDF) films were fabricated. BaTiO3 NPs
dispersed uniformly in the PVDF matrix and formed an oriented structure without aggregations.
By using this special oriented BaTiO3 NPs @ PVDF composite film, the highest open-circuit
voltage reaches 150 V, which is one of the most outstanding output performance in the lead-
free piezoelectric field to date. The energy generated from the p-NC NG can light three light-
emitting diode (LED) bulbs instantaneously without any storage unit.
& 2014 Elsevier Ltd. All rights reserved.

n
Corresponding author at: State Key Laboratory for Advanced
Metals and Materials, School of Materials Science and Engineering,
University of Science and Technology Beijing, Beijing 100083,
China.
E-mail address: yuezhang@ustb.edu.cn (Y. Zhang).
1
These two authors contributed equally to this work.
Introduction
Harvesting energy from the moving objects has been considered
as a splendid approach to solve the energy problem. [1–3] Over
the past few years, numerous piezoelectric nanostructures have
been used to construct nanogenerators (NGs). Mechanical
energy can be scavenged and converted into electrical energy

http://dx.doi.org/10.1016/j.nanoen.2014.11.061
2211-2855/& 2014 Elsevier Ltd. All rights reserved.
720
by the NGs. During these piezoelectric NGs, ZnO was firstly used
to construct NG [4–6] and had been investigated extensively. [7–
9] Moreover, perovskite piezoelectric materials have a high
piezoelectric coefficient and are suitable for piezoelectric NGs.
[10–16] Served as a piezoelectric material, Barium titanate
(BaTiO3) has drawn significant attentions due to its strong
piezoelectric properties, simple and convenient preparation,
and low cost. However, being a traditional ceramic material,
BaTiO3 with poor flexibility is not well appropriate for the
applications of flexible devices.
In order to solve the fragile problems of the piezoelectric
NGs, piezoelectric nanocomposites (p-NC) composed of piezo-
electric NPs and flexible polymer have been developed and
have demonstrated outstanding piezoelectric properties
towards flexible and wearable applications. [17–20] In the
previous reports, Polydimethyl siloxane (PDMS) was widely
used as a matrix in the composite NGs. [21–23] However,
piezoelectric polymers are better candidates for p-NC NGs
owing to their remarkable flexibility and excellent mechanical
properties. [24–26] Polyvinylidene fluoride (PVDF) is a kind of
semicrystalline polymer with piezoelectric properties, which
has α, β, γ, δ and ε crystal forms. Among them, the β phase has
a high piezoelectric coefficient. [27–30] Since PDMS is too
viscous, NPs could not be well-dispersed in the PDMS.
Compared to the conventional PDMS, the PVDF solution has
low viscosity and the solvent can be easily evaporated, which
makes NPs incorporated into PVDF matrix more uniformly. In
addition, as a piezoelectric material, PVDF plays a part in
generating piezoelectric potentials. In the previous reports,
the composite of BaTiO3 NPs and PVDF exhibited good
dielectric properties. [31] The fibrous BaTiO3-reinforced PVDF
composite showed high flexibilities and could be applied in the
transducers. [32] Hemispherically aggregated BaTiO3 NPs and
P (VDF-HFP) composite demonstrated enhanced outputs in the
application of NGs [33].
In this article, a high-performance, flexible composite NG
was proposed based on the BaTiO3 NPs and PVDF (BaTiO3 NPs @
PVDF) composite film. This film combined the advantages of
BaTiO3 NPs with the virtues of PVDF. By a facile and scalable
solvent evaporation process, the BaTiO3 NPs @ PVDF composite
film was prepared. BaTiO3 NPs dispersed uniformly in the fiber-
like PVDF matrix and formed an oriented structure without
aggregations. The BaTiO3 NPs not only help to increase the
piezoelectric potential, but also reinforce the local stress of the
PVDF and induce larger deformation of the polymer compared
with the pure PVDF. As a result, the output of PVDF is enhanced.
The highest open-circuit voltage and short-circuit current
achieved were 150 V and 1500 nA respectively with the stress
of 10 Mpa. At last, the energy generated from the p-NC NG can
light three light-emitting diode (LED) bulbs successfully without
any storage units. The NG was made by lead-free materials,
which was satisfied with the environmental protection. The
proposed approach was simple, cost-effective, and applicable
to fabricate large-scale high-performance flexible NGs.
Experimental
Fabrication of BaTiO3 NPs @ PVDF composite film
0.3 g PVDF powders were dissolved in 3 ml 1-Methyl-2-
pyrrolidinone (NMP) by stirring at 45 1C for 12 h to obtain a
Y. Zhao et al.
uniform solution. Afterwards, 0.7 g BaTiO3 NPs powders were
added into the PVDF solution and dispersed by ultrasonic
stirring for 1 h at room temperature. The as-mixed suspension
was dropped onto a glass substrate and dried in a vacuum oven
at 60 1C for 1 h. After the vacuum drying process, a solid p-NC
film was formed on the glass substrate. Finally, the film was
peeled off from the glass substrate easily.
Construction of the NG
The p-NC film was cut into small pieces (1
1 cm2). Poly-
ethylene terephthalate (PET) films deposited with ITO were
covered onto the top and bottom surface of the film. The
conductive ITO-coated PET film was served as both electro-
des and package layers. In order to improve the output of
the NG, the poling process for NG was necessary. An electric
field of 2 kV was applied on the NG, and the electric field
was maintained for 8 h.
Characterization
The morphology and size of the BaTiO3 NPs and PVDF films
were characterized by the field-emission scanning electron
microscopy (FE-SEM, Quanta 3D FEG). The crystalline struc-
tures of BaTiO3 NPs and PVDF films were characterized by
X-ray diffractometer (TTRIII). The poled PVDF film was
scanned from 1600 cm  1 to 400 cm  1 with Fourier transform
infrared (FTIR) spectrophotometer in attenuated total reflec-
tance mode (ATR). The Raman spectrum of BaTiO3 NPs was
obtained by the Raman spectroscopy (JY-HR800) with an Ar +
laser source at room temperature. The open-circuit voltage
signals were gained by a digital oscilloscope (DS4052, RIGOL).
Connecting the p-NC device, digital oscilloscope and load cell
in series, the short-circuit current can be calculated by the
output voltage and extrinsic load resistance [34].
Results and discussions
The detailed fabrication procedure of the flexible p-NC NG is
shown in Figure 1a. BaTiO3 NPs are well-dispersed into NMP
solution of PVDF. The p-NC film can be obtained by a solvent
evaporation process on a glass substrate. The NG is con-
structed by sandwiching the p-NC film between two ITO-
coated PET films. Figure 1b shows the as-fabricated p-NC film
with the size of 1
1 cm2. Figure 1c shows a NG bended by
fingers, indicating that the device has good flexibility.
Figure 2a shows the SEM image of the BaTiO3 NPs, which
indicates that the diameter of BaTiO3 NPs is about 150 nm.
The Raman spectrum of the BaTiO3 NPs is shown in the inset of
Figure 2a. The sharp peak of spectrum in the range of 305 to
720 cm  1 is attributed to the A1 and E (longitudinal optical)
modes, which declares that the BaTiO3 NPs have high crystal-
linity with an excellent tetragonal phase. [35] Figure 2b shows
the X-Ray diffraction (XRD) pattern of BaTiO3 NPs. It can be
found that the BaTiO3 NPs have six diffraction peaks ((1 0 0),
(1 1 0), (1 1 1), (2 0 0), (2 1 0), (2 1 1)). Furthermore, the
double-peak profile at 45 1 indicates that BaTiO3 NPs are
well-crystallized with a tetragonal phase. Figure 2c shows the
XRD pattern of the unpoled PVDF film. It has two obvious
characteristic peaks, (0 2 0) and (1 1 0) at 18.81 and 20.21
respectively. The unpoled film is α phase of monoclinic system
High output piezoelectric nanocomposite generators composed of oriented BaTiO3 NPs@PVDF
Figure 1 (a) The detailed fabrication procedure of flexible p-NC NG. (b) Photograph of the p-NC film with dimension of 1 cm2.
(c) Photograph of the flexible p-NC NG.
which exhibits negligible piezoelectric properties. After pol-
ing, it is found out that these peaks decrease compared to the
unpoled PVDF. However, (1 1 0) peak at 20.61 demonstrates
that crystalline phase of the poled PVDF is β phase. The poled
PVDF film was also investigated by the FTIR spectrophot-
ometer. The characteristic absorption bands attributing to the
β phase at 840 cm  1(CH2 rocking) 1275 cm  1 (trans band) and
1430 cm  1(CH2 bending) are clearly distinguished. [19] The
NG is well poled, as similarly observed by XRD patterns. The
side-view SEM image of the BaTiO3 NPs @ PVDF composite film
is shown in Figure 2e. It is found that the oriented fiber array
structure is formed across the thickness of the p-NC film. In
addition, BaTiO3 NPs are dispersed along the PVDF fibers
uniformly. This fiber array structure is different from the
conventional structure reported previously. [36] The inset of
the Figure 2e is a low-magnification side-view SEM image of
the p-NC film. Based on the inset figure, the thickness of the
p-NC film is about 60 μm. The top-view SEM image in Figure 2f
shows that we get a compact p-NC film.
721
The generated outputs of the p-NC are measured when the
stress is applied and released on the p-NC NG repeatedly.
Figure 3a and b show the outputs in the forward connection.
When stress of 1 MPa is applied on the p-NC NG, the generated
short-circuit current and open-circuit voltage signals of the NG
reach up to 600 nA and 35 V respectively. The inset of the
Figure 3a shows a positive piezoelectric output is generated.
In order to prove that the signals are generated by the NG, the
output signals are measured under the reverse connection,
which are shown in Figure 3c and d. [37,38] As a result, an
opposite signal is generated. To exploit the contribution of
BaTiO3 NPs within the NG, the NG without BaTiO3 NPs was
measured under the same test conditions. Figure 3e and
Figure S2 show that the open-circuit voltage of pure PVDF
NG under stress of 1 MPa is 15 V and the generated short-
circuit current of the NG is about 180 nA. The outputs are
smaller than the outputs of p-NC NG. It works out that the
addition of BaTiO3 NPs improves the output of the NG greatly.
The poling process is important, so a comparative trial of the
722 Y. Zhao et al.

Figure 2 (a) SEM image of BaTiO3 NPs. Inset is the Raman spectrum pattern of the BaTiO3 NPs. (b) X-ray diffraction pattern of
BaTiO3 NPs. (c) X-ray diffraction pattern of the poled and unpoled PVDF film. (d) FTIR spectroscopy of the poled PVDF film. (e) Side-
view SEM image of the p-NC film, Inset is the low-magnification SEM image. (f) Top-view SEM image of a p-NC film.

p-NC NG without poling is indispensable. From the Figure 3f, it
turns out that the piezoelectric voltage of the unpoled p-NC
NG is 1.5 V, which is much smaller than the poled p-NC NG. It
proves that the poling process is an essential step for
enhancing the output performance of the p-NC NG.
The work mechanism of p-NC NG is depicted in Figure 4.
When the electrical field is applied on the p-NC film in
Figure 4a, the dipoles in BaTiO3 NPs tend to align along the
direction of the electrical field. At the same time, as for
PVDF, α phase will be transformed into piezoelectric β phase
through the rearrangement of F ions and H ions along the
carbon chains. Finally, the dipoles in BaTiO3 NPs and PVDF will
align in one direction along the electric-field. When the NG
suffers a compressive stress as shown in Figure 4c, the
mechanical stress can induce piezoelectric charges, which
results in a potential difference between the two electrodes.
In order to screen the piezoelectric potential in the p-NC film,
external free charges will move to and accumulate at the
electrodes, during which a positive signal can be detected.
When the stress is released, the piezoelectric potential
between the two sides of the NG disappears. The accumulated
charges will flow back in an opposite direction, generating an
negative electrical signal shown in Figure 4d [22].
Unlike previously reported p-NC NGs, the polymer matrix
here is PVDF. PVDF is not only functioned as a binder for
BaTiO3 NPs, but also plays a part in generating piezoelectric
High output piezoelectric nanocomposite generators composed of oriented BaTiO3 NPs@PVDF 723

Figure 3 (a) The short-circuit current generated from the p-NC NG under stress of 1 MPa in the forward connection. Inset shows the zoom
in data. (b) The open-circuit voltage generated from the p-NC NG in the forward connection. Inset shows the short-circuit current and open-
circuit voltage are measured under the forward connection mode. (c) The generated short-circuit current of the p-NC NG in reverse
connection. Inset indicates the zoom in data. (d) The open-circuit voltage signal generated from the p-NC NG in reverse connection. Inset
shows measured output potential and current under the reverse connection mode. (e) The open-circuit voltage signals generated from the
pure PVDF film NG. (f) The open-circuit voltage signals generated from the unpoled p-NC NG. Inset is the zoom in data.

potential. Under the same poling electric field, BaTiO3 and
PVDF will produce the dipole moments with the same
direction. As a result, the piezoelectric output will be the
sum of two materials. As reported before, it is proved that
uniformly dispersing of the BaTiO3 NPs in the polymer is the
key factor for improving the piezoelectric output. [22,23]
BaTiO3 NPs tend to be localized at the bottom surface
owning to aggregations in the PDMS matrix. However, PVDF
solution is beneficial for dispersing BaTiO3 NPs into solution
due to its low viscosity. Figure 2e shows that the BaTiO3 NPs
are homogeneously dispersed in the PVDF matrix. Thus, the
piezoelectric output of the p-NC NG will be maximized.
Moreover, the addition of the BaTiO3 NPs promotes the
piezoelectric potential of the PVDF. The total induced
electric potential of the p-NC film between two electrodes
can be expressed as follows:
V ¼ Q =C ¼ d 33 TL=ε ð1Þ
Q ¼ d 33 TA ð2Þ
724 Y. Zhao et al.

Figure 4 (a) The schematic diagram of poling process. (b) After poling, the dipoles in BaTiO3 NPs and PVDF will align in one
direction along the electric-field. (c) When the stress is applied on the p-NC NG, a positive potential is generated. (d)When the stress
is released, the accumulated electrons flow back in the opposite direction.

Figure 5 Schematic diagram of the vertical stress applied on (a) p-NC NG. (b) pure PVDF NG.

C ¼ εA=L ð3Þ
Q, C, d33 and ε represent the induced charge, the capaci-
tance in parallel, the piezoelectric coefficient, and the
dielectric coefficient of PVDF. T is the vertically stress
distributed on the film. L is the film thickness. A is the
top surface area of film. It is obvious that the generated
electric potential is decided by the verti stress T, the
piezoelectric coefficient d33, the thickness of the film L
and dielectric coefficient ε. The vertical stress T depends on
elastic constant E and the deformation y along the vertical
direction of the p-NC film. [20] As a result, the deformation-
induced electric potential can be expressed as:
V ¼ d 33 EyL=ε ð4Þ
Figure 6 The output potential recorded during the stability
Figure 5 shows a schematic diagram of the p-NC NG and test for over 2000 cycling times. The inset shows the magnified
pure PVDF NG under vertical stress. We regard both of the output signals.
High output piezoelectric nanocomposite generators composed of oriented BaTiO3 NPs@PVDF
Figure 7 Output performance of the NGs under stress of 10 MPa.
(a) The short-circuit current generated from the p-NC NG. (b) The
open-circuit voltage generated from the p-NC NG. (c) Three LED
bulbs lighted by the power source generated from the p-NC NG.
The inset shows a schematic diagram of connection circuit.
film as closely packed PVDF nanofibers. In the case of p-NC
film, PVDF fibers are separated into many segments by
BaTiO3 NPs. The NPs can act as stress concentration points
when the film is subjected to a compression stress. [39,40]
Therefore, the local deformations of the PVDF segments will
be dramatically increased and larger piezoelectric potential
will be generated according to formula (4). However, there
is no deformation enhancement in the pure PVDF NG. As a
result, the generated piezoelectric output of p-NC NG will
be larger than pure PVDF NG.
Long-term stability test is conducted to confirm the mechan-
ical endurance of the NGs. Measurements of more than 2000
725
cycling times with the stress of 1 Mpa are demonstrated in
Figure 6. The magnified output signal in the inset shows that
the open-circuit voltage is about 35 V. The generated potential
does not appear to change significantly after 2000 cycles, which
indicates that the device is very stable.
Figure 7a and b show the output performances when the
stress applied on the NG is 10 MPa, which is compatible with
the stress generated from human walking. The open-circuit
voltage and short-circuit current generated are 150 V and
1500 nA respectively, which is one of the most outstanding
output performance to date. [10,17,23] The Figure 7c shows
that the high piezoelectric output from the NG can drive
three LED bulbs without any storage units. This proves that
the BaTiO3 NPs @ PVDF composite NGs we proposed here
would be valuable in powering commercial electronics.
Conclusions
In summary, we have demonstrated a high output NG using
BaTiO3 NPs @ PVDF composite film. BaTiO3 NPs were
dispersed homogeneously in the PVDF matrix and formed a
uniform and oriented structure. Compared to pure PVDF
based NG, the addition of BaTiO3 NPs into PVDF matrix could
increase the output potential from 15 V to 35 V. The key
reasons for high output power generation can be attributed
to the well-dispersion of BaTiO3 NPs and the stress concen-
tration of PVDF resulted from the addition of NPs. The NG
shows the significant stability under repeated mechanical
stress. The short-circuit current and open-circuit voltage
are as high as 1500 nA and 150 V under a stress of 10 MPa,
respectively, which is large enough to light three LED bulbs
directly. Due to the advantages of low cost, simple fabrica-
tion and excellent output of the BaTiO3 NPs @ PVDF
composite NG, it would have outstanding applications in
energy harvesting and realizing self-powered electronics.
Acknowledgments
This work was supported by the National Major Research
Program of China (2013CB932602), the Major Project of
International Cooperation and Exchanges (2012DFA50990),
Program for New Century Excellent Talents in University
(NCET-12-0777), the Program of Introducing Talents of Dis-
cipline to Universities (B14003), NSFC (51172022, 51232001,
51372023, 51372020), the Fundamental Research Funds for
the Central Universities (FRF-SD-12-032A).
Appendix A. Supporting information
Supplementary data associated with this article can be
found in the online version at http://dx.doi.org/10.1016/
j.nanoen.2014.11.061.
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Yingli Zhao received her B.S degree in
School of Physics and Technology Materials
Science and Engineering from Hebei Univer-
sity in 2012. She is currently a master
student in Materials Science and Engineer-
ing, University of Science & Technology
Beijing. Her recent research concen-
trates on the piezoelectric composite
nanogenerators.
Qingliang Liao received his Ph.D. degree
from University of Science and Technology
Beijing (USTB) in 2009. Now he is an associ-
ate professor at School of materials science
and Engineering in USTB. His scientific
interests focus on synthesis and character-
ization of one-dimensional nanomaterials,
design and application of functional
nanodevices.
Guangjie Zhang received his B.S. degree
from University of Science and Technology
Beijing (USTB) in 2011 and now is a Ph.D.
student at School of materials science and
Engineering in USTB. His research interests
focus on synthesis of nanomaterials for high
efficient energy conversion devices.
Zheng Zhang is currently a Ph.D. candidate
at the School of Material Science and Engi-
neering, University of Science and Technol-
ogy Beijing. His research interests focus on
ZnO based electromechanical nanodevice,
nanogenerator, and piezotronic effect.
Qijie Liang received his B.S. degree in
Materials Science and Engineering from
Anhui Jianzhu University in 2012. He is a
Ph.D. candidate at physics and chemistry of
material, University of Science & Technol-
ogy Beijing. His research interests include
nanogenerators and self-powered systems.
High output piezoelectric nanocomposite generators composed of oriented BaTiO3 NPs@PVDF 727

Xinqin Liao received his B.S. degree from behavior. He has published more than 270 papers in peer reviewed
Fuzhou University in 2012 and now is a Ph.D. scientific journals and 8 monograph, and held 25 patents in his
student at School of materials science and research area. His publication has been cited more than 1000 times
Engineering in University of Science and by peers.
Technology Beijing. His research interests
in clued synthesis of nano materials for
electromechanical nano device, and piezo-
tronic effect.

Yue Zhang is a professor of Material Physics

and vice-president of University of Science
and Technology Beijing, China. He has been
awarded the financial support for outstand-
ing young scientist foundation of China and
selected as the chief scientist of Major
National Scientific Research Projects. His
research focuses on functional nanomater-
ials and nano-devices, new energy materi-
als, and nanoscale failure and service