Applied Surface Science 392 (2017) 10551061

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Applied Surface Science

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Full Length Article

sintesis sangat tipis tellurium serpih tekstil untuk
Synthesis of ultra-thin tellurium
fleksible
nanoakes on textiles for
dapatdipakai
tinggi hasil/kualitas nanogenerator
high-performance exible and wearable nanogenerators
Wen He a,1 , Huynh Van Ngoc a,1 , Yong Teng Qian a , Jae Seok Hwang a , Ya Ping Yan a ,
Hongsoo Choi b , Dae Joon Kang a,
a
Department of Physics and Interdisciplinary Course of Physics and Chemistry, Sungkyunkwan University, 2066, Seobu-ro, Jangan-gu, Suwon 16419,
Gyeoggi-do, Republic of Korea
b
Department of Robotics Engineering, Daegu Gyeongbuk Institute of Science and Technology (DGIST), 711-873, Daegu, Republic of Korea

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

Article history: We report that ultra-thin tellurium (Te) nanoakes were successfully grown on a sample of a gold-
Received 3 June 2016 coated textile, which then was used as an active piezoelectric material. An output voltage of 4 V and a
Received in revised form current of 300 nA were obtained from the bending test under a driving frequency of 10 Hz. To test the
12 September 2016
practical applications, Te nanoake nanogenerator (TFNG) device was attached to the subjects arm, and
Accepted 30 September 2016
Available online 30 September 2016
mechanical energy was converted to electrical energy by means of periodic arm-bending motions. The
optimized open-circuit voltage and short-circuit current density of approximately 125 V and 17 A/cm2 ,
respectively, were observed when a TFNG device underwent a compression test with a compressive force
Keywords:
Textile of 8 N and driving frequency of 10 Hz. This high-power generation enabled the instantaneous powering
Tellurium nanoake of 10 green light-emitting diodes that shone without any assistance from an external power source.
Bending 2016 Elsevier B.V. All rights reserved.
Compressing
Nanogenerators

1. Introduction based devices to fabricate self-powered systems that have potential

Nanogenerators (NGs) that harvest mechanical and human-
motion-based energy have garnered huge technological interest in
accordance with the growing popularity of portable, smart elec-
tronics [1]. Researchers have developed approaches based upon
a variety of phenomena, including electromagnetic elds [2], the
piezoelectric effect [36], the electrostatic effect [7,8], and the tri-
boelectric effect [912], for transforming mechanical motion to
electrical energy. Piezoelectric and triboelectric NG devices have
been investigated intensively to develop self-powered electron-
ics with high output power. However, fabricating triboelectric NGs
remains complicated and time-consuming, considering the large
scale of the devices [13]. Piezoelectricity is considered to offer the
best option for self-charging NG devices, owing to the ability of
these materials to directly convert mechanical energy into electri-
cal energy and to the mechanisms reliance on small components.
Piezoelectric NGs can be integrated effectively with nanomaterial-
Corresponding author.
E-mail address: djkang@skku.edu (D.J. Kang).
1
These authors contributed equally to this work.
applications in robotic sensory skins and biomedical devices [14].
However, the energy-harvesting efciency of traditional NGs is
greatly impeded due to their high cost, fragility, and low output
power [13]. Thus, innovative approaches are needed to develop
exible and small wearable electronic devices with high output
performance.
One approach to solving the issue of energy harvesting is to
develop textile-based NGs, which have gained tremendous atten-
tion for their wide degree of freedom in being formed into shapes
with exible, stretchable, and even wearable characteristics. Flexi-
ble, textile-based piezoelectric NG devices can provide continuous
and effective generation of electrical energy from human motions,
such as compression and bending, and from external sources of
wasted mechanical energy [1517]. To gain high output power, it is
vital to choose the appropriate piezoelectric materials. Over the last
two decades, CdS [18], GaN [19], NaNbO3 [20], PbZrx Ti1-X O3 [21],
BaTiO3 [2224], and ZnO [25,26] have been considered as highly
efcient piezoelectric materials.
Tellurium (Te), with a high work function (4.95 eV), has the
highest strain piezoelectric coefcient among all existing piezo-
electric materials [27]. As a new class of piezoelectric material, Te
has shown a strong potential for use as the active material in NGs.

http://dx.doi.org/10.1016/j.apsusc.2016.09.157
0169-4332/ 2016 Elsevier B.V. All rights reserved.
1056 W. He et al. / Applied Surface Science 392 (2017) 10551061

Fig. 1. The schematic diagrams of the fabrication process and general characterization of the TFNG device. (a) Schematic of the process for fabricating the TFNG devices. (b)
Optical images depicting the TFNG devices in different states: at, folded, and rolled. (c) SEM image of the Te nanoakes synthesized by the low hydrothermal method; the
inset represents a magnied view. (d) XRD patterns of the Te nanoakes as synthesized. (e) TEM image of Te NFs and (f) HRTEM image showing individual NF with [110]
growth direction, Inset shows the SAED pattern of Te NF.

Lee et al. reported that a laterally assembled Te-nanowire-based 2. Experimental section

NG offered a high power density and showed both excellent long-
term stability and bending frequency stability [27]. However, the
output voltage and current of Te-nanowire-based NGs are still too
low for uses in practical applications.
We herein, report for the rst time a new type of fully exible
and wearable Te-nanoake-based NG with high output power. Te
nanoakes (NFs) with plate-like morphologies were grown verti-
cally on a piece of textile through a low-temperature, hydrothermal
method. Novel, wearable NGs were exploited to achieve high
output power through periodic bending and compressive tests.
Arm-bending was also carried out to conrm the devices prac-
tical applicability for converting vibrational energy sources from
human activity into electrical energy. The excellent performance
of these fabricated, wearable devices during compressive testing
was veried by powering 10 LEDs without using any energy storage
systems.
2.1. Fabrication of Te nanoakes
All chemicals used in the experiments were purchased from the
Sigma Aldrich Co., Korea. They were analytical grade and required
no further purication. In a typical synthesis of Te nanoakes, one
piece of gold-coated textile was cleaned three times by sonica-
tion using isopropanol and ethanol. A transparent solution was
formed by adding 2 ml of NH3 H2 O and 0.145 g of ethylenedi-
aminetetraacetic acid disodium salt (EDTA-Na2 ) to 25 ml of distilled
water and stirring for 5 min. In another glass bottle, 50 mg of NaOH,
80 mg of TeO2 , and 36.445 mg of cetyltrimethylammonium bro-
mide (CTAB) were dissolved into 20 ml of distilled water and stirred
continuously for 5 min. These two solutions were labelled as A and
B, respectively. Then solution B was slowly added to solution A. The
nal mixture was adjusted to a pH of 9 by using nitric acid (60%).
 W. He et al. / Applied Surface Science 392 (2017) 10551061 1057

Fig. 2. Electrical measurements of the TFNG device during bending test. (a) Optical images of the TFNG device in its original, bending, and release stages. (b) Measured
output voltage and current of the TFNG device during repeated bending and unbending motions. The device exhibited a maximum peak open-circuit voltage of 3.0 V (i) and
a short-circuit current of 290 nA (ii), while the power was 0.87 mW.

Fig. 3. Electrical measurements of the TFNG device attached to a human arm. (a) Optical images of the TFNG device attached to a human arm in original, folding, and releasing
states. (b) Open-circuit voltage during periodic bending and straightening of the human arm. The arm was bent to an angle of 60 . (c) Closed-circuit currents produced by
the TFNG device during periodic bending and straightening of the human arm.

Finally, 2 ml of hydrazine hydrate was added into the above mix-
ture and stirred continuously until the solution became pink. The
gold-coated textile was then immersed and held in the solution.
The encapsulated glass bottle was permitted to undergo reactions
in a dry oven at 50 C for 4.5 h. Finally, the gold-coated textile was
washed several times with distilled water and ethanol and dried at
60 C in a vacuum oven.
2.2. Fabrication of the piezoelectric nanogenerator
Before assembling the TFNG device, polydimethylsiloxane
(PDMS) solutions were prepared using a one-pot sol-gel process in
which tetraethyl orthosilicate was used as an inorganic precursor
and hydroxyl-terminated PDMS was used as an organic modier at
a weight-ratio of 10:1. Then, the uid mixture was dip-coated onto
1058 W. He et al. / Applied Surface Science 392 (2017) 10551061

Fig. 4. Electrical measurements of the TFNG device during compressive test. (a) Optical images of the TFNG device in its original, compressive, and release stages. (b) The
output voltage (i) and current (ii) of the TFNG device during repeated compressive motions under the driving frequency of 10 Hz and various compressive force. (c) The
measured output voltage (i) and current (ii) of the TFNG device during repeated compressive motions under the compressive force of 10 Hz and various driving frequencies.
(d) (i) Plot of power density versus force under the driving frequency of 10 Hz, (ii) Plot of power density versus driving frequencies under the compressive force of 8 N.

the Te-NF-based Au/textile and cured at 80 C for 2 h in an oven. The 2.3. Characterization
Au layer on the textile was used as a bottom electrode, while the
top electrode was prepared by depositing a 50-nm-thick Au layer The morphology of the Te NFs was characterized using eld
onto the surface of the PDMS. emission scanning electron microscopy (JEOL JSM-7401F). An
 W. He et al. / Applied Surface Science 392 (2017) 10551061
assessment of the X-ray diffraction (XRD) spectrum (D8 FOCUS
2200V, Bruker AXS) was carried out to study the crystal phase.
The crystalline structure of the ZnO NFs was examined via high-
resolution transmission electron microscopy (HRTEM, FE-TEM
JEM2100F). A compressing tester was used to apply programmed
forces to the TFNGs. A Lecroy WaveRunner 6100a oscilloscope and
a low-noise current amplier (MODEL SR570) were used to detect
the output signals generated from the TFNG.
3. Results and discussion
The schematic diagrams in Fig. 1(a) present the synthetic pro-
cess for fabricating a exible TFNG device; detailed information
about this process is described in the section on methods. The
TFNG device has a sandwich-like structure with PDMS-coated Te
NFs in the middle, while the Au/textile and the Au layer served as
both bottom and top electrodes, respectively. The photographs in
Fig. 1(b) illustrate three different bending states: at, folded, and
rolled. This record of performance conrms that the TFNG devices,
as prepared, are highly exible and even stretchable. The scan-
ning electron microscopy (SEM) images in Fig. 1(c) and the insets
show that 20-nm-thick Te NFs are well grown on textiles. The crys-
talline structure of the Te NFs is characterized by XRD (Fig. 1(d)).
The peaks in the diffractogram are in good agreement with those
of hexagonal Te (JCPDS le No. 36-1452) [28]. Before starting mea-
surements, the TFNG device was placed on the machined holder and
the system was ensured to be grounded to avoid external electro-
static charges. We examined the crystalline nature of the Te NFs by
using high-resolution transmission electron microscopy (HRTEM,
FE-TEM JEM2100F) as shown in Fig. 1e. The selected area electron
diffraction (SAED) and HRTEM images of individual Te nanoake
are shown in Fig. 1f. The SAED pattern clearly indicates that the Te
NFs are of single crystalline and predominantly grown along the
[110] crystallographic direction. The regular and visible fringes in
HRTEM are clearly seen from the individual Te NF. The distance
between neighboring fringes was measured to be 0.44 nm, which
is consistent with the (110) plane of hexagonal Te.
3.1. Bending test
We measured the generated outputs of the TFNG device during
periodic bending and unbending motions. Fig. 2(a) shows the opti-
cal images of the TFNG device of size 1 4 cm2 in different bending
stages: original, bending, and release. In order to apply an identical
strain along the whole device, the TFNG device was covered with
a supporting substrate (PET). The embedded device was xed at
the bending stage and bent along with the supporting substrate.
Under identical strains, our TFNG device reached an open-circuit
voltage and a closed-circuit current of 3 V and 290 nA, respectively
(Fig. 2(b)). For practical applications, we demonstrated that elec-
trical energy can be obtained through human movement. Since the
motivation for constructing our device is to make exible and wear-
able NGs, the device was attached to a human arm as shown in
Fig. 3(a). The supporting substrate (PET) used here also prevented
the device from making direct contact with human skin, which
could have caused unexpected electrical noise [1]. The output volt-
age (Fig. 3(b)) and current (Fig. 3(c)) produced by the repeated
bending and straightening actions of the human arm reached up
to 2.5 V and 650 nA, respectively.
3.2. Compressing test
In order to obtain the maximum power density during the peri-
odic compression test, the output voltage and current of the TFNG
(1 1 cm2 ) were measured under the same frequency (10 Hz) but
different compressive forces (F = 2, 4, 6, 8, 10, 12 N). As shown in
1059
Fig. 5. LEDs lighting with the electricity generated form the TFNG device. (a) Image
showing 10 commercial LEDs incorporated into the circuit. (b) Photograph showing
the 10 LEDs lit up by the electrical energy generated by the tested TFNG device.
Fig. 4(a), the measured devices corresponded to the three states:
the original, bending, and release states. The output voltage and
the current increased with an increase in F, while maintaining the
driving frequency at 10 Hz (Fig. 4(b)). However, the performance
began to decrease as the compressive force grew larger than 8 N;
this is ascribed to the fact that a strong compressive force will
eventually break the Te NF. To further optimize the performance
of the devices, a series of comparative experiments was also car-
ried out using the same compressive force (F = 8 N) but various
driving frequencies (f = 4, 5, 6, 7, 8, 10 Hz). As the data presented
by Fig. 4(c) indicate, the output voltage gradually increased from
72.7 V to 125.3 V, while the output current density increased from
8.23 A/cm2 to 16.5 A/cm2 . The output power density (P) of the
TFNG device was calculated as P = UI, where U and I is the output
Voltage and current, respectively. As shown in Fig. 4(d), the maxi-
mum output power density of 2.07 mW/cm2 could be achieved for
the TFNG device under a compressive force of 8 N and a working
frequency of 10 Hz.
To show the potential utilization of our energy harvesting tech-
nology, we demonstrated that the high output of a TFNG device can
be used to light up at least 10 LEDs (Fig. 5(a) and (b)). Video S(1)
provides a video clip of the LEDs powered by the electricity gen-
erated from the TFNG device. This excellent performance suggests
the high potential of the TFNG device for portable self-powered
electronics. Furthermore, we didnt notice any appreciable change
in the output power of TFNG device after keeping it in vacuum for
three months as shown in Fig. S(1).
The power-generating mechanisms of the TFNG device during
bending and compression tests are depicted in the schematic dia-
grams in Fig. 6(a) and (b), respectively. The fundamental working
mechanism for the TFNG device is similar to that of a ZnO-nanoake
nanogenerator (NFNG) [29,30]. The NFs that have plate-like mor-
phologies are expected to play vital roles both in power generation
and the devices performance. The piezoelectric potential can be
generated in the NFs when an external mechanical force is applied
to the TFNG device through bending or compressing motions.
To balance the piezoelectric potentials, the free electrons in the
circuit ow from the bottom electrode to the top electrode, result-
ing in an electric pulse in response to mechanical deformation. The
piezoelectric potential between the electrodes vanishes when the
1060 W. He et al. / Applied Surface Science 392 (2017) 10551061
Fig. 6. Proposed mechanism for DC power generation from the TFNG through bending (a) and compressing test (b).
external stress on the TFNG device is removed during the unbend-
ing (decompressing) motion. Subsequently, the free electrons that
accumulate at the top electrode move back to the bottom side
through the external circuit, generating an electric pulse in the
opposite direction. Thus, both positive and negative currents and
voltages can be observed clearly.
Tellurium (Te), with a high work function (4.95 eV), has the high-
est strain piezoelectric coefcient among all existing piezoelectric
materials. It is well known that surface piezoelectricity that is
inherent in nanoake structure produces a signicant piezoelectric
effect when the thickness of the nanoake is reduced to less than
30 nm as reported elsewhere [29,31,32], thus enhancing the output
voltage performance dramatically even with the random distribu-
tion of nanoakes. We thus believe that the observation of such
large output power from our Te NFNG devices could be originated
from the dominant surface piezoelectricity, not alone with a large
surface area and high density of Te nanoakes whose thickness is
less than 20 nm. Furthermore, the randomly distributed nanoakes
proves to be more structurally robust under the repeated huge
external force when compared with the nanowires or nanorods due
to the interconnected morphology [30], leading to higher and more
stable output power compared to other Te based NGs reported
elsewhere. [27]
4. Conclusions
In summary, we have fabricated a novel form of Te NF, a new
class of piezoelectric nanomaterial suitable for wearable NGs with
ultrahigh output power. The generated outputs of the TFNG device
during the bending and compression tests were all systematically
investigated. Typically, our TFNG device reached an open-circuit
voltage and a closed-circuit current of 3 V and 290 nA, respectively,
during periodic bending tests under identical strains. Arm-bending
was also carried out to conrm the materials practical applica-
tion for converting vibrational energy from human activities into
electrical energy. The output voltage and current produced by the
repeated bending and unbending actions of a human arm reached
up to 2.5 V and 650 nA, respectively.
Furthermore, the maximum output open-circuit voltage of
125.3 V, the closed-circuit current density of 16.5 A/cm2 , and the
output power density of 2.07 mW/cm2 were generated during the
compression test under a driving frequency of 10 Hz and compres-
sive force of 8 N. Such a high output power was sufcient to light
up at least 10 LEDs. We believe our study of this TFNG device can
be expanded to explore the capacities of various Te nanomateri-
als with different morphologies to convert mechanical energy into
electrical energy using the piezoelectric effect. With the advantages
of high output power, this TFNG device has prospects for broad
application in the elds of exible and wearable NGs.
Acknowledgments
This work was supported by the BioNano Health Guard
Research Center, funded through the Ministry of Science,
ICT & Future Planning (MSIP) of Korea as a Global Frontier
Project (HGUARD 2013M3A6B2) and the Fundamental Technol-
ogy Research Program through the National Research Foundation
of Korea, with grants funded by the Korean government
(2014M3A7B4052201). HSC would also like to acknowledge the
nancial support provided by the Korean Evaluation Institute of
Industrial Technology (KEIT) funded by the Ministry of Trade,
Industry & Energy (MOTIE) (NO. 10052980).
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.apsusc.2016.09.
157.
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