Article

pubs.acs.org/JPCC

Novel Concept for Fabricating a Flexible Transparent Electrode Using

the Simple and Scalable Self-Assembly of Ag Nanowires
Young-Tae Kwon,#,† Jong Woon Moon,#,‡ Yo-Min Choi,§ Seil Kim,† Seung Han Ryu,†
and Yong-Ho Choa*,†,‡
†
Department of Fusion Chemical Engineering, and ‡Department of Bionano Technology, Hanyang University, Ansan 426-791,
Republic of Korea
§
Material and Components Technology Center, Korea Testing Laboratory, Ansan 426-791, Republic of Korea
*
S Supporting Information

ABSTRACT: We introduce a new concept for transparent electrodes via the

self-assembly of a silver nanowire (Ag NW) network with a cell shape. A
transparent conductive network was achieved by forming an array of Ag NWs
around droplets of a solvent with higher vapor pressure in Ag NWs ink. The
difference in vapor pressure and viscosity of the solvent causes an Ag NWs
network with a cell shape, and the cell size can be easily controlled from 10 to
100 μm using the solvent ratio. The cell network of Ag NWs with a high optical
transmittance (>92%) and low sheet resistance (40 Ω/sq) was simply
fabricated on flexible polymer films of large scale using a Meyer rod coating. In
addition, we also studied and demonstrated the figure of merit of the
transparent electrode between our method and a random Ag NWs network
from the general method. The performance of the transparent electrode may be
applied to a wide array of optoelectronic devices and can replace transparent
conductive oxides such as Al-doped ZnO and indium tin oxide.

1. INTRODUCTION materials are well-known for having a high conductivity and

Transparent electrodes are fundamental components in
optoelectronic devices, including displays and solar cells.
Recently, many researchers have moved toward the manufac-
turing of flexible electronics with a low-cost, easy, and large-
scale process. The sheet resistance (Rs) and optical trans-
mittance (T) are the most important features for transparent
electrodes, which require different performances depending on
the application. For example, >1 kΩ/sq is sufficient for the
application of antistatic and electromagnetic shielding; touch
screens require 400−1000 Ω/sq; organic light-emitting diodes
(OLED) and solar cells require <10 Ω/sq.1−3 To date, indium
tin oxide (ITO) has been commonly used for this purpose,
resulting in a market share reaching 90% for transparent
electrode fields due to the high optical transmittance and low
sheet resistance.3,4 However, the use of ITO as transparent
electrodes has many drawbacks for the next generation of
optoelectronic devices with flexibility due to the brittleness of
conductive oxide, scarcity of indium, and difficulty in large
areas. Therefore, many transparent electrode materials have
been considered to replace ITO for future flexible optoelec-
tronics. Several promising candidates include carbon-based
materials such as CNT5−7 and graphene,8−10 polymer materials
such as PEDOT:PSS,11−13 and Ag metal materials such as
nanoparticles (NPs)14−18 and nanowires (NWs).19−23 Among
these materials, Ag metal materials have attractive performance
as transparent electrodes in terms of conductivity and stability
compared to carbon-based materials and polymers.15,20 Ag
resistance to oxidation compared to different metals.24
Transparent electrodes based on Ag nanomaterials are
divided into two configurations, a regular Ag grid14−18,25 and
random Ag NWs self-assembly,26−30 which can exhibit optical
transparency and sheet resistance superior to other materials.
However, the Ag grid and random Ag NWs self-assembly
methods have several drawbacks. In the case of the Ag grid,
although the transparent electrodes with a high repeatability
and device stability can be fabricated by controlling the grid
width, spacing, and thickness of the grid, the fabrication
method is often complicated, costly, and time-consuming
because the process can include photolithography, direct
printing, or embossing.2,3,25 Especially, the transparent
electrode fabrication method using coffee ring effect is time-
consuming due to repetition of dropping one droplet and then
drying and the need for additional expensive equipment for
formation of the constant droplet. Additionally, the random Ag
self-assembly method, which is suitable for solution-based
processes, is simple and easy to mass-produce; however, the
performance of the resultant transparent electrodes is depend-
ent on the length of the nanowire, resulting in poor
connectivity and high resistivity.15,25 Therefore, to fabricate
the transparent electrode of high performance for simple and
Received: January 5, 2017
Revised: February 20, 2017
Published: February 27, 2017

© 2017 American Chemical Society 5740 DOI: 10.1021/acs.jpcc.7b00148

J. Phys. Chem. C 2017, 121, 5740−5746
The Journal of Physical Chemistry C
Figure 1. (a) Contact angle image of DI water on oxygen plasma treated PET film. The inset image is contact angle of DI water on bare PET. (b)
SEM image of Ag nanowires. (c) Water-dispersed Ag nanowire solution with concentration of 0.5 wt %. (d) Schematic of Meyer rod coating process
for Ag nanowire coating on the PET film.
inexpensive method, it is important to manufacture the Ag grid
pattern using the self-assembly capable of solution process.
In this work, we successfully manufactured transparent
electrodes with a novel concept and report several new
advancements using Ag NWs. First, the Ag NWs network with
a cell shape similar to the Ag grid was self-assembled on flexible
polyethylene terephthalate (PET) films by mixing water-
dispersed Ag NWs and a small amount of solvents such as α-
terpineol, cyclohexanol, and 1-dodecanol. This cell-structured
self-assembly would be an easily scalable and fast fabrication
method using the existing cheap coating equipment, such as
Meyer rod, slot die, doctor blade, spin coating, and gravure
techniques. Furthermore, we experimentally explained the
mechanism by differences in solvent evaporation. In this
regard, the self-assembled cell size was easily controlled from 10
to 100 μm with respect to the solvents ratio. Transparent
electrodes were employed on a Meyer rod technique for
scalable coating roll-to-roll of Ag NWs. Finally, the method was
compared to the random Ag NWs self-assembly method,
resulting in self-assembly into cell-shaped Ag NWs clearly
showing enhanced performance of the transparent electrodes.
2. EXPERIMENTAL METHODS
Preparation of Ag NWs Ink. The aqueous solution
contained 0.5 wt % Ag NWs and was purchased from
NANOPYXIS. The concentration of Ag NWs in the aqueous
solution was adjusted from 0.1 to 3.0 wt %. The ink formulation
was made by mixing the Ag NWs solution (2.5 g), methanol (6
g, MeOH), α-terpineol solvent (1.5 g, 90% Sigma-Aldrich),
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cyclohexanol (99%, Sigma-Aldrich), or 1-dodecanol (98%,
Sigma-Aldrich). The ink was then briefly sonicated for 1 min to
retain the length and diameter of Ag NWs.
Fabrication of Ag NWs Transparent Electrodes. To
fabricate the transparent electrode, the PET films were treated
using oxygen plasma equipment (ICP-PIE, Standard Asher RIE
System, SNTEK) for 10 s to form a hydrophilic surface. The Ag
NW ink was dropped on the PET film and then quickly pulled
down using a Meyer rod (R.D. Specialties #16, 40.6 μm wet
film thickness), as shown in Figure 1d. The Ag NWs coated
PET film was dried at 70 °C. To remove the residual solvents,
the Ag NWs electrode was dipped in methanol for 10 min and
heated at 150 °C for annealing the Ag NWs for 1 h.
Characterization. The contact angle of DI water was
analyzed using a contact angle analyzer (Phoenix 300 plus,
SEO) at room temperature to evaluate the wettability of the
PET films. The optical transmittance and sheet resistance
values of the Ag NWs electrode were measured by a UV/vis
spectrometer (Mega-2100, Scinco) and a four-point probe
(CMT-SR2000N, AIT). The reference of the UV/vis
spectrometer was the original PET film. The haze value was
analyzed using a haze meter (NDH-2000N, Nippon
Denshoku). The sheet resistance of the samples was the
average of 10 measurements. The cell structure of the Ag NWs
was observed using a field-emission scanning electron micro-
scope (FE-SEM; S-4800, Hitachi).
To investigate the mechanical properties of the prepared Ag
NWs transparent electrodes, a bending test was performed
using the homemade IPC sliding tester.31 The samples (20 mm
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Figure 2. (a−c) SEM images of Ag nanowire array with respect to α-terpineol volume of 0.5, 1.5, and 2.5 mL. (d) Optical transmittance spectra of
the self-assembled Ag nanowire.
Figure 3. SEM images of Ag nanowire array according to Ag nanowire concentration using the random and cell-shaped self-assembly.
wide, 150 mm long) were loaded into the bending system
consisting of lower and upper plates. In the system, the upper
plate is fixed, while the lower plate moves laterally with stroke
of 180 cycles/min. The resistance changes were measured over
the bending test of 10 000 cycles. We also tested their
mechanical properties under the extreme condition of folding
and crushing the transparent electrodes. The Ag NWs self-
assembled on PET film (12 × 12 cm2) were connected with a
blue LED and an external voltage of 5 V. The condition of ink
component was the Ag NWs solution (2.5 g), methanol (6 g,
MeOH), and α-terpineol solvent (1.5 g). After the folding,
crushing, and then unfolding, the LED test was performed.
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3. RESULTS AND DISCUSSION
The contact angle images were captured using a charge-coupled
device (CCD) camera. The contact angle of Ag NWs ink on
untreated PET film was 74.22°, which decreased to 34.68° after
oxygen plasma treatment (Figure 1a). The introduction of
polar groups (−OH, −COOH, and −CO) to the PET film
surface enhances wettability between the Ag NWs ink and PET
films, resulting in a uniform Ag NWs film coating without
agglomeration.32 As shown in Figure 1b and Figure S1, the
average diameter and length of the Ag NWs used was
approximately 31.73 ± 4.41 nm and 20.75 ± 3.03 μm,
respectively. Figure 1c shows a formulated Ag NW ink
composed of an aqueous Ag NWs solution with 0.5 wt % Ag
NWs, MeOH, and α-terpineol. The Ag NWs ink was developed
for a simple and scalable Meyer rod coating in Figure 1d.
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Figure 2a, b, and c show the self-assembled Ag NW cell
network on PET films fabricated with respect to the α-terpineol
volume of 0.5, 1.5, and 2.5 g; because the Ag NWs inks were
fixed to a weight of 10 g, the volume of MeOH was adjusted to
7.0, 6.0, and 5.0 g, respectively. As the α-terpineol volume
increased, the cell size also increased from 6.71 to 126 μm. The
size of the cell composed of Ag NWs was constant, while the
network was similar to transparent electrodes of a metallic grid
made by a complicated process in terms of repetition of
constant spacing and size. However, there are no significant
differences in optical transmittance (Figure 2d) and sheet
resistance, as listed in Table S1, because the absolute Ag NWs
in the ink was the same. Recently, the printed array of rings
composed of Ag NPs were reported for a coffee stain effect,
where a droplet containing solid particles was dropped, the
droplet was dried, and the solid particles were closely packed to
the droplet rim.14,33 Although the transparent electrodes have a
high optical transmittance, they have some intrinsic limitations:
various nozzle sizes for forming the droplet would be required
for controlling the ring size, and the process is complicated and
time-consuming. By tuning the volume of the solvents, various
cell sizes of conductive Ag NWs can be fabricated, and the
performance was ∼50 Ω/sq.
We evaluated the performance of the cell-shaped self-
assembly and random self-assembly for comparing the two
types of Ag NWs in the optical transmittance and sheet
resistance. The cell-shaped self-assembly was fixed by the
solvent volume of 2.5 g. In contrast, random self-assembly was
conducted by experiments under the same condition with inks
composed of an aqueous Ag NWs solution (2.5 g) and MeOH
(7.5 g) without additional solvents. The cell-shaped and
random self-assembled transparent electrodes with several
concentrations of Ag NWs are shown in Figure 3. First of all,
it could be confirmed that the morphology of the Ag NWs is
well retained after sonication process, as shown in the random
self-assembly images of 0.1 and 0.25 wt % of Figure 3. Different
Ag NW coverage densities were obtained with increasing
concentration of Ag NW ink. Interestingly, the average cell size
of Ag NWs was nearly similar at ∼30 μm, despite the different
densities of the Ag NWs. The volume of α-terpineol was most
likely the dominant parameter determining the cell size. Figure
S2 is the optical transmittance spectra for the cell-shaped and
random self-assemblies with different densities. Based on these
spectra, the optical transmittance at a wavelength of 550 nm
was plotted as a function of sheet. Based on these spectra, the
optical transmittance at a wavelength of 550 nm was plotted as
a function of sheet resistance in Figure 4. It seems reasonable
that the cell-shaped self-assembly is ready to build the specific
conductive network and transmittance at the same Ag NWs
content loading as the random self-assembly. To judge the
performance of the silver network as a transparent electrode, we
used the figure of merit defined as the ratio of the bulk dc
conductivity and optical conductivity (σdc/σop).34−36 Herein,
the higher σdc/σop, the better performance of the transparent
electrodes.
⎛ Z σop ⎞
−2
T = ⎜1 + 0 ⎟
⎝ 2R s σdc ⎠ (1)
In eq 1, Z0 is the impedance of free space (377 Ω). The fits of
the data following eq 1 result in figures of merit of σdc/σop =
218.6 and σdc/σop = 146.0, as shown in the inset data, with good
linearity. The values of the Ag NWs networks were superior to
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Figure 4. Transmittance at 550 nm plotted as a function of film sheet
resistance for random and cell-shaped self-assembly Ag nanowire. The
performance of two methods is shown for comparison. The inset
graph represents fits to the transparent versus sheet resistance using eq
1.
the industry standard of σdc/σop = 35 required in the
transparent electrode market, especially the cell-shaped self-
assembly presenting a better performance than the random self-
assembly. In addition, we measured the haze of cell-shaped self-
assembly with the different concentration of Ag nanowire, in
Figure S3. As the concentration of self-assembled Ag NWs inks
increased, the haze values were increased from 0.48, 0.64, 3.11,
5.59 to 10.27%. The haze value of 0.5% concentration with the
transmittance and sheet resistance of 91.22% and 54.17 Ω/□
meet the industrial standard for transparent electrode at the
optical haze of 2−4%.
Figure 5a shows a schematic diagram of the cell network
mechanism that was divided into three steps. First, the high
vapor pressure MeOH was first evaporated in the Ag NW inks.
Second, because the α-terpineol is insoluble in DI water, the
low-viscosity DI water spreads around the droplet of α-
terpineol. The Ag NWs dispersed in DI water were then self-
assembled around the droplet of α-terpineol. Finally, all
solvents were evaporated, resulting in the formation of Ag
NWs cell structures. The process of Ag NWs self-assembly was
confirmed in the Supporting Information Movie S1. For a proof
of mechanism, we tested other solvents, such as cyclohexanol
and 1-dodecanol, which are commonly insoluble in DI water
and soluble in MeOH and have a high viscosity (DI water: 0.89
cP, MeOH: 0.54 cP, α-terpineol: 36.5 cP, cyclohexanol: 41.07
cP, 1-dodecanol: 18.8 cP). The ink formulation composed of
cyclohexanol and 1-dodecanol is the same as the Ag NWs of α-
terpineol. The Ag NWs inks with cyclohexanol and 1-
dodecanol self-assembled into a cell network, as shown in
Figure 5b and c. The cell size, optical transmittance, and sheet
resistance are summarized in Table S1. Figure S4 is the optical
transmittance spectra with different solvents. In the case of 1-
dodecanol, the cell size was larger than those of the Ag NWs
inks of α-terpineol or cyclohexanol due to the different viscosity
values. The viscosity is representative of fluid resistance to flow.
Therefore, although the volume of 1-dodecanol was the same as
that of α-terpineol, 1-dodecanol, which has a lower viscosity
than α-terpineol or cyclohexanol, is more spread on the films,
resulting in the formation of a larger cell size. This mechanism
can also explain the relation between α-terpineol volume and
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Figure 5. (a) Schematic illustration of the self-assembly process of Ag nanowires. SEM images of Ag nanowire films with different additives: (b)
cyclohexanol and (c) 1-dodecanol.

Figure 6. Graph showing resistance change of Ag NWs network with a cell shape under the 10 000 bending cycles at the bends radius of 5, 10, 15
mm. (a) Detailed graph for verifying specific changes. (b) Illustration of the resistance fatigue test sample. The samples are prepared for the size of
150 mm × 20 mm in accordance with the image after the Ag NWs coating on PET film of 15 × 15 cm2. The real optical image of (c) sample and (d)
bending test machine.

cell size in Figure 2. As the volume of α-terpineol determining
cell size is increased, the cell size of Ag NWs is increased
because the remaining α-terpineol is increased after the
evaporation of MeOH.
The mechanical stability of transparent electrodes is one of
the most important characteristics for flexible electronics. The
samples for the bending test were prepared by cutting the Ag
NWs self-assembled on PET film as shown in Figure 6b and c.
The transparent electrode was loaded into the bending system
halfway, and the resistance change was measured in both ends
of samples. Figure 6 shows a repeated fatigue bending test with
respect to the bending radius of 5, 10, and 15 mm. The
resistance of transparent electrodes did not change by within
2% deviation during 10 000 cycles of bending (5, 10, and 15
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mm of bending radius = 1.28, 1.29, and 1.73% increase). The
cell-structured Ag NWs transparent electrode demonstrated an
excellent mechanical performance compared to the previously
reported Ag NWs transparent electrodes.15,37,38 Additionally, a
blue light emitting diode (LED) connected to the transparent
electrodes was successfully fabricated on a flexible PET film
with a large area, as shown in Figure S5. After the extreme
stress of folding and crushing, the LED intensity with cell-
shaped Ag NWs had no obvious changes, and the conductivity
remained. Lastly, intense pulsed light (IPL) sintering was
employed in the transparent electrodes self-assembled with 0.5
wt % Ag NWs. The IPL sintering has recently been known as
an effective ways of enhancing the conductivity of metallic
materials without the deformation of polymeric substrates, such
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as PET, PI, and PC, caused by thermal energy.39,40 A top and
tilt SEM image of the Ag NWs after 8.0 J·cm−2 illumination is
shown in Figure S6, and the junctions between wires were
enhanced to form tight contacts. The sheet resistance and
optical transmittance are 20.53 ± 2.09 Ω/□ and 89.02%. These
figures were much more enhanced than thermal annealing
which is 50.71 ± 4.75 Ω/□ (92.64%). Although the results of
IPL annealing were fundamental experiment stage, the
properties of transparent electrode were improved, and this
will be further studied.
To the best of our knowledge, the cell-shaped self-assembly
of Ag NWs on transparent electrodes has not been previously
fabricated based on differences in solvent evaporation. This self-
assembly method might be an easily scalable coating using slot
die or gravure techniques and may be applied to metal
nanowires and other nanowire materials.
4. CONCLUSIONS
In conclusion, the Ag NWs networks of new concept were
fabricated via self-assembly of Meyer rod on the PET films. The
principle of cell network with Ag NWs is demonstrated by
difference of vapor pressure and viscosity among the DI water,
MeOH, and various solvents such as α-terpineol, cyclohexanol,
and 1-dodecanol. The Ag NWs cell network has identified that
the performances with a high optical transmittance (>92%) and
low sheet resistance (40 Ω/sq) are superior to random network
of Ag NWs using figure of merit (σdc/σop). The mechanical
testing demonstrated that the transparent electrodes have
extreme flexibility under bending fatigue test with resistance
change being less than 2% during 10 000 cycles. The novel
concept with cell-shaped self-assembly of Ag NWs should be
made to increase the transparent electrodes performance if the
annealing condition, such as intense pulse light or plasma
technique, is optimized, and this will be further studied.
■
ASSOCIATED CONTENT
*
S Supporting Information
The Supporting Information is available free of charge on the
ACS Publications website at DOI: 10.1021/acs.jpcc.7b00148.
Additional figures of the length and diameter of Ag NWs
and optical transmittance spectra; graph of haze value
with self-assembled Ag NWs; tables detailing the cell size,
optical transmittance, and sheet resistance of Ag NWs
network; photograph of transparent electrodes con-
nected with LED; FE-SEM images of IPL sintered Ag
NWs (PDF)
Video showing a self-assembled process of Ag NWs inks
after the Meyer rod coating (AVI)
■ AUTHOR INFORMATION
Corresponding Author
*E-mail: choa15@hanyang.ac.kr.
ORCID
Yong-Ho Choa: 0000-0002-1254-3593
Author Contributions
# (19) Wu, H.; Kong, D.; Ruan, Z.; Hsu, P.-C.; Wang, S.; Yu, Z.;
These authors equally contributed to this work. The
manuscript was written through contributions of all authors.
Notes
The authors declare no competing financial interest.
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■ ACKNOWLEDGMENTS
This work was supported by the Human Resources Develop-
ment program No. 20154030200680 of the Korea Institute of
Energy Technology Evaluation and Planning (KETEP) grant
funded by the Korea government Ministry of Trade, Industry
and Energy.
■
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5746 DOI: 10.1021/acs.jpcc.7b00148

J. Phys. Chem. C 2017, 121, 5740−5746