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

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 cyclohexanol (99%, Sigma-Aldrich), or 1-dodecanol (98%,
pattern using the self-assembly capable of solution process. Sigma-Aldrich). The ink was then briefly sonicated for 1 min to
In this work, we successfully manufactured transparent retain the length and diameter of Ag NWs.
electrodes with a novel concept and report several new Fabrication of Ag NWs Transparent Electrodes. To
advancements using Ag NWs. First, the Ag NWs network with fabricate the transparent electrode, the PET films were treated
a cell shape similar to the Ag grid was self-assembled on flexible using oxygen plasma equipment (ICP-PIE, Standard Asher RIE
polyethylene terephthalate (PET) films by mixing water- System, SNTEK) for 10 s to form a hydrophilic surface. The Ag
dispersed Ag NWs and a small amount of solvents such as α- NW ink was dropped on the PET film and then quickly pulled
terpineol, cyclohexanol, and 1-dodecanol. This cell-structured down using a Meyer rod (R.D. Specialties #16, 40.6 μm wet
self-assembly would be an easily scalable and fast fabrication film thickness), as shown in Figure 1d. The Ag NWs coated
method using the existing cheap coating equipment, such as PET film was dried at 70 °C. To remove the residual solvents,
Meyer rod, slot die, doctor blade, spin coating, and gravure the Ag NWs electrode was dipped in methanol for 10 min and
techniques. Furthermore, we experimentally explained the heated at 150 °C for annealing the Ag NWs for 1 h.
mechanism by differences in solvent evaporation. In this Characterization. The contact angle of DI water was
regard, the self-assembled cell size was easily controlled from 10 analyzed using a contact angle analyzer (Phoenix 300 plus,
to 100 μm with respect to the solvents ratio. Transparent SEO) at room temperature to evaluate the wettability of the
electrodes were employed on a Meyer rod technique for PET films. The optical transmittance and sheet resistance
scalable coating roll-to-roll of Ag NWs. Finally, the method was values of the Ag NWs electrode were measured by a UV/vis
compared to the random Ag NWs self-assembly method, spectrometer (Mega-2100, Scinco) and a four-point probe
resulting in self-assembly into cell-shaped Ag NWs clearly (CMT-SR2000N, AIT). The reference of the UV/vis
showing enhanced performance of the transparent electrodes.
spectrometer was the original PET film. The haze value was
analyzed using a haze meter (NDH-2000N, Nippon
2. EXPERIMENTAL METHODS Denshoku). The sheet resistance of the samples was the
Preparation of Ag NWs Ink. The aqueous solution average of 10 measurements. The cell structure of the Ag NWs
contained 0.5 wt % Ag NWs and was purchased from was observed using a field-emission scanning electron micro-
NANOPYXIS. The concentration of Ag NWs in the aqueous scope (FE-SEM; S-4800, Hitachi).
solution was adjusted from 0.1 to 3.0 wt %. The ink formulation To investigate the mechanical properties of the prepared Ag
was made by mixing the Ag NWs solution (2.5 g), methanol (6 NWs transparent electrodes, a bending test was performed
g, MeOH), α-terpineol solvent (1.5 g, 90% Sigma-Aldrich), using the homemade IPC sliding tester.31 The samples (20 mm
5741 DOI: 10.1021/acs.jpcc.7b00148
J. Phys. Chem. C 2017, 121, 5740−5746
The Journal of Physical Chemistry C Article

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 3. RESULTS AND DISCUSSION
consisting of lower and upper plates. In the system, the upper The contact angle images were captured using a charge-coupled
plate is fixed, while the lower plate moves laterally with stroke device (CCD) camera. The contact angle of Ag NWs ink on
untreated PET film was 74.22°, which decreased to 34.68° after
of 180 cycles/min. The resistance changes were measured over
oxygen plasma treatment (Figure 1a). The introduction of
the bending test of 10 000 cycles. We also tested their polar groups (−OH, −COOH, and −CO) to the PET film
mechanical properties under the extreme condition of folding surface enhances wettability between the Ag NWs ink and PET
films, resulting in a uniform Ag NWs film coating without
and crushing the transparent electrodes. The Ag NWs self-
agglomeration.32 As shown in Figure 1b and Figure S1, the
assembled on PET film (12 × 12 cm2) were connected with a average diameter and length of the Ag NWs used was
blue LED and an external voltage of 5 V. The condition of ink approximately 31.73 ± 4.41 nm and 20.75 ± 3.03 μm,
component was the Ag NWs solution (2.5 g), methanol (6 g, respectively. Figure 1c shows a formulated Ag NW ink
composed of an aqueous Ag NWs solution with 0.5 wt % Ag
MeOH), and α-terpineol solvent (1.5 g). After the folding, NWs, MeOH, and α-terpineol. The Ag NWs ink was developed
crushing, and then unfolding, the LED test was performed. for a simple and scalable Meyer rod coating in Figure 1d.
5742 DOI: 10.1021/acs.jpcc.7b00148
J. Phys. Chem. C 2017, 121, 5740−5746
The Journal of Physical Chemistry C Article

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: Figure 4. Transmittance at 550 nm plotted as a function of film sheet
various nozzle sizes for forming the droplet would be required resistance for random and cell-shaped self-assembly Ag nanowire. The
for controlling the ring size, and the process is complicated and performance of two methods is shown for comparison. The inset
time-consuming. By tuning the volume of the solvents, various graph represents fits to the transparent versus sheet resistance using eq
cell sizes of conductive Ag NWs can be fabricated, and the 1.
performance was ∼50 Ω/sq.
We evaluated the performance of the cell-shaped self- the industry standard of σdc/σop = 35 required in the
assembly and random self-assembly for comparing the two transparent electrode market, especially the cell-shaped self-
types of Ag NWs in the optical transmittance and sheet assembly presenting a better performance than the random self-
resistance. The cell-shaped self-assembly was fixed by the assembly. In addition, we measured the haze of cell-shaped self-
solvent volume of 2.5 g. In contrast, random self-assembly was assembly with the different concentration of Ag nanowire, in
conducted by experiments under the same condition with inks Figure S3. As the concentration of self-assembled Ag NWs inks
composed of an aqueous Ag NWs solution (2.5 g) and MeOH increased, the haze values were increased from 0.48, 0.64, 3.11,
(7.5 g) without additional solvents. The cell-shaped and 5.59 to 10.27%. The haze value of 0.5% concentration with the
random self-assembled transparent electrodes with several transmittance and sheet resistance of 91.22% and 54.17 Ω/□
concentrations of Ag NWs are shown in Figure 3. First of all, meet the industrial standard for transparent electrode at the
it could be confirmed that the morphology of the Ag NWs is optical haze of 2−4%.
well retained after sonication process, as shown in the random Figure 5a shows a schematic diagram of the cell network
self-assembly images of 0.1 and 0.25 wt % of Figure 3. Different mechanism that was divided into three steps. First, the high
Ag NW coverage densities were obtained with increasing vapor pressure MeOH was first evaporated in the Ag NW inks.
concentration of Ag NW ink. Interestingly, the average cell size Second, because the α-terpineol is insoluble in DI water, the
of Ag NWs was nearly similar at ∼30 μm, despite the different low-viscosity DI water spreads around the droplet of α-
densities of the Ag NWs. The volume of α-terpineol was most terpineol. The Ag NWs dispersed in DI water were then self-
likely the dominant parameter determining the cell size. Figure assembled around the droplet of α-terpineol. Finally, all
S2 is the optical transmittance spectra for the cell-shaped and solvents were evaporated, resulting in the formation of Ag
random self-assemblies with different densities. Based on these NWs cell structures. The process of Ag NWs self-assembly was
spectra, the optical transmittance at a wavelength of 550 nm confirmed in the Supporting Information Movie S1. For a proof
was plotted as a function of sheet. Based on these spectra, the of mechanism, we tested other solvents, such as cyclohexanol
optical transmittance at a wavelength of 550 nm was plotted as and 1-dodecanol, which are commonly insoluble in DI water
a function of sheet resistance in Figure 4. It seems reasonable and soluble in MeOH and have a high viscosity (DI water: 0.89
that the cell-shaped self-assembly is ready to build the specific cP, MeOH: 0.54 cP, α-terpineol: 36.5 cP, cyclohexanol: 41.07
conductive network and transmittance at the same Ag NWs cP, 1-dodecanol: 18.8 cP). The ink formulation composed of
content loading as the random self-assembly. To judge the cyclohexanol and 1-dodecanol is the same as the Ag NWs of α-
performance of the silver network as a transparent electrode, we terpineol. The Ag NWs inks with cyclohexanol and 1-
used the figure of merit defined as the ratio of the bulk dc dodecanol self-assembled into a cell network, as shown in
conductivity and optical conductivity (σdc/σop).34−36 Herein, Figure 5b and c. The cell size, optical transmittance, and sheet
the higher σdc/σop, the better performance of the transparent resistance are summarized in Table S1. Figure S4 is the optical
electrodes. transmittance spectra with different solvents. In the case of 1-
dodecanol, the cell size was larger than those of the Ag NWs
⎛ Z σop ⎞
−2
inks of α-terpineol or cyclohexanol due to the different viscosity
T = ⎜1 + 0 ⎟
⎝ 2R s σdc ⎠ (1) values. The viscosity is representative of fluid resistance to flow.
Therefore, although the volume of 1-dodecanol was the same as
In eq 1, Z0 is the impedance of free space (377 Ω). The fits of that of α-terpineol, 1-dodecanol, which has a lower viscosity
the data following eq 1 result in figures of merit of σdc/σop = than α-terpineol or cyclohexanol, is more spread on the films,
218.6 and σdc/σop = 146.0, as shown in the inset data, with good resulting in the formation of a larger cell size. This mechanism
linearity. The values of the Ag NWs networks were superior to can also explain the relation between α-terpineol volume and
5743 DOI: 10.1021/acs.jpcc.7b00148
J. Phys. Chem. C 2017, 121, 5740−5746
The Journal of Physical Chemistry C Article

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 mm of bending radius = 1.28, 1.29, and 1.73% increase). The
cell size is increased, the cell size of Ag NWs is increased cell-structured Ag NWs transparent electrode demonstrated an
because the remaining α-terpineol is increased after the excellent mechanical performance compared to the previously
evaporation of MeOH. reported Ag NWs transparent electrodes.15,37,38 Additionally, a
The mechanical stability of transparent electrodes is one of blue light emitting diode (LED) connected to the transparent
the most important characteristics for flexible electronics. The electrodes was successfully fabricated on a flexible PET film
samples for the bending test were prepared by cutting the Ag with a large area, as shown in Figure S5. After the extreme
NWs self-assembled on PET film as shown in Figure 6b and c. stress of folding and crushing, the LED intensity with cell-
The transparent electrode was loaded into the bending system shaped Ag NWs had no obvious changes, and the conductivity
halfway, and the resistance change was measured in both ends remained. Lastly, intense pulsed light (IPL) sintering was
of samples. Figure 6 shows a repeated fatigue bending test with employed in the transparent electrodes self-assembled with 0.5
respect to the bending radius of 5, 10, and 15 mm. The wt % Ag NWs. The IPL sintering has recently been known as
resistance of transparent electrodes did not change by within an effective ways of enhancing the conductivity of metallic
2% deviation during 10 000 cycles of bending (5, 10, and 15 materials without the deformation of polymeric substrates, such
5744 DOI: 10.1021/acs.jpcc.7b00148
J. Phys. Chem. C 2017, 121, 5740−5746
The Journal of Physical Chemistry C Article

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
■ ACKNOWLEDGMENTS
This work was supported by the Human Resources Develop-
shown in Figure S6, and the junctions between wires were ment program No. 20154030200680 of the Korea Institute of
enhanced to form tight contacts. The sheet resistance and Energy Technology Evaluation and Planning (KETEP) grant
optical transmittance are 20.53 ± 2.09 Ω/□ and 89.02%. These funded by the Korea government Ministry of Trade, Industry
figures were much more enhanced than thermal annealing and Energy.

■
which is 50.71 ± 4.75 Ω/□ (92.64%). Although the results of
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5746 DOI: 10.1021/acs.jpcc.7b00148

J. Phys. Chem. C 2017, 121, 5740−5746