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B. Tugba Camic, Faruk Oytun, M. Hasan Aslan, Hee Jeong Shin, Hyosung Choi,
Fevzihan Basarir
PII: S0021-9797(17)30592-1
DOI: http://dx.doi.org/10.1016/j.jcis.2017.05.065
Reference: YJCIS 22372
Please cite this article as: B. Tugba Camic, F. Oytun, M. Hasan Aslan, H. Jeong Shin, H. Choi, F. Basarir, Fabrication
of a Transparent Conducting Electrode based on Graphene/Silver Nanowires via Layer-by-Layer Method for
Organic Photovoltaic Devices, Journal of Colloid and Interface Science (2017), doi: http://dx.doi.org/10.1016/j.jcis.
2017.05.065
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Fabrication of a Transparent Conducting Electrode based on Graphene/Silver
Nanowires via Layer-by-Layer Method for Organic Photovoltaic Devices
1
Department of Physics, Gebze Technical University, 41400, Gebze, Kocaeli, Turkey
2
Department of Chemistry, Istanbul Technical University, 34469, Maslak, Istanbul, Turkey
3
Department of Chemistry and Research Institute for Natural Sciences, Hanyang University,
04763 Seoul, South Korea
4
Materials Institute, TUBITAK Marmara Research Center (MRC), 41470 Gebze, Kocaeli,
Turkey
5
Next Chemicals & Plastics, 34490, Ikitelli, Istanbul, Turkey
*Corresponding Author
Dr. Fevzihan Basarir
Address: TUBITAK Marmara Research Center (MRC), Materials Institute, 41470 Gebze,
Kocaeli, Turkey
E-mail address: fevzihan@gmail.com
Tel: +90 262 677 2000
Fax: +90 262 677 2309
1
Abstract
(LBL) deposition of graphene oxide (GO) and silver nanowires (Ag NWs). First, graphite was
highly controllable thin films in terms of optical transmittance and sheet resistance. Next, the
reduction of GO sheets was performed to improve the electrical conductivity of the multilayer
films. The resulting GO/Ag NWs multilayer was characterized by a UV-Vis spectrometer,
field emission scanning electron microscope (FE-SEM), optical microscope (OM) and sheet
resistance using a four-point probe method. The best result was achieved with a 2-bilayer
film,
resulting in a sheet resistance of 6.5 sq-1 with an optical transmittance of 78.2% at 550 nm,
which values are comparable to those of commercial ITO electrodes. The device based on a 2-
bilayer hybrid film exhibited the highest device efficiency of 1.30% among the devices with
2
1. Introduction
Transparent conducting electrodes (TCEs) play an important role in organic electronic devices
such as solar cells, light emitting diodes, and transistors [1,2]. Indium tin oxide (ITO) is
typically used in TCEs for its superior optical and electrical characteristics. Although ITO has
excellent transparency in the visible spectrum, low sheet resistance, and effective work
function for injection and collection of charge carriers in organic semiconductors, its further
use has been restricted because of the lack of indium resources, brittleness, and complex
processing system [3]. Therefore, cheap, flexible and solution-processable ITO alternatives
have been developed, including graphene nanosheets (GNs) [4], carbon nanotubes (CNTs)
[5], conducting polymers [6], and metallic nanowires [7]. Among them, one-dimensional (1D)
silver nanowires (Ag NWs) and GNs have been attracting more attention because of
electrodes is less than 80 sq1 for 90% transmittance in the visible region [8]. These
optoelectrical properties meet industrial requirements, however the Ag NWs electrodes have
several drawbacks such as resistance [9], high surface roughness [10], and a hollow-space
area between the Ag NWs [11]. The voids between neighboring nanowires create shunting
and a corresponding leakage current, resulting in a high sheet resistance. The oxidation of Ag
NWs also increases sheet resistance due to junctionjunction resistance between nanowires
overcome these problems. Graphene has been widely used in optoelectronic devices because
of its unique properties such as high carrier mobility [14], a quantum hall effect [15], high
thermal and electrical conductivity [16], large surface area [17], ease of surface modification,
and excellent electrocatalytic activity [18]. Moreover, a GO layer can prevent the oxidation of
3
Ag NWs in a graphene/Ag NWs (G/Ag NW) hybrid film because of the gas barrier property
of graphene. GO laminates the Ag NWs surface by filling empty space, resulting in a low
groups. Alternatively, these polar groups make the GO surface hydrophilic, which leads to
high dispersibility in a polar solvent, particularly in water [19]. Moreover, this property
eliminate the oxygen containing functional groups on GO and restore sp2 carbon networks
[20]. Researchers have investigated various reducing agents, including hydrazine (N2H4) [21],
sodium borohydride (NaBH4) [22], lithium triethylborohydride [20], and hydrohalic acids
[23]. Among these reducing agents, GO reduction by hydrazine causes a high sheet resistance,
while it is not suitable for practical applications because of its high toxicity [24]. In this
However, NaBH4 does not effectively reduce epoxy groups and carboxylic acids [26], and
In this study, we fabricated G/Ag NWs hybrid transparent electrodes as an ITO alternative.
3- and 2-bilayer G/Ag NWs structures exhibited good electrical conductivity and optical
NWs (Ag NWs-NH2) by grafting of cysteamine, which forms -NH2 functional groups on the
Ag NWs. After the Ag NWs-NH2 were coated on the GO surface, the Ag NWs-NH2 reacted
with the epoxy functional groups of GO. By the strong electrostatic interaction between GO
and Ag NWs-NH2, the hybrid film was obtained using a layer by layer (LBL) coating, which
is a versatile method to assemble the solution processed nanomaterial on the thin film.
4
Furthermore, this technique makes it possible to control the thickness, transmittance, and
sheet resistance. For LBL coatings of GO and amine-functionalized Ag NWs (Ag NWs-NH2),
a spin-assisted assembly and dip coating method were used, respectively. Researchers have
reported many methods of coating GO on the glass substrate, including spin coating, dip
chemical vapor deposition (CVD) technique [28]. Most of these methods are difficult for
obtaining homogeneous GO thin film because of the tendency to crumble. However, the spin-
assisted assembly coating is a convenient and simple method for GO coating. Although many
methods have been used to fabricate Ag NW thin films, including vacuum filtration [29],
drop-casting [30], Meyer rod coating [31], and transferring [32] methods, dip coating is
Finally, the GO/Ag NWs hybrid film is reduced by NaBH4. The LBL process allows for the
production of G/Ag NWs hybrid TCEs with a low sheet resistance and high optical
transmittance.
Fig. 1. Schematic illustration for (a) modification process of Ag NWs with cysteamine and (b)
grafting of Ag NWs-NH2 on the GO layer.
5
2. Experimental
2.1. Materials
Graphite flakes (~150 m flakes), sulfuric acid (H2SO4, 95-98%), phosphoric acid (H3PO4,
anhydrous ethanol, methanol, and isopropyl alcohol (IPA) were purchased from Sigma
Aldrich. Silver nanowires (Ag NWs) dispersed in IPA (20 mg/ml) with an average diameter
of 50 nm and length of 5-10 m were obtained from ACS Materials. Glass slides (Menzel-
Glaser, 15 15 mm2) were sonicated in acetone and ethanol for 15 minutes and treated with
oxidant and should be handled with care). The samples were then sonicated in deionized (DI)
2.2. Synthesis of GO
GO was synthesized according to a modified procedure [33]. Briefly, graphite flakes (3.0 g)
were added to 400 ml of a concentrated H2SO4/H3PO4 mixture (9:1 v/v) and stirred until a
homogeneous suspension was obtained. Then, KMnO4 (18.0 g) was added to the mixture
slowly and allowed to stir at 50 C for 24 h. After the reaction was cooled to room
temperature, the solution was poured onto ice (360 g) and stirred with a magnetic stirrer.
Next, hydrogen peroxide (7 ml, 30%) was added to the solution and stirred for 4 h in an ice
bath, followed by centrifuging (5000 rpm, 20 min) to remove the acid and other impurities.
The final product was washed with DI water, hydrochloric acid (HCl), and ethanol
6
2.3. Preparation of amine-functionalized Ag NWs
procedure [34]. First, Ag NWs (10 mg) were centrifuged to remove IPA and dispersed in 50
ml ethanol. Then, cysteamine (30 mg) was added to the Ag NWs solution followed by stirring
for 24 h at room temperature. Then, the Ag NWs-NH2 were precipitated by centrifugation and
The LBL coating of GO and Ag NWs-NH2 was performed for preparation of TCE, which is
schematically shown in Fig. 1. First, the glass substrates were functionalized by immersing in
a 3% APTES solution for 3 h, followed by rinsing with excess methanol and drying under N2
flow. The substrates were then annealed at 100 C for 1 h to enable crosslinking of the
APTES molecules on the surface. The GO solution (1 mg/mL, 150 L) was spin-coated
(2.500 rpm and 25 s) on the APTES modified substrate, washed with DI water vigorously,
and dried at 50 C for 30 min. Next, the substrates were dipped into the Ag NWs-NH2
dispersion (0.5 mg/ml) for 20 min, followed by rinsing with DI water and drying at 50 C for
30 min. Multilayer films were obtained by repeating these processes. Consequently, the films
were dipped in the 150 mM NaBH4 solution at room temperature for 2 h to reduce the GO and
then washed with excess DI water. Finally, the films were annealed in a tube furnace at 230
7
Fig. 2. Schematic process for LBL assembly of GO and Ag NWs-NH2.
Renishaw) using a 514 nm argon ion laser in the range of 1003200 cm-1. The surface
Alpha, Thermo). Surface charges of GO and NH2-Ag NWs were determined by zeta potential
analysis (Nano ZS, Malvern Instruments, UK). The surface morphology of the TCEs was
analyzed by optical microscope (OM, ECLIPSE L150, Nikon), atomic force microscope
(AFM, Bruker Dimension Icon), and field emission scanning electron microscope (FE-SEM,
JEOL 63335F JSM). The sheet resistances of the TCEs were measured with a four-point
probe technique (RM3000, Jandel) while the optical properties were examined using an
8
2.6. Device fabrication and characterization
For fabrication of the reference device, ITO-coated glass substrates were cleaned by
ultrasonicating sequentially in DI water, acetone, and IPA. The following procedure was
utilized for both ITO and G/Ag NWs TCE substrates. A precursor solution of vanadium oxide
NWs-coated glass substrates at 6000 rpm for 40 sec, forming the hole transport layer. After
transferring samples into the nitrogen-filled glovebox, the active layer was spin-cast on the
V2O5 layer using a P3HT:PCBM solution (1:0.8 [wt.%]) dissolved in a mixed solvent of
electrode with a thickness of 100 nm was deposited on the active layer via a thermal
evaporator at 10-6 torr. The J-V curves of the devices were measured under AM 1.5G
illumination (100 mW cm-2) and inside a nitrogen-filled glove box without encapsulation
The obtained GOs were characterized by Raman spectroscopy (Fig. 3a). The first-order G and
D peaks, both arising from the vibrations of sp2 carbon, appeared at approximately 1580 cm-1
and 1350 cm-1, respectively. The G peak is due to the optical E2g phonons at the Brillouin
zone center resulting from the bond stretching of sp2 carbon pairs in both rings and chains
[35]. The D peak is due to the breathing modes of sp2 atoms in the rings [36].
NWs using cysteamine via a ligand exchange reaction. The thiol group of cysteamine reacts
with the silver atoms on the surface of Ag NWs, which in turn led to the formation of amine-
functionalized silver nanowires (Ag NWs-NH2). The XPS analysis was utilized for evaluating
9
the composition of the Ag NWs after surface modification. As shown in Fig. 3b, the XPS
spectra of Ag NWs-NH2 illustrated peaks at 162.3, 163.3, and 164.4 eV, which could be
attributed to the SAg bond between cysteamine and Ag NWs, SH bond of unreacted
cysteamine, and the SC bond of cysteamine, respectively. These results are in good
water to determine the surface charges and stability. Regardless of the pH, the surface charge
of GO was highly negative due to the oxygen groups (Fig. S1a). However, the best dispersion
was obtained for pH 10 (-40.8 mV in) due to the protonation of the COOH groups.
Additionally, the surface charge of Ag NWs-NH2 was determined as +31.2 mV (Fig. S1b).
Particles with highly negative or positive zeta potentials (more than 30 mV or less than -30
mV) provide sufficient mutual repulsion to ensure a stable dispersion [39]. The results
indicate that GO and Ag NWs-NH2 possessed sufficient surface charge for the stability of the
dispersions.
10
Fig. 3. (a) Raman spectra of GO and graphite (b) XPS S2p spectra of Ag NWs-NH2 (c)
Optical microscope images of 1 layer, (d) 2 and (e) 3 layer GO/Ag NWs films
The morphology of the GO/Ag NWs films was strongly influenced by the number of
GO/Ag NWs bilayers. As shown in Fig. 3 (c-e), the density of the Ag NWs on the substrate
was increased with an increasing number of bilayers, indicating successful LBL deposition. It
is noticeable that even 1-bilayer film resulted in a high density of nanowires (Fig. 3c).
Increasing the number of bilayers led to an increase in the packing density of the nanowires
11
Fig. 4. (a) Macro-images and (b) transmittance of GO/Ag NWs multilayer films.
Macro-images of the GO/Ag NWs multilayer films with different bilayers are shown in
Fig. 4a. It is clear that increasing the number of bilayers increased the concentration of the
yellowish color due to the increase in the Ag NWs density. This implies successful LBL
deposition. The sample is still transparent after deposition of 3-bilayer. As shown in Fig. 4b,
the optical transmittance of hybrid films decreased with increasing the number of layers. Each
GO and Ag NWs layer led to a decrease in optical transmittance of approximately 2.3% and
8.6%, respectively. The transmittance values of 1-, 2- and 3-bilayer TCEs were 89.1%, 78.3%
and 67.5%, respectively. These results proved that GO and Ag NWs were successfully coated.
This strong bonding between the GO and Ag NWs was derived from the ionic interactions
12
Table 1 shows the sheet resistance and transmittance values of the GO/Ag NWs and G/Ag
NWs hybrid films with different number of bilayers. The sheet resistances of 2- and 3-bilayer
GO/Ag NWs films were 537 k sq-1 (78.3%) and 520 k sq-1 (67.5%), respectively.
Compared to Ag NWs, GO has a lower electrical conductivity due to the rich hydrophilic
oxygen-containing groups such as carbonyl, epoxide, and carboxylic acid. For this reason,
when GO was introduced to the top layer of the multilayer film (TCE), the sheet resistance
increased from k sq-1 to M sq-1 (Table 1). Upon reduction, most of the oxygen-containing
groups, in particular the hydroxyl, epoxide, and carboxylic acid, were completely removed
[40] and the sheet resistance of the 2- and 3- bilayer GO/Ag NWs films decreased from 537
and 520 k sq-1 to 6.5 and 5.7 sq-1, respectively (Table 1). We suspect that both graphene
and Ag NWs network contributed to the conductivity of the hybrid film. The graphene acted
as a conducting bridge between disconnected Ag NWs and linker molecules, which generated
conducting path in the G/Ag NWs film. Therefore, the G/Ag NWs film revealed better
electrical conductivity.
Pristine GO 97.7 -
13
3-bilayer G/Ag NWs 65.3 5.7
3-bilayer G/Ag NWs
67.3 4.0
(anneal.) a
a
anneal.: Thermal annealing
To date, a wide range of chemical reducing agents have been reported to eliminate oxygen-
containing functional groups and restore pi-pi conjugation of GO. Among them, GO reduction
by NaBH4 is simple and effective in the restoration of the graphene structure [41]. As a result,
NaBH4 was employed for GO reduction in this work. The molarity of NaBH4 and reduction
time are important for the efficient reduction of GO. The degree of reduction affected the
sheet resistance of the reduced GO. According to literature [42], the sheet resistance was still
high with 15 mM NaBH4-reduced GO due to the presence of boron oxide complexes. A low
sheet resistance was obtained when using 150 mM NaBH4 for GO reduction. At a low molar
concentration, boron oxide complexes were formed and produced a slightly expanded
concentration, functional groups of GO removed, and thus boron oxide complexes eliminated
along with functional groups in GO. And higher NaBH4 concentration resulted in decreasing
interlayer distance and sheet resistance. In this work, 150 mM NaBH4 was used for reduction
processes and reduction was performed for a dipping time of 2 hours to prevent the self-
oxidation of NaBH4 in water. Finally, the sheet resistance of the 2- and 3-bilayer TCEs
decreased to 6.5 sq-1 (transmittance: 78.2%) and 4.0 sq-1 (67.3%) after thermal annealing
at 230 C (Table 1). The annealing treatment further decreased the sheet resistance by
inducing nanowire welding [43]. The G/Ag NWs-NH2 hybrid film showed lower optical
transmittance than GO/Ag NWs-NH2, suggesting a slightly higher optical absorption due to
partial restoration of the -electron system within the carbon structure after reducing the GO
film [44].
14
The performances of TCEs in terms of transparency and sheet resistance were calculated
by the figure-of-merit (FOM) equation, which is the ratio of the electrical and optical
where Z0 is the impedance of free space [377 ], Rs is the sheet resistance of the film [ sq-1],
and T is the transmittance of the film. The FOM values of 2- and 3-bilayer TCEs were 218
and 214, respectively. For comparison, the FOM of ITO TCE was 297, which is calculated
from its sheet resistance of 15 sq-1 and transmittance of 85% [45]. This evaluation indicated
that hybrid TCEs had comparable FOM values to that of typical ITO.
Fig. 5 shows typical scanning electron microscope (SEM) images of the surface
morphology of GO/Ag NWs hybrid films as a function of the number of layers. It is difficult
to understand from the SEM images of GO whether it fully covers the substrate. However, a
sparse network of Ag NWs in Fig. 5a illustrates that a fully covered GO layer was not
obtained. Although the Ag NWs network was sparse, it created electrical conductive paths for
the TCEs. However, this structure caused a high sheet resistance. The Ag NWs network
became dense with increasing the number of GO layers (Fig. 5b and 5c). The GO sheets
circumvents Ag NWs due to the flexible and stretchable properties of graphene [46]. This
situation ensures a tight contact between the Ag NWs that decreased the sheet resistance of
the film.
15
Fig. 5. SEM images of the GO/Ag NWs films with different number of bilayers: (a) 1-bilayer,
The extensive morphological characteristics of the GO/Ag NWs and GO/Ag NWs/GO film
were analyzed by AFM. The AFM images of the GO/Ag NWs (Fig. S2a and S2c) reveal that
the Ag NWs adhered tightly to the GO sheets. AFM images of the GO/Ag NWs/GO (Fig. S2b
and S2d) show that the Ag NWs were embedded between the GO layers.
To evaluate the performance of the G/Ag NWs hybrid film, the device was fabricated
using G/Ag NWs film as the anode. We employed a conventional and simple device
levels between the anode and hole transport material has a negative effect on device
performance, the work function of the anode should be high and well matched to the valence
band of HTL [47]. The work functions of graphene and silver nanowire are 4.48 and 4.20 eV,
respectively, which are similar to that of ITO (4.7 eV) and thus suitable for anode material.
of vanadium precursor with G/Ag NWs. For the active layer, P3HT and PCBM were used as
the electron donor and acceptor, respectively. Fig. 6b exhibits the current density-voltage (J-V)
curves of the devices based on the ITO and G/Ag NWs anode. The device with an ITO anode
showed a short-circuit current density (JSC) of 7.31 mA cm-2, an open-circuit voltage (VOC) of
16
0.57 V, fill factor (FF) of 0.56, and power conversion efficiency (PCE) of 2.31%. In terms of
electrical conductivity and transmittance, we chose G/Ag NWs film with 2-bilayer structure
for device optimization. The device with 2-bilayer G/Ag NWs electrode showed a lower PCE
than that of the device with ITO. A JSC of 7.21 mA cm-2, VOC of 0.52 V, FF of 0.35, and PCE
of 1.30% were obtained for the device with the G/Ag NWs electrode. This situation resulted
from high roughness of G/Ag NWs transparent electrode [48]. The electrical and optical
Fig. 6. (a) Device structure and (b) J-V curves of the devices based on ITO and G/Ag NWs as
the anode.
4. Conclusion
alternative to an ITO transparent electrode using the LBL method in this work. GO thin film
was prepared by spin coating on a functionalized glass substrate. After cysteamine was
grafted to the surfaces of Ag NWs, the Ag NWs were deposited on the GO layer by
electrostatic force using dip coating. Sodium borohydride reduction substantially improved
the film conductivity. Additionally, the GO-Ag NWs hybrid electrode exhibited low sheet
resistance. While a 2- bilayer hybrid film had a transmittance of % 78.2 and a sheet resistance
17
of 6.5 sq-1, a 3-bilayer hybrid film had a transmittance of % 67.3 and a sheet resistance of
4.0 sq-1, which was comparable to ITO. Because of that, the FOM values of the 3-bilayer
(214) and 2-bilayer (218) TCEs were also comparable to that of ITO (297). The P3HT:PCBM
device based on 2-bilayer hybrid film as the anode exhibited PCE of 1.30%, implying that
Acknowledgements
This research was supported by the Technology Development Program to Solve Climate
Changes of the National Research Foundation (NRF) funded by the Ministry of Science, ICT
(113M772).
18
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Supplementary Information
1
Department of Physics, Gebze Technical University, 41400, Gebze, Kocaeli, Turkey
2
Department of Chemistry, Istanbul Technical University, 34469, Maslak, Istanbul, Turkey
3
Department of Chemistry and Research Institute for Convergence of Basic Sciences,
Hanyang University, 04763 Seoul, South Korea
4
Materials Institute, TUBITAK Marmara Research Center (MRC), 41470 Gebze, Kocaeli,
Turkey
5
Next Chemicals & Plastics, 34490, Ikitelli, Istanbul, Turkey
22
Fig. S1. Zeta potential of (a) the GO suspension (as a function of pH) and (b) Ag NWs-NH2.
23
Fig. S2. 2D topological AFM images of (a) GO/Ag NWs and (b) GO/Ag NWs/GO thin film.
3D topological AFM images of (c) GO/Ag NWs and (d) GO/Ag NWs/GO thin film.
24
Graphical abstract
Highly transparent and conductive graphene/Ag NWs hybrid electrode has been successfully
developed by using layer-by-layer method for organic photovoltaic cells as an alternative to
conventional indium tin oxide electrode.
25