Journal Pre-proof

Facile Synthesis of Ag Nanowires Enhanced PVB for Transparent Conductive Film

Fan Zhang, Bo Cheng, Jianping Liu, Yanmin Yue, Zhichao Huang, Yi Zhang,
Dongmian Zang

PII: S2238-7854(20)31876-7
DOI: https://doi.org/10.1016/j.jmrt.2020.10.039
Reference: JMRTEC 2322

To appear in: Journal of Materials Research and Technology

Received Date: 5 August 2020

Revised Date: 2 October 2020
Accepted Date: 6 October 2020

Please cite this article as: Zhang F, Cheng B, Liu J, Yue Y, Huang Z, Zhang Y, Zang D, Facile Synthesis
of Ag Nanowires Enhanced PVB for Transparent Conductive Film, Journal of Materials Research and
Technology, https://doi.org/10.1016/j.jmrt.2020.10.039.

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Facile Synthesis of Ag Nanowires Enhanced PVB for
Transparent Conductive Film
Fan Zhang a,d, Bo Cheng e, Jianping Liu f, Yanmin Yue a, Zhichao Huang a,b,*, Yi Zhang a,c,* and
Dongmian Zang a
a
Department of Polymer Materials and Chemical Engineering, School of Materials Science and Engineering, East
China Jiaotong University, Nanchang, 330013, China
b
Key Laboratory of Vehicle tool and Equipment of Ministry of Education, East China Jiaotong University,
Nanchang, 330013, China
c
School of Energy Sciences and Engineering, Nanjing Tech University, Nanjing, 211816, China
d
Jiangsu Dingsheng Filter Bag Co., Ltd., Yancheng, 224400, China
e
School of Materials Science and Engineering, Henan University of Technology, Zhengzhou, 450001, China

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f
China Certification & Inspection Group Hunan Co., Ltd., Changsha, 410021, China
* Correspondence: hzcosu@163.com (Z.H.); zhangy@njtech.edu.cn, Tel: +86-791-87046425 (Y.Z., https://orcid.

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org/0000-0002-1603-8623)

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Abstract: Transparent conductive films (TCFs) are highly desirable for making full use of solar energy.
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However, the production and application of TCFs are seriously restricted by two obvious weaknesses:
complex processes and poor properties. In this research, simple and direct approaches including
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condensation reflux and hot-pressing are selected to gain a cheap TCF with good properties. The
polyvinyl butyral enhanced by 6 spray layers of Ag nanowires (AgNWs/PVB) TCF is found to achieve an
optical transmittance of 80.1 % and a sheet resistance of 86.4 Ω/sq, and meanwhile, withstand bending
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cycles over 150 and an extensile rate of 15%. Additionally, the AgNWs/PVB TCF has a deep potential to
be further improved by hot-pressing treatment and its sheet resistance can be reduced to 19.7 Ω/sq. Our
findings may show a facile way to produce low-cost and high-performance TCFs.
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Keywords: Transparent conductive film; Ag nanowires; polyvinyl butyral; optical transmittance; sheet
resistance
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1. Introduction
Transparent conductive films (TCFs) have played an indispensable role in the modern manufacturing
and engineering fields, due to the varied applications of optoelectronic devices for photodetectors [1],
functional sensors [2], flexible electronics [3], transparent actuators [4], transparent heaters [5], PM filters
[6]. In the past years, indium tin oxide (ITO) consisted of indium oxide (In2O3) and tin oxide (SnO2) set an
example for good TCFs, relying on its high optical transmittance (> 80 %) and low sheet resistance (< 30
Ω/sq) [7,8]. Together with some cheap and nontoxic alternatives including fluorine-doped tin oxide (FTO)
and aluminum-doped zinc oxide (AZO), ITO is classified as transparent conductive metal oxides which
have greatly promoted the development of optoelectronic devices. However, these inorganic oxide films are
very brittle and seldom associated with fine flexibility (tensile fracture strain < 1 %).
Recent advances in TCFs require not only high transparency and electrically conductivity, but also
high tensile property and long-term cyclic bending. TCFs which can keep their performance with certain

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foldability and elongation are essentially needed to adapt to a complex stress environment, and therefore
increasingly researched towards future markets. 1D nanomaterials (e.g. carbon nanotubes [9], Ag

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nanowires [10], Cellulose nanofibers [11], Copper nanowires [12]), film materials (e.g. graphene [13], Cu-
based ZnO thin films [14]), polymers (e.g. PEDOT:PSS [15], polyethylene furanoate [16]) and their
hybrids have drawn much attention, and many of they are frequently reported as promising materials for
flexible TCFs and very close to commercialization.
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Till now, simple processes, large-scale fabrications and stable properties are still big challenges for
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commercial TCFs. The former two mean a low cost of production, which requests common and mature
synthetic methods for TCFs. While stable properties require reliable structures of TCFs, even under a high
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strain or after repeated bending. Aiming at these challenges, we present Ag nanowires enhanced polyvinyl
butyral (AgNWs/PVB) films with high visible transmission, stretchability and low surface square resistance
for stretchable TCFs by using polyvinyl butyral (PVB) as a polymer substrate and AgNWs as conducting
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networks. We prepare AgNWs via a regular and simple reflux reaction at 150 °C, and obtain AgNWs/PVB
films after a quick ultrasonic spraying process and a hot-pressing treatment. We characterize the
morphology of AgNWs, test the optical transmittance of AgNWs/PVB films, and research the sheet
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resistance change of the films with different AgNWs ratios, extensile rates and bending cycles. The results
suggest an excellent TCF based on AgNWs/PVB with an optical transmittance over 80 % and a sheet
resistance of 86.4 Ω/sq was gained, and the property of this film changed very little with an extensile rate
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of 15 % and bending times up to 150. More importantly, all the operations employed in the research are
commercialized, including flux, centrifugation, ultrasonic spray and hot-pressing between 100 - 200 °C.
Our work shows a parallel to low-cost and scaled up stretchable TCF and benefits a lot to the industry of
transparent electrics.

2. Experimental

2.1. Materials
Silver nitrate (AgNO3, AR) was purchased from Chemical Reagent Co., Ltd, and polyvinyl
pyrrolidone (PVP, AR) was brought from Shanghai Jingchun Biochemical Technology Co., Ltd. Ethylene
glycol (EG, AR) was offered by Shanghai Tongya Chemical Technology Development Co., Ltd. PVB
powder (AR, M.W. 170000 - 250000) was supplied by Aladdin Reagent Co. Ltd. Sodium sulfide dihydrate
(Na2S▪2H2O, AR), acetone (AR) and absolute ethyl alcohol (AR) were provided by Sinopharm Chemical
Reagent Co., Ltd.

2.2. Synthesis of AgNWs

 10 ml EG was poured to a three-necked flask, heated to flux, stirred and kept condensation refluxing
for 5 min. Then a uniform mixture of 0.34 g AgNO3 in 20 ml EG was added into the fluxing EG.
Afterward, 30 ml EG solution containing Na2S▪2H2O (1 mmol/L) and PVP (0.3 mol/L) was dropped into
the flask in 5 min. The reaction system was kept at 150 °C for 35 min and a grey precipitate was obtained.
The precipitate was collected after a centrifugal operation, then washed with acetone, deionized water and
absolute ethyl alcohol for several times.

2.3. Preparation of AgNWs/PVB

PVB films with a thickness of 0.2 mm were obtained by compression molding of PVB powder at 160
°C for 10 min. A suspension of AgNWs dispersed in ethanol (0.25mg/ml) was ultrasonically sprayed onto
the PVB film to form Ag layers using an ultra-coat equipment (Prism300, USI Chemical America, U.S.A.).
After the volatilization of ethanol, AgNWs were attached to the top of the PVB film. Finally, the
AgNWs/PVB composite films were pressed at 100 °C to obtain stable structures.

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2.4. Characterization

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Morphology of AgNWs was characterized by a scanning electron microscopy (SEM, JSM-6360LV,
JEOL co., Japan) and a transmission electron microscopy (TEM, H-800, Hitachi co., Japan). The crystal

Bruker AXS, German).

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structure and chemical component of AgNWs were analyzed with X-ray diffraction (XRD, D2 Phaser,

The sheet resistance and transmittance of AgNWs/PVB films were tested by a Micro-controlled four-
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probe tester (RTS-8, Probes Tech, China) and a UV-VIS spectrophotometer (Cary 3500, Agilent
Technologies, Inc., U.S.A.).
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3. Results and discussion

During the reaction, many factors play important roles in the formation of AgNWs, for example, the
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EG condition, the reduction temperature, PVP : AgNO3 molar ratios, AgNO3 mixture sonication time, PVP
solution dropping rate, magnetic stirring rate. EG decomposes into acetaldehyde during the reflux, which
can assist with the reduction from Ag+ to Ag atoms. Temperature makes great sense to the shape and purity
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of AgNWs. According to Sahin Coskun’s report [17], a temperature low than 110 °C results in micrometer-
sized Ag structures rather than AgNWs, while a temperature higher than 170 °C will lead to AgNWs with
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low aspect ratios. The effect of PVP : AgNO3 molar ratios is similar with the one of the reduction
temperature, too much PVP would stop Ag nanoparticles from growing into AgNWs. Likewise, PVP
solution dropping rate and magnetic stirring rate are also important for the fabrication of AgNWs. Only if
these conditions and synthetic parameters are optimized, can we obtain good AgNW products without
irregular shapes or impurities. Additionally, an appropriate sonication duration of AgNO3 mixture was also
reported as be helpful to reduce the sizes of byproducts [18].
In virtue of the induction of PVP, the Ag atoms linked with each other and grew anisotropically to
form AgNWs. Anion S2- is essential for the formation of AgNW. At the beginning of the reaction, S2-
“deposited” Ag+ in the form of Ag2S gel, which slowed down the reaction of Ag+ and prevented too much
Ag atoms from agglomerating to Ag particles. When most of Ag+ was consumed, Ag2S gel then dissolved
in EG and “released” Ag+ to maintain the reducing reaction [19]. Owing to the strong induction of PVP and
the controlling effect of Na2S, AgNWs were successfully fabricated.
PVP played an essential role in the formation of AgNWs, but would result in entanglements of the Ag
wires. Therefore, the removal of PVP during the collection of AgNW precipitate is necessary. For doing
this, a wash treatment including centrifugation (3000 rpm, 5 min) for 2 times was carried out as mentioned
in Section 2.3.
Ultrasonic spray is an automatic coating technology which can produce films with thicknesses ranging
from 5 to 150 μm. In our experiment, the ultra-coat sprayed droplets of AgNWs and ethanol onto the
surface of a PVB film. When the ethanol evaporated, AgNWs were left in forms of networks. A schematic
diagram of the process from Ag atoms to AgNWs/PVB is illustrated in Figure 1.

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Figure 1. Schematic diagram of the preparation of AgNWs/PVB.
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SEM images of AgNWs are shown in Figure 2a–b. It can be seen that AgNWs with diameters ranging
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from 50 to 120 nm and lengths over 2 μm were obtained. Few bright spots representing Ag nanoparticles
can be observed from Figure 2a–b, manifesting that the formation of AgNWs was completely finished.
XRD spectrum of AgNWs in Figure 2c indicates that the AgNWs are of a highly crystalline multitwinned
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pentagonal structure. Four characteristic peaks locating at 38.22°, 44.54°, 64.64° and 77.56° are assigned to
Ag (111), (200), (220) and (311) lattice planes (PDF#04-0783) [20]. Among the four peaks, the one at
38.22° is the highest, suggesting the preferred growth towards (111) plane [21] under the induction of PVP.
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Figure 2. a) Low resolution SEM image, b) High resolution SEM image and c) XRD curve of AgNWs.
 TEM image of the purified AgNWs in Figure 3a has further confirmed that the Ag product is of a
wirelike shape. Figure 3b provides the image of a monodispersed AgNW, which suggests that typical
AgNWs have a cylindrical appearance and high length-diameter ratios more than 20. The inset in Figure 3b
is the image of AgNW under 2 nm scale bar. The spacing of the twin boundaries labeled by red lines is ca.
0.24 nm, which can be associated with the interplanar distance of the (111) faces [22]. Figure 3c–d show
the EDS mapping and spectrum of AgNWs. No S or O element was detected by EDS, meaning that the
AgNWs synthesized via the refluxing reduction are of high purity.

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Figure 3. a) Low resolution TEM image, b) High resolution TEM image, c) EDS mapping and d) EDS
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spectrum of AgNWs. The inset in 3b) shows the interplanar distance of (111) faces of AgNWs.
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To research the structure of AgNWs enhanced PVB, both schematic diagrams and SEM images are
used to illustrate the morphology of the composite film, as are shown in Figure 4 a–f. Top view on the
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sample (Figure 4a, c and e) shows that there are micrometers AgNWs jointing with each other to generate
crossing points and conductive networks after being sprayed on the film. While cross section image of the
sample (Figure 4b, d and f) suggests some AgNWs imbedded into the film under the pressing operation,
which improved the stability of the AgNWs/PVB films.
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Figure 4. Schematic diagrams of AgNWs/PVB: a) top view observation, b) cross section observation; Low
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resolution SEM images of AgNWs/PVB: c) top view observation, d) cross section observation; High
resolution SEM images of AgNWs/PVB: e) top view observation, f) cross section observation.
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Sheet resistance is one of the most important properties to TCFs. Herein, the resistance of each
AgNWs on PVB film was tested for 5 times by selecting 5 points on the top of each film, and the results are
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listed in Table. 1. For a clear comparison, the average value and standard deviation of each sample are also
included in Table.1. All standard deviation values between 2 to 3 Ω/sq are attributed to the uniform
distribution of AgNWs on PVB films, and less than 10 % of standard deviations in the resistances suggest
the promising accuracy of the resistance values.
 Table 1. Sheet resistances of the AgNWs/PVB films as a function of AgNW spray layers.
sheet sheet sheet sheet sheet average
standard
spray resistance resistance resistance resistance resistance sheet
deviation
layers at point 1 at point 2 at point 3 at point 4 at point 5 resistance
(Ω/sq)
(Ω/sq) (Ω/sq) (Ω/sq) (Ω/sq) (Ω/sq) (Ω/sq)

2 209.5 211.4 205.7 211.6 208.6 209.4 2.15

4 137.5 141.5 139.9 143.6 144.3 141.4 2.48

6 83.4 89.7 85.6 88.2 85.1 86.4 2.26

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8 53.1 55.3 52.9 60.3 58.7 56.1 2.98

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10 39.8 37.3 39.1 32.5 38.6 37.5 2.61

12 27.5 23.2 25.6

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14 24.2 26.9 22.8 20.1 25.3 23.9 2.31
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The average resistance decreased significantly with the increase in the spray layers of AgNWs on
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PVB, namely, the conductive property of the AgNWs/PVB TCF is dependent closely on the amount of
AgNWs. This can be explained with that the AgNWs had been woven to a conductive network in PVB
(also see Figure4a and e), which can greatly improve the conductivity of the composite film. For the TCF,
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12 spray layers led to a decline in sheet resistance low to ca. 24.3 Ω/sq, which is almost 1/9 of the
resistance of the PVB with 2 spray layers of AgNWs embedding. More layers than 12 benefited little to the
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conductive property, as the amount of AgNWs (spray layers of AgNWs in this work) is saturated for a
conductive film.
On the other hand, the spraying of AgNWs on PVB caused obvious reductions in light transmittance
performance from UV to visible range, which is in line with the result of AgNWs on mixed esters of
cellulose membranes (AgNW-MCE) [23]. Spray layers over 8 resulted in a total decrease in transmittance
of more than 20 % (Figure 5a). For a visual comparison, the effects of AgNWs improving the sheet
resistance and weakening the visible transmittance at 460 nm of PVB are illustrated in Figure 5b. It is clear
that the amount of AgNWs is critical to the PVB-based TCF, both too much or too less can result in
performance-hungry issues. For the TCF of 6 spray layers of AgNWs enhanced PVB, it had an average
sheet resistance of 86.4 Ω/sq and an optical transmittance of 80.1%, which are a little lower than previous
transparent conductors. The reasons of these two properties can be stated as follows: First, the PVB film
made by hot-pressing is 0.2 mm thick, which will cause more optical transmittance losses than other TCFs
with very thin substrates or glass substrates. Second, the as-fabricated AgNWs are 2 – 60 μm long and not
as excellent as very-long AgNWs (100 – 500 μm) synthesized by hydrothermal or successive multistep
growth methods for transparent conductive networks [24,25], though short AgNWs are easy obtained and
of better dispersibility than long ones.
To further research the trade-off relationship between transparency and sheet resistance of the TCFs, a
figure of merit [26] is defined by
 =
where T is the optical transmission (transmittance in this work) and Rs is the electrical sheet resistance.
When the visible transmittance at 460 nm, the values of T, T10 and ΦTC of the TCFs can be defined. As are
shown in Table 2, the TCF with 6-layer AgNWs has the highest ΦTC, hinting that this TCF has achieved a
better trade-off between transparency and sheet resistance than the other TCFs.
The bending performance of each AgNWs/PVB was tested to evaluate the flexibility of the film.
Figure 5c displays the change in sheet resistance of the TCFs as a function of bending cycles. For all the
samples, bending cycles less than 100 had a slightly negative effect on the surface conductivity. But once
the bending times over 150, the resistance largened quickly, indicating that the conductivity of
AgNWs/PVB film dropped a lot after many times of bending. As AgNWs are brittle and easily broken after
being folded, the conductive networks often get damaged during the breaking of the wires. Increasing spray
layers of AgNWs can suppress the enlarging effect on the resistance, as more AgNW networks form with
the adding amount of Ag. Overall, most of the samples can bear 150 bending cycles with the resistance

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rising less than 100 Ω/sq.
The tensile property is another parameter to examine the performance of flexible TCF. To investigate

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the tensile property of the AgNWs/PVB films, the relationship between the resistances and the elongations
of the samples is presented in Figure 5d. For the TCFs, an elongation ratio of less than 15 % can hardly
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influence the resistances. This is mainly because AgNWs are slightly crooked (see Figure 4d–e above)
rather than straight after attaching on PVB films, while PVB films are always known as fine flexible
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substances. Crooked AgNWs can endow the TCFs with certain conductivity retention ability. However,
when the elongation rate is more than 15 %, the changes in the conductive properties of the TCFs become
significant, indicating that AgNWs-formed networks are gradually broken. Excessive tensile strength can
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cause serious damage to the conductive property of the TCFs. According to previous researches [27,28],
increasing the length of AgNWs may improve the stretchability of the TCF.
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 Figure 5. a) Transmittance of different AgNWs/PVB TCFs with different AgNW spray layers; b) Sheet
resistances (red line) and transmittances at 460 nm visible light (blue line) of AgNWs/PVB as a function of
Ag spray layer; Sheet resistance of AgNWs/PVB TCFs as a function of c) bending cycles and d) elongation
ratios.

Table 2. Comparison of figure-of-merit ΦTC values for the TCFs as a function of AgNW spray layers.

spray T Rs ΦTC
T10
layers at 460 nm (Ω/sq) (Ω-1)

2 85.4% 20.6% 209.4 9.84×10-4

4 82.6% 14.8% 141.4 1.05×10-3

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6 80.0% 10.7% 86.4 1.24×10-3

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8 71.2% 3.35% 56.1 5.88×10-4

10 65.0%
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1.35% 37.5 3.47×10-4
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12 58.9% 0. 502% 24.3 2.06×10-4
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14 53.9% 0.207% 23.9 8.37×10-5

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The pressing treatment is very important for the TCFs, as this action not only creates a stable structure
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during the formation of AgNWs/PVB films (Figure 4d–f), but also improves the conductive property.
Before a press treatment, AgNWs are conventional random, leading to poor conductive networks on the
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PVB film (Figure 1, the picture in the bottom center) and a high junction resistance [27]. After an effective
pressing, the spatial disordering status of AgNWs was greatly improved, most AgNWs were concentrated
on the top of the PVB film and jointed with each other. Then good conductive networks formed (Figure 1,
the picture in the bottom left corner), reduced the junction resistance of the structure and endowed the TCF
with a much better conductivity.
In order to further improve the conductive property of the TCFs, the pressing treatment was carried
out at different temperatures ranging from 100 - 200°C. For the 6-layer AgNWs enhanced PVB TCF (see
Figure 6a), the increase in hot-pressing temperature had resulted in a down first and then up change in sheet
resistance. This interesting phenomenon can be accounted for by the temperature-caused shape change of
PVB. As is well known, the melting point of PVB is 165 - 185 °C. At low-temperature range (100 - 175
°C), softening PVB acted as an adhesive for AgNW networks, which made the conductive network
complete. This adhesive effect became significant with the temperature rising. However, when the
temperature goes too high (> 175 °C), PVB begins to melt and results in a fall of AgNWs into PVB films
(Figure 4b, d and f), namely, there are fewer AgNW networks existing on the top at a high temperature than
a low temperature. It is noted that a hot-pressing treatment at 175 °C (Figure 6 a) can endow the AgNW
with well-organized distribution like the one in Figure 6 b. As are shown, a low-cost and promising TCF
with a sheet resistance low to 19.7 Ω/sq is gained, despiting of slightly optical transmittance losses (Figure
6 c–d).
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Figure 6. a) Sheet resistances of an AgNWs/PVB film as a function of hot-pressing temperatures;
b) Ideal model of AgNWs enhanced PVB after a hot-pressing;.c) photograph of 6-layer AgNWs enhanced
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PVB via a pressomg at 175 °C and d) details of optical transmittance losses caused by AgNW networks.

4. Conclusion
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To sum up, we have presented the research on the preparation and property of Ag nanowires enhanced
PVB for TCFs. The AgNWs/PVB films are successfully fabricated by employing some simple and
commercial synthesis methods, including ultrasonic spraying AgNWs/ethylene glycol solution on PVB
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film with 0.2 mm thickness. We found that the TCF with 6 spray layers of AgNWs embedding possesses
not only promising optical transmittance (80.1 %) and sheet resistance (86.4 Ω/sq), but also excellent
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bending resistance (up to 150 cycles) and tensile resistance (over 15 % elongation ratios). Importantly,
optimized hot-pressing treatment can enable the sheet resistance of the AgNWs enhanced PVB to further
reduce to 19.7 Ω/sq. This work indicates that AgNWs/PVB can be used for practical TCFs, and probably
better properties (lower resistance and higher optical transmittance) can be achieved after further
optimizing the composite structures (increasing the AgNWs amount or decreasing the PVB thickness),
showing low-cost and economical products for transparent electrics.
Acknowledgments: This research is supported by the National Natural Science Foundation of China (51265012) and
(51565014), Ganpo excellence 555 engineering talents of Jiangxi Province. The authors would like to thank Ms.
Xinyue Huang at Michigan State University for assisting in the English language editing.
Conflicts of interest: There are no conflicts to declare.
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There are no conflicts to declare.

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