Carbon 183 (2021) 809e819

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Carbon
journal homepage: www.elsevier.com/locate/carbon

Research Article

A one-step graphene induction strategy enables in-situ controllable

growth of silver nanowires for electromagnetic interference shielding
Hui Jia a, b, 1, Zong-Lin Yi a, b, 1, Xian-Hong Huang a, Fang-Yuan Su a, Qing-Qiang Kong a, b,
Xiao Yang d, Zheng Wang a, b, Li-Jing Xie a, *, Quan-Gui Guo a, c, **, Cheng-Meng Chen a, c, ***
a
CAS Key Laboratory of Carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan, 030001, China
b
University of Chinese Academy of Sciences, Beijing 100049, China
c
Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
d
School of Electronic Science and Engineering,Fujian Engineering Research Center for Solid-State Lighting, Xiamen University, Xiamen 361005, China

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

Article history: The introduction of silver nanowires (AgNWs) with high electrical conductivity into graphene skeletons
Received 20 May 2021 significantly enhances its electromagnetic shielding performance. However, the complicated procedures
Received in revised form and low yield of the AgNWs preparation and the lack of strong interaction between graphene and
1 July 2021
AgNWs by physical self-assembly method limits the electromagnetic shielding application. Herein, a
Accepted 24 July 2021
Available online 28 July 2021
one-step graphene induction strategy without other nucleating and morphology agents of halide ion is
exploited for the in-situ synthesis graphene/AgNWs composite. The O¼CeO groups of graphene provide
a nucleation site to combine Ag nucleus. Importantly, graphene with oxygen functional groups acts as an
Keywords:
Graphene induction strategy
“Agþ pool” to store and release abundant Agþ, supplying consecutively Agþ for AgNWs growth and
In-situ silver nanowires growth inhibiting excessive nucleation. Benefiting from the high ohmic loss of 3D conductive network, the
Nucleation mechanism resulting graphene/AgNWs coating exhibits remarkable electromagnetic shielding effectiveness of
Electromagnetic interference shielding 76.59 dB. This provides a broad prospect for the as high-performance electromagnetic shielding
materials.
© 2021 Elsevier Ltd. All rights reserved.

1. Introduction and silver nanowires (Ag NWs) [12,13].

Electromagnetic radiation and interference have become very
severe in high-precision, integrated, and miniaturized electronic
devices due to the development of artificial intelligence, industry
4.0, and the fifth-generation (5G) communication [1]. Especially,
the issues of electromagnetic interference (EMI) between different
devices urgently require to be addressed [2]. To this end, the design
of high-performance, low-density, and ultra-thin EMI shielding
materials is highly desired. Currently, commonly used EMI shield-
ing materials are divided into two types of carbon-based shielding
blocks including carbon black [3], carbon nanotubes [4,5], gra-
phenes [6,7], graphite [8], and metal-based shielding blocks
including iron and iron oxides, MXene [9e11], copper nanowires,
Among carbon-based materials, graphene, composed of the ar-
omatic ring with hybridized sp2 carbon atoms, has attracted
extensive attention for an EMI shielding material owing to its
outstanding electrical conductivity, low density, easy processing,
and corrosion resistance. Besides, graphene with an intrinsic 2D
sheet structure as building units can self assembly into for the EMI
shielding 3D macroscopic, such as films [14], aerogels [15], macro-
fiber [16]and coatings [17]. Shen et al. prepared an ultra-thin
graphitized graphene film with a thickness of 8.4 mm, and its EMI
shielding effectiveness (SE) can reach 20 dB [18]. The carbon hon-
eycomb/graphene foam reported by Yuan et al. exhibits an EMI SE
of 43 dB with ~5 mm in thickness [19]. These results show that
graphene has great potential for EMI shielding application.

* Corresponding author.
** Corresponding author. CAS Key Laboratory of Carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan, 030001, China.
*** Corresponding author. CAS Key Laboratory of Carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan, 030001, China.
E-mail addresses: xielijing@sxicc.ac.cn (L.-J. Xie), qgguo@sxicc.ac.cn (Q.-G. Guo), ccm@sxicc.ac.cn (C.-M. Chen).
1
Hui Jia and Yi Zong-Lin contributed equally to this work.

https://doi.org/10.1016/j.carbon.2021.07.067
0008-6223/© 2021 Elsevier Ltd. All rights reserved.
H. Jia, Z.-L. Yi, X.-H. Huang et al.
However, there are still several problems of full carbon material due
to the poor ohmic loss from limited electrical conductivity, such as
relatively low EMI shielding performance and large thickness,
which do still not satisfy the demand for miniaturized electronic
devices.
In response to the above issues, AgNWs are the preferred choice
for the enhancement of EMI shielding of carbon-based materials
due to the ultra-high electrical conductivity and intrinsic 1D linear
structure to construct the ultra-thinness 3D conductive network
[20,21] Thus, the introduction of AgNWs can help graphene-based
EMI shielding materials to enhance the ohmic loss [22,23]. Simul-
taneously, the Ag NWs can also form heterojunction with 2D gra-
phene to contribute polarization loss. Given these advantages, the
graphene/Ag NWs composite stimulated the huge interest of many
researchers as an attractive EMI shielding material. For example, a
flexible graphene oxide/Ag NWs film possesses an extremely high
EMI SE of 92 dB with a thickness of 18 mm [14]. Our previous work
has also fabricated a multilayer graphene oxide/Ag NWs film. The
resulting film exhibited remarkable EMI shielding performance of
62 dB and a thickness of merely 8 mm [24]. Notably, the thickness
was distinctly reduced, and the EMI shielding performance was also
greatly improved compared to full carbon-based materials.
However, the typical path of the Ag NWs preparation is the
polyol method [20], which still presents many challenges for large-
scale synthesis, such as the low yield, precise preparation and
complex purification procedures for the removal of introduced
AgNPs impurity [25e28]. Moreover, the as-prepared Ag NWs re-
quires to further assemble with graphene by the physical mixing to
obtain graphene/AgNWs composite, which lacks a strong combine
interaction between Ag NWs and graphene.
Herein, a one-step graphene inducted strategy without other
nucleating and morphology agents of halide ion was exploited for
in-situ controllable synthesis of Ag NWs. In the synthesis process,
the effect of the graphene inducers was investigated by the com-
bined experimental and theoretical calculations. The nucleation
and growth mechanism of Ag NWs were elucidated by HR-TEM.
Based on the structure advantages, the EMI shielding perfor-
mance of graphene/Ag NWs composites coatings were explored
and the demonstration application in the 5G mobile phone was
implemented. Finally, the relationship among preparation method,
structure, and EMI shielding performance was established. The
work provides a new path for the large-scale preparation of gra-
phene/Ag NWs EMI shielding materials.
2. Experimental section
2.1. Materials
Graphene with different types (G400 and G3000) was obtained
from the Institute of Coal Chemistry Chinese Academy of Sciences.
Polyvinyl pyrrolidone (PVP, K30 Mw ¼ 58000) and Ethylene glycol
(EG, purity >99 %) were purchased from Tianjin Guangfu Chemical
Research Institute and Sinopharm Chemical Reagent Co., Ltd,
respectively. Silver nitrate (AgNO3, purity >99 %) was bought from
Tianjin Fengchuan Chemical Reagent Technologies Co., Ltd. All re-
agents are not purified before use.
2.2. Synthesis of graphene/Ag NWs and graphene/Ag NPs
composites
Graphene-induced growth of Ag NWs and Ag NPs was imple-
mented via a one-step hydrothermal route. Firstly, 300 mg PVP and
200 mg Ag NO3 were mixed and poured into the container with
30 ml Ethylene glycol (EG) solution. Then, 20 mg G400 graphene
was added to the system. Subsequently, the mixture was
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Carbon 183 (2021) 809e819
continuously stirred overnight (around 10 h) under 600 rpm to
obtain a homogeneous dispersion. Stopping stirring, the suspen-
sion was transferred to a Teflon autoclave and heated to 160  C to
maintain for 8 h. Finally, the mixture was filtered and washed
several times to obtain the G400 graphene/Ag NWs (G400/Ag)
composite. Similar to the steps above, G3000 graphene/Ag NPs
(G3000/Ag) was prepared by replacing the G400 graphene inducer
with G3000 graphene. In contrast, no adding any graphene inducer
system was carried out by the same procedures, and the corre-
sponding pure Ag NPs were synthesized.
2.3. Preparation of graphene/Ag NWs and graphene/Ag NPs coating
The coating was prepared by two steps, including vacuum-
assisted self-assembly and mechanical pressing. Firstly, the as-
obtained G400/Ag power (80 mg) was dispersed in the aqueous
solution with a concentration of 3 mg/ml. Afterward, the aqueous
was poured into the vacuum equipment using filter paper (0.45 mm
in pore size) to prepared graphene/Ag NWs coating. Secondly, a
dense graphene/Ag NWs coating was fabricated by a further me-
chanical pressing procedure under a pressure of 20 MPa for 5 min.
Similarly, a comparative sample of graphene/Ag NPs coating was
manufactured via the above same procedures.
2.4. Characterization
The micro-morphology was recorded by a high-resolution
transmission electron microscopy (HR-TEM, JEM-2100F, Japan)
and a field emission scanning electron microscope (SEM, JSM-
7900F, Japan) at 10 kV. The crystal phase was analyzed using an
X-ray diffractometer (XRD, D8 ADVANCE A25, Cu Ka, l ¼ 0.154 nm,
Germany) with a scanning rate of 8 /min. The local Plasmon reso-
nance was studied by a UVevis diffuse absorption spectroscopy
(Shimadzu Lambda 650, Japan) in the wavelength range from 200
to 800 nm. A thermogravimetric analyzer (TGA, STA449F3,
Netzsch) was employed to investigate the yield of Ag NWs and Ag
NPs with temperatures from 40 to 800  C under the air atmosphere.
The oxygen content of graphene and binding energy changes of the
composite were investigated by an X-ray photoelectron spec-
trometer (XPS, Thermo scientific ESCALAB 250 Xi, America). To
clarify the ability of graphene to adsorb Agþ, the Zeta potentials of
mixed solution were tested using a Malvern Zetasizer nano (ZS90,
UK) with a concentration of 2 mg mL1. The electrical conductivity
of the graphene/Ag NWs coating was measured by a four-point
probe resistivity measurement system (RTS-9, China). A vector
network analyzer was employed to test the EMI scattering pa-
rameters (S11, S21, S12, and S22) of shielding coating at a thickness of
~10 mm, which was used to calculate EMI SE according to the
following equation (1)-(6) [24,29].
R ¼ jS11 j2 (1)
T ¼ jS21 j2 (2)
A¼1  T  R (3)
1R 1  jS11 j2
SEA ¼ 10 logð Þ ¼ 10 logð Þ (4)
T jS21 j2
1 1
SER ¼ 10 logð Þ ¼ 10 logð Þ (5)
1R 1  jS11 j2
H. Jia, Z.-L. Yi, X.-H. Huang et al.
SET ¼ SEA þ SER þ SEM (6)
Where SEA, SER, and SEM correspond to absorption, reflection,
multiple-reflection shielding effectiveness, which is described by
decibel (dB) as a unit. The corresponding R, T and A are reflection
coefficient, transmission coefficient, and absorption coefficient,
respectively. Moreover, when the total shielding effectiveness (SET)
is above 15 dB, the SEM can be ignored.
2.5. Computational methods
Spin-polarized density functional theory (DFT) calculations
were conducted using the Vienna ab initio Simulation Package
(VASP) 5.4 [30]. The generalized gradient approximation (GGA)
using the Perdew-Burke-Ernzerhof (PBE) exchangecorrelation
function was chosen as the exchangecorrelation interaction
[31]. The frozen-core projector augmented wave (PAW) method
was applied to describe the ionelectron interactions [32]. The
effect of dispersion was included by the empirical correction
scheme of Grimme (DFT-D3) [33]. A 3  3  1 and 9  9  1 g k
grids were used for structural optimization and self-consistent field
(SCF) calculations in DFT, respectively. The electron wave functions
were expanded on a plane wave basis with an energy cut off of
450 eV. The convergence criteria of maximum force less than
0.04 eV/Å and energy changes less than 1  107 eV were
employed. Different oxygen-containing functional groups were
constructed on zigzag edged graphene nanolayers. Edged carbon
atoms were saturated with hydrogen atoms.
3. Results and discussion
3.1. Synthesis and morphology of graphene/Ag NWs/and graphene/
Ag NPs
The Ag NWs and Ag NPs were in-situ controllable fabricated via
a graphene-induced method as described in Fig. 1a. The AgNO3 acts
as an Ag þ source, and the graphene of G400 and G3000 served as
the inducers. In the growth process, no other nucleating agent and
morphology control agent of halide ion was introduced. All re-
agents were added for the one-pot reaction without precise control
of adding rate and order. The as-obtained G400/Ag and G3000/Ag
composites solution exhibits black and clay gray, respectively. In
the XRD pattern (Fig. 1b), five typical peaks of (111), (200), (220),
(311), and (222) appear in the pure Ag NPs, G400/Ag and G3000/Ag
composite, indicating that the Ag NWs and Ag NPs crystal are the
face-centered cubic phase. From the UVevisible extinction spectra
(Fig. 1c). The G400/Ag exhibits two peaks at 387 nm and 342 nm,
which are attributed to longitudinal and lateral surface plasmon
resonance of Ag NWs. In the G3000/Ag and pure Ag NPs, only one
plasmon peak appears at 422 nm caused by the surface plasmon
resonance of Ag NPs [26,34]. The yield of Ag NWs and Ag NPs was
investigated in the G400/Ag and G3000/Ag composite by TG anal-
ysis,. It can be seen that the content of obtained Ag2O under the air
atmosphere is 78.03 % and 76.77 %, respectively (Fig. 1d). After
calculating by chemical reaction: 4Agþ O2¼ 2Ag2O, the yield of Ag
NWs and Ag NPs are 72.8 % and 71.6%, respectively (Fig. 1e), which
indicates that the graphene induced growth strategy possesses a
controllable synthesis and high-yield characteristics.
The morphology shows that G400/Ag composite contains a large
number of Ag NWs (Fig. 2aeb), which further demonstrates the
high-yield characteristics. From the macro-morphology, the Ag
NWs are distributed between the graphene sheets (red arrow in
Fig. 2b), which connects the graphene to form a continuous 3D
conductive network. From the micro-morphology, the Ag NWs
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Carbon 183 (2021) 809e819
exhibit a semicircular top (Fig. 2c) [35]. The elemental mapping
reveals that the Ag NWs achieve uniform distribution in the G400/
Ag composite (Fig. 2d). When G3000 graphene act as a growth
inducer, plenty of Ag NPs are generated (Fig. 2e and f). Almost all Ag
NPs are attached homogeneously to the surface of G3000 graphene
(Fig. 2h), and the diameter of Ag NPs is close to that of pure Ag NPs
(Fig. 2g). The fine structure of Ag NWs was further observed by HR-
TEM. Surprisingly, we found that the grafted-like Ag NWs appear
(Fig. 2i), which has not been reported so far. Moreover, the {111}
twin plane was formed as the Ag NWs grown along with the <111>
crystal direction (Fig. 2j and k). The interplanar spacing of Ag NWs
is about 0.24 nm (inset of Fig. 2k), which is in accordance with the
previous reports [24,36].
3.2. The role of graphene in the nucleation and growth process
The role of graphene is analyzed from two stages of nucleation
and growth. First, the nucleation process is study by HR-TEM at
different temperatures. At 25  C, no Ag nuclei are formed on the
surface of G400 graphene (Fig. 3aec). As heating to 60  C, it is can
be seen that many tiny Ag particles appear on the surface of G400
graphene (Fig. 3def). The diameter of Ag particles is ~2 nm. Yet, no
change was observed on the surface of G3000 graphene (Fig. 3gei).
This result shows that Ag crystal nuclei are formed on the G400
graphene while G3000 graphene cannot induce the formation of
crystal nuclei. As the temperature rise to 120  C, the size of the Ag
nuclei increases (Fig. 3jel). When the temperature reaches 160  C,
the size of the Ag nuclei increases to ~20 nm as crystal seeds
(fig.3meo).
The nucleation difference depends on Agþ concentration and
nucleation sites, which is related to the different structure of G400
and G3000 graphene.To investaget relationship between Agþ
concentration and graphene inducers, the XRD was employed to
study the graphitized structure of graphene (Fig. 4a). The typical
(002) peak of G400 graphene is located at 24.7 while it appears at
26.02 in G3000 graphene. The corresponding interlayer d-
spacing is 0.356 nm and 0.342 nm, respectively. It is obvious that
the interlayer d-spacing of G400 is larger than that of G3000,
which is attributed to the insertion involves massive oxygen
functional groups between the G400 graphene. The oxygen con-
tent of G400 graphene reaches 14.39 %, whereas the oxygen
content of G3000 is nearly negligible from elemental analysis
results (Table S1). For the oxygen functional group type, the FT-IR
manifests that it mainly include CeO (1281 cm1) and C¼O
(1756 cm1) and the content in G400 graphene is markedly higher
than that of the G3000 graphene (Fig. 4b). The results are also
further verified by UVevis spectroscopy. In the G3000 graphene,
there are two peaks at 270 nm and 384 nm, which is due to the n-
p* electronic transition of the CeO and the strong conjugated p-
electronic structure from the sp2 hybrid carbon aromatic ring
(Fig. 4c). Compared to G3000 graphene, the n-p* electron tran-
sition peak of the CeO of G400 graphene is red-shifted to 281 nm,
and the peak at 384 nm disappears completely [37]. This indicates
that the presence of abundant oxygen functional groups on the
G400 graphene surface destroys the conjugated p-electronic
structure. Thus, these electron-rich oxygen functional groups of
G400 graphene endows the surface negative charge property.
Meanwhile, the G400 graphene has a high specific surface area of
612.31 m2/g, which is 6 times that of G3000 graphene (Fig. 4d).
Based on the huge specific surface area and negativity charge
surface of the G400 graphene, it is speculated that each G400
graphene sheet can absorb the Agþ, which is like a tiny “Agþ pool”
to store the Agþ for controlling Agþ concentration during the
nucleation.
H. Jia, Z.-L. Yi, X.-H. Huang et al. Carbon 183 (2021) 809e819

Fig. 1. Illustration of fabrication procedure of Ag NWs and Ag NPs induced by graphene (a). XRD patterns (b) and UVevis absorption spectra (c) of pure Ag, G400/Ag, and G3000/Ag.
TG patterns (d) and Ag content (e) in G400/Ag and G3000/Ag. (A colour version of this figure can be viewed online.)

Fig. 2. SEM images of G400/Ag (aeb) and Ag NWs locally enlarged (c) at different magnifications. Elemental mapping (d) of G400/Ag. SEM images of G3000/Ag and pure Ag (g) at
different magnifications. Elemental mapping (h) of G3000/Ag. High-resolution TEM images of G400/Ag (iek). (A colour version of this figure can be viewed online.)

To monitor the effect of the absorb the Agþ, the zeta potentials higher than that of G3000/Ag NO3 (4.79 mV) and pure Ag NO3
of three mixed systems of Ag NO3 and graphene inducer were (1.2 mV), indicating that the G400/Ag NO3 system has high sta-
investigated before the reaction starts. As shown in Fig. 4e, the zeta bility because the graphene adsorbs a large amount of Agþ. In other
potential (23.9 mV) of the G400/Ag NO3 system is significantly words, the formation of the “Agþ pool” was confirmed to store the

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H. Jia, Z.-L. Yi, X.-H. Huang et al.
Fig. 3. High-resolution TEM images of G400 at 25  C (aec), 60  C (d-f), 120  C (j-l) and160  C (m-o) at different magnifications during nucleation process. High-resolution TEM
images of G3000 graphene after 60  C (gei) at different magnifications. (A colour version of this figure can be viewed online.)
Agþ. Furthermore, the “Agþ pool” can control the Agþ concentra-
tion of the system to avoid a mass of nucleation in a short time,
reducing the formation of Ag NPs [38]. Compared to the G400/Ag
NO3 system, G3000/Ag NO3 and pure Ag NO3 system cannot form
the “Agþ pool”, which leads to that nucleation process occurring in
a short time, thereby generating huge amounts of Ag NPs. To
intuitively observe the effect of “Agþ pool”, a series of control ex-
periments of three types were implemented. Before the reaction
starts, we separated the graphene inducers and solutions by
filtering method. In the resulting filtrate, pure AgNO3 and G3000/
AgNO3 exhibited light yellow and red, respectively, indicating that
part of the Agþ has been oxidized to Ag2O particles (Fig. S1a). Note
that G400/AgNO3 filtrate exhibits an initial transparent state, which
means that Agþ is not oxidized. Based on this phenomenon, the
same system was separated at 60  C. Obviously, the filtrate color of
the G3000/AgNO3 and pure AgNO3 has changed to dark red, which
indicates that a lot of the Ag þ has been transformed into Ag2O
particles. However, the G400/AgNO3 mixture still maintains a
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Carbon 183 (2021) 809e819
transparent state, which is ascribed to that G400 graphene as an
“Agþ pool” can absorb substantial Agþ, thereby preventing the
oxidization from Agþ to Ag2O. At 60  C, the Ag content of G400
precipitate is 4.42% (Figs. S1b and c), which indicates that Agþ was
absorbed.
For nucleation site on the surface of G400 graphene, the second
key factor, the oxygen functional groups may be play a key role. The
content and composition of oxygen functional groups were studied
by XPS (Fig. 4f). It can be clearly seen that the O content of G400
graphene far exceeds that of G3000 graphene. The O/C atomic ratio
of G400 graphene is 17.73 %, whereas the content of G3000 is only
1.88 % (Fig. S2). The oxygen species consists of four components:
O¼CeO (531.2 eV), C¼O (531.9 eV), CeO (532.7 eV), and OeH
(533.5 eV) (Fig. 4g h). A significant difference between the two
inducers is that G400 graphene contains O¼CeO (1.709 at.%) while
it does not exist in G3000 (Table S2). Therefore, the O¼CeO group is
likely to be the nucleation site of Ag nucleus. Furthermore, the
binding energy of Ag3d in G400/Ag composite is greater than that of
H. Jia, Z.-L. Yi, X.-H. Huang et al. Carbon 183 (2021) 809e819

Fig. 4. XRD pattern (a), FT-IR spectra (b), UVevis absorption spectra (c), and specific surface area (d) of G400 and G3000. Zeta potential (e) of pure AgNO3, G400/AgNO3, and G3000/
AgNO3 solution. High-resolution XPS spectrum (f) of G400 and G3000. O1s XPS spectrum of G400 (g) and G3000 (h). Ag3d XPS spectrum of pure Ag, G400/Ag, and G3000/Ag
composite (i). Optimized structures of graphene with the O¼CeO (j), C¼O (k), CeO (l), and OeH (m). The values represent the number of charge transfer. Bader charge transfer (n) of
all groups. Charge density difference of Ag atom and graphene with O¼CeO structure (o). Adsorption energy(p) and distance between Ag and O (q) of all groups. (A colour version of
this figure can be viewed online.)

G3000/Ag and pure Ag NPs, which indicates the existence of a
bond-like interaction between the G400 graphene and the Ag NWs.
To clarify the bond-like interaction, the DFT calculations were
conducted. The combining ability between the Ag atom and
different oxygen species were studied. All O¼CeO (Fig. 4j), C¼O
(Fig. 4k), CeO (Fig. 4l), and OeH (Fig. 4m) are constructed on zigzag
edged graphene nanolayers, which are simulated the interaction
with Ag atoms. As shown in Fig. 4n, the sequence of Bader charge
transfer between different functional groups and Ag atoms is
O¼CeO > C¼O > CeO > OeH, which indicates that the O¼CeO
group has a high electron-withdraw ability. The charge density
difference that a significant charge offset appears from Ag atom to
the O¼CeO group (Fig. 4o). Meanwhile, the adsorption energy of
the O¼CeO group is markedly higher than other oxygen functional
groups, which can reach -0.56 eV (Fig. 4p). The resulting distance
between the O and Ag atom is O¼CeO < C¼O < CeO < OeH
(Fig. 4q). The minimum distance of the O¼CeO group is as low as
2.2 Å. These results further demonstrate that the O¼CeO group can
provides a nucleation site. In the nucleation process, the O¼CeO
group has a better combine ability with Ag, which can capture the
Ag NWs crystal nuclei as crystal seeds.
After Ag crystal seeds formation on the G400 graphene, the
AgNWs growth process begins at 160  C. After 60 min reaction,
short Ag nanorods were grown along the <111> crystal direction
(Figs. S3a and c), which indicated that the initial state of Ag NWs
was formed. It is worth noting that the wheat-like Ag NWs appear
(Fig. S3b) because free Ag NPs in the solution is deposited on the
(100) crystal plane of the Ag NWs (Fig. 5aec), which may be due to
the lower surface energy of the small Ag NPs. At this time, the
corresponding diameter of the Ag NWs is 136 nm. After 120 min of
reaction, the content of Ag NWs increases, and it gets became
longer (Figs. S3d and e). The cross-section of the Ag NWs shows a
pentagonal shape (blue circle of Fig. S3f) [39]. A significant change
is that the number of deposited Ag NPs is reduced (Fig. 5d,e and
Fig. S3f). Simultaneously, the deposited AgNPs on the surface of the
Ag NWs becomes thinner (Fig. 5f)which is similar to the Ostwald
ripening process [40,41].After growth of 240 min, the content and
the length of the Ag NWs (Figs. S3g and h) increases significantly.
The size of the deposited Ag NPs on the surface of the Ag NWs is
obviously reduced (Fig. 5i and Fig. S3i). Importantly, the "welding”
phenomenon was observed among multiple short rod-shaped Ag
NWs （Fig. 5g,h and Fig. S3c）, and the notch of the joint site ap-
pears. The formation mechanism is as follows: Due to the growth
along the <111> direction, its will be connected to form notch
defect at the joint sites when two short rods meet. At this time, the
notch has low energy, which is easily deposited by Ag atom to
repair the defect. This mechanism can also explain well the for-
mation of grafted-like Ag NWs. After growth for 360 min, most of

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H. Jia, Z.-L. Yi, X.-H. Huang et al.
Fig. 5. High-resolution TEM images of Ag NWs growth process in 60 min (a-c), 120 min (d-f), 240 min (gei) 360 min (jel) and 480 min (m,n). Equivalent selected area electron
diffraction (SAED) pattern of Ag NWs growth process in 480 min. (A colour version of this figure can be viewed online.)
the Ag NWs have finished growing, and the cross-section exhibits a
semi-circular top (Figs. S3jel and Fig. 5l). The notches caused by the
“welding” process have also been repaired but it still retains
dislocation defects (Fig. 5j and k). After the growth of 480 min, a
large number of Ag NWs were formed (Fig. S3m,n). All the depos-
ited Ag NPs on the surface of Ag NWs disappeared to form a smooth
surface (Fig. S3o and Fig. 5m). In the whole growth process, the
diameter of the Ag NWs rises to 223 nm from 136 nm upon
increasing the growth time from 60 min to 480 min. In the
UVevisible extinction spectrum, the peak at 373 nm red-shifted to
387 nm as the growth time increase, at the same time, a peak
appeared at 480 nm (Fig. S4). A plausible reason for this result could
be the formation of AgNWs as the deposited AgNPs disappear
during the ripening process.
3.3. Induced mechanism of Ag NWs by graphene
Based on the above analysisthe induced AgNWs formation
mechanism is proposed, including three stages: nucleation, growth,
and ripening. In the mixing stage of Ag NO3 and graphene, G400
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Carbon 183 (2021) 809e819
graphene as an “Agþ pool” can adsorb the Agþ by electrostatic
interaction, thereby reducing the concentration of Agþ in the glycol
system (Fig. 6a1). As the system was heated, the nucleation reaction
begins with a low Ag þ concentration according to the chemical
reaction formula (1~3). When the temperature rises to 60  C, the
system is accompanied by the generation of tiny Ag particles with a
diameter of ~2 nm from the supersaturated solution [42,43],
implying that the initial Ag particles were formed. Part Ag particles
are captured by the O¼CeO groups as the Ag nuclei due to the
larger adsorption energy between the O¼CeO groups and the Ag
(Fig. 6a). With heating to 160  C, the diameter of the Ag nuclei
gradually increases to ~20 nm. At this time, the final crystal seeds
are formed.
4Ag NO3/4Ag þ4NO2þ2O2 (1)
2HOCH2CH2OH/2CH3CHO þ2H2O (2)
2Agþ þ2CH3CHO/CH3CHOeOHCCH3þ2Agþ2Hþ (3)
H. Jia, Z.-L. Yi, X.-H. Huang et al. Carbon 183 (2021) 809e819

Fig. 6. Schematic showing the proposed nucleation (a), growth (b), and ripening (c) mechanism of Ag NWs film. (A colour version of this figure can be viewed online.)

Fig. 7. Digital photos of G400/Ag coating (a-a4). SEM images of G400/Ag (b,c) and G3000/Ag coating (d,e) at different magnifications. Areal density (f), carrier mobility, and carrier
concentration (g) of G400/Ag and G3000/Ag coating. SET (h), SER(i), SEA(j), and T (k)of G400/Ag and G3000/Ag coating in X-band. (A colour version of this figure can be viewed
online.)

816
H. Jia, Z.-L. Yi, X.-H. Huang et al.
In the growth stages, the Ag NWs grow along the <111> crystal
direction from Ag crystal seeds by accumulating of Ag atom,
resulting in a length increase of the Ag NWs (Fig. 6b) [44]. In the
process, the Ag atoms are derived from the “Agþ pool” through the
following steps. First, Agþ are desorbed from the “Agþ pool” to
become free Agþ due to the presence of a large Agþ concentration
difference caused by the consumption of Agþ during the growth.
Subsequently, the free Agþ are reduced to Ag0 at 160  C by the
reaction formula (2-3), depositing on the (111) plane (Fig. 6b1)39.
Meanwhile, many free Ag NPs are deposited on the surface of Ag
NWs, resulting in the formation of initial wheat-like Ag NWs. With
the growth time increase, the deposited Ag NPs gradually de-
creases. At the end of growth, the deposited Ag NPs have dis-
appeared and the Ag NWs surface becomes smooth, which is called
the ripening process (Fig. 6c).
3.4. EMI shielding performance of G400/Ag NWs and G3000/Ag NPs
film
On the basis of the advantages of the 3D network constructed
from 1D Ag NWs and 2D graphene, the EMI shielding coatings were
prepared by vacuum-assisted self-assembly and further mechanical
pressing. The thickness of the coating is ~10 mm. We cut the G400/
Ag composite coating into 4  1.5 cm rectangular strips (Fig. 7a),
which can endure being bent, rolled, twisted, and folded without
the composite falling off (Fig. 7a1-a4). The shilding coating exhibits
high flexibility and adhesion properties. The microstructure of
G400/Ag was observed as displayed in Fig. 7b. It shows a dense
Fig. 8. Demonstration diagram of mobile phone signal before (a) and after (b) G400/Ag coating shielding. SET (c), SER(d), SEA(e) and T(f) of G400/Ag and G3000/Ag coating in
3.94e5.99 GHz frequency range (belongs to 5G frequency). (A colour version of this figure can be viewed online.)
817
Carbon 183 (2021) 809e819
surface, and the island-shaped graphene is connected by 1D Ag
NWs to form a continuous 3D network (Fig. 7c). However, G3000/
Ag composite coating shows pores and gaps among the graphene
because the AgNPs are adsorbed on the graphene. Besides, the areal
densities of G400/Ag and G3000/Ag NPs coatings are 3.42 mg/cm2
and 4.22 mg/cm2, respectively (Fig. 7f), indicating that the G400/Ag
have a relatively low density.
Ohmic loss is an important attenuation factor in the EMI
shielding process for conductive EMI shielding materials. In the
graphene and Ag NWs (or Ag NPs) composite, electron migration is
the basic unit for ohmic loss. Thus, the carrier concentration and
carrier mobility of the two coatings were measured. As shown in
Fig. 7g, the carrier mobility of G400/Ag is 4.6 times higher than that
of G3000/Ag. Simultaneously, the carrier concentration of G400/Ag
is 8.334  1022 cm3, which is far more than that of G3000/Ag. This
can endow G400/Ag with the high electrical conduction capability.
The following electrical conductivity of the G400/Ag and G3000/Ag
coatings are 2329.67 S/cm and 369.95 S/cm, respectively (Fig. S5).
According to Simon's formula (7), the high electrical conductivity
implies an excellent EMI shielding performance [9].
s pffiffiffiffiffi
SE ¼ 50 þ 10 logð Þ þ 1:7t sf (7)
f
(where s and f represent the electrical conductivity and frequency,
respectively, and t represents the material thickness.)
As shown in Fig. 7h, the EMI SE of G400/Ag coating is as high as
76.59 dB while the EMI SE of G3000/Ag coating is 46.06 dB in X-
H. Jia, Z.-L. Yi, X.-H. Huang et al.
band, which has satisfied the commercial standard requirement of
20 dB. Simultaneously, this value also far outperformed our previ-
ous reported value of 35.7 dB from the graphene/Ag NWs film
prepared by the merely physical mixing method [24]. According to
formula (6), the SET is composed of SEA and SER. In Fig. 7i and j, it
can be observed that SER is lower than SEA Thus, for G400/Ag and
G3000/Ag, the difference of EMI shielding performance mainly
comes from the contribution of SEA, which the SEA of G400/Ag is
significantly higher than G3000/Ag (Fig. 7j). From the transmission
coefficient (T) in Fig. 7k, G400/Ag coating is can block the electro-
magnetic wave (EMW) energy of 99.999998 %, which suggests that
it has brilliant EMI shielding ability.
The high EMI shielding performance of G400/Ag mainly comes
from the following two aspects. First, the constructed 3D conduc-
tive network by 1D Ag NWs and 2D graphene provide a fast elec-
tron transfer channel. Meanwhile, G400/Ag coating has a super
high intrinsic carrier concentration and mobility. Under the exci-
tation of high-frequency electromagnetic wave, a surface current
can be generated inside the structure, which can contribute to a
high ohmic loss. Second, the presence of nucleation sites of G400/
Ag NWs will contribute to a heterogeneous interface between Ag
nucleus and the O¼CeO of G400 graphene in the growth process,
which will cause the accumulation of electrons under high-
frequency electromagnetic fields. The process leads to the inter-
face polarization loss to attenuate electromagnetic wave energy,
which is the idiographic advantage of the in-situ growth strategy
compared to the graphene oxide/Ag NWs fabricated by physical
self-assembly. To further illustrate the EMI shielding effect of the
G400/Ag composite coating, we covered the EMI shielding coating
on the signal receiving position of the 5G mobile phone (Huawei
Honor). In Fig. 8a, the 5G new radio (NR) signal strength of the
mobile phone is 97 dBm and 43 asu (alone signal unit) before
shielding. After shielding by the G400/Ag NWs coating, the phone
exhibits no 5G NR signal strength (Fig. 8b). To specifically evaluate
the ability of 5G, the electromagnetic shielding performance is
tested. As shown in Fig. 8c, the results show that the G400/Ag
coating exhibits excellent electromagnetic shielding effectiveness
(>57.1 dB) in 3.94e5.99 GHz. The maximum EMI SE can reach
66.2 dB, which is 2 times higher than that of G2800/Ag coating.
Similarly, the main contribution of electromagnetic shielding per-
formance comes from SEA (Fig. 8e) rather than SER(Fig. 8d).
Transmission rate of electromagnetic wave energy is below
0.000019% (Fig. 8f), indicating that it has superior shielding ability
of electromagnetic radiation from 5G frequency range.
4. Conclusion
A one-step controllable in-situ growth of Ag NWs and Ag NPs
strategy was developed without other nucleating agents and
morphology agent of halide ion. The growth inducers of Ag NWs
and Ag NPs correspond to G400 and G3000 graphene, respectively.
By experimental and DFT theoretical calculations, the O¼CeO
group of G400 graphene provide the nucleation sites. Compared to
G3000 graphene, the G400 graphene can act as an “Agþ pool” to
store the Agþ, avoiding excessive nucleation and providing a
continuous Ag source for the growth of Ag NWs. Subsequently, an
Ag NWs formation mechanism was proposed with graphene-
induced nucleation, growth and ripening. At last, the distinctive
structure advantage from the 3D conductive network endows the
G400/Ag NWs coating with high electrical conductivity of
2329.67 S/cm and excellent EMI SE of 76.59 dB. This work provides
a comprehensive explanation of controllable metal nanomaterials
synthesis as high-performance EMI shielding materials.
818
Carbon 183 (2021) 809e819
CRediT authorship contribution statement
Hui Jia: Investigation, Formal analysis, Data curation, Writing e
original draft, Writing e review & editing, Validation, Methodology,
Software. Zong-Lin Yi: Investigation, Formal analysis, Data cura-
tion, Validation, Methodology, Software. Xian-Hong Huang:
Funding acquisition, Project administration. Fang-Yuan Su: Inves-
tigation, Formal analysis, Methodology. Qing-Qiang Kong: Re-
sources, Writing e original draft, Formal analysis, Writing e review
& editing, Project administration. Xiao Yang: Resources, Writing e
original draft, Formal analysis. Zheng Wang: Investigation, Formal
analysis, Methodology. Li-Jing Xie: Writing - Original Draft, Writing
e review & editing, Project administration, Funding acquisition.
Quan-Gui Guo: Funding acquisition, Project administration.
Cheng-Meng Chen: Conceptualization, Resources, Project admin-
istration, Supervision, Funding acquisition.
Declaration of competing interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
Acknowledge
This research was supported by the National Science Foundation
for Excellent Young Scholars of China (21922815), Research and
Development Project of Key Core and Common Technology of
Shanxi Province (20201102018), Key Research and Development
(R&D) Projects of Shanxi Province (201903D121180), Key Research
and Development (R&D) Projects of Shanxi Province
(201903D121007), Industrialization Technology of Graphene
Conductive Ink (20200716), and Research Project Supported by
Department of Resource and Social Security of Shanxi Province and
was provided technical support by “Ceshigo Research Service
Agency” for VNA, www.ceshigo.com.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.carbon.2021.07.067.
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