Journal of Energy Chemistry 26 (2017) 1276–1281

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Journal of Energy Chemistry

http://www.journals.elsevier.com/
journal-of-energy-chemistry/
journal homepage: www.elsevier.com/locate/jechem

Enhanced cycle performance of Li/S battery with the reduced

graphene oxide/activated carbon functional interlayer
Haipeng Li a, Liancheng Sun a, Yongguang Zhang a,∗, Taizhe Tan b, Gongkai Wang a,∗,
Zhumabay Bakenov c
a
School of Materials Science & Engineering, Research Institute for Energy Equipment Materials, Hebei University of Technology, Tianjin 300130, China
b
Synergy Innovation Institute of GDUT, Heyuan 517000, Guangdong, China
c
Nazarbayev University, Institute of Batteries LLC, 53 Kabanbay Batyr Avenue, Astana 010000, Kazakhstan

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

Article history: The high-energy lithium/sulfur (Li/S) battery has become a very popular topic of research in recent years
Received 2 July 2017 due to its high theoretical capacity of 1672 mAh/g. However, the polysulfide shuttle effect remains of
Revised 1 September 2017
great concern with a great number of publications dedicated to its mitigation. In this contribution, a
Accepted 1 September 2017
three-dimensional (3D) reduced graphene oxide/activated carbon (RGO/AC) film, synthesized by a sim-
Available online 15 September 2017
ple hydrothermal method and convenient mechanical pressing, is sandwiched between the separator and
Keywords: the sulfur-based cathode, acting as a functional interlayer to capture and trap polysulfide species. Con-
Lithium/sulfur battery sequently, the Li/S cell with this interlayer shows an impressive initial discharge capacity of 1078 mAh/g
Shuttle effect and a reversible capacity of 655 mAh/g even after 100 cycles. The RGO/AC interlayer impedes the move-
Functional interlayer ment of polysulfide while providing unimpeded channels for lithium ion mass transfer. Therefore, the
Reduced graphene oxide/activated carbon RGO/AC interlayer with a well-designed structure represents strong potential for high-performance Li/S
composite
batteries.
© 2017 Science Press and Dalian Institute of Chemical Physics, Chinese Academy of Sciences. Published
by Elsevier B.V. and Science Press. All rights reserved.

1. Introduction synthesis processes, which restrict the application of Li/S batteries

With the rapid development of electrical vehicles and portable
electronic devices, rechargeable batteries are presented with an
increasing demand of high energy and high power density [1,2].
Lithium/sulfur (Li/S) batteries have become a promising candidate
due to its high theoretical specific capacity of 1675 mAh/g and
its high energy density of 2600 Wh/kg [3]. Additionally, low cost,
environmental benignity, and natural abundance of sulfur offer
the opportunity for a significant cost reduction of energy storage
[4–6]. Despite of these advantages, poor conducting nature of ele-
mental sulfur, polysulfides dissolve into organic electrolyte, causing
low utilization of sulfur and poor cycle performance [4–6].
Recently, much efforts and improvements have been made to
overcome these challenges, such as optimization of the organic
electrolyte [7,8], the synthesis of sulfur hybrid structures with
porous conductive materials [9–12], and the modifications of sep-
arators [13–16]. In spite of the improved utilization of active ma-
terial, the various solutions all contain complicated and elaborate
∗
Corresponding authors.
E-mail addresses: yongguangzhang@hebut.edu.cn (Y. Zhang),
wang.gongkai@hebut.edu.cn (G. Wang).
[17]. Another promising strategy is the implementation of a func-
tional film as a polysulfide-trapping interlayer between sulfur cath-
ode and the separator which has attracted lots of recent research
interest. There have been several investigations on the develop-
ment of a functional interlayer for the Li/S battery system, such
as carbon [18–20], polymer [21,22], and metal oxide based inter-
layers [23]. The introduction of a propitious interlayer not only can
enhance the utilization of active materials, but can also trap the
polysulfides at the cathode side. In addition, the advantage gained
by employing interlayers has huge potential in achieving commer-
cial Li/S batteries. In the work of Manthiram et al. [21], a polyethy-
lene glycol-supported microporous carbon was synthesized by the
slurry coating method as an interlayer for Li/S batteries, which
works as an upper current collector to facilitate electron transport
for enhancing the electrochemical utilization of sulfur and for trap-
ping polysulfides.
Graphene has become a popular material in Li/S battery due
to its unique properties, such as excellent electrical conductiv-
ity, chemical stability, abundant specific surface area and flexi-
ble mechanical strength [24–26]. These advantages indicate that
graphene is a good candidate as a functional interlayer for enhanc-
ing the performance of Li/S batteries. For example, Zhang et al. re-

http://dx.doi.org/10.1016/j.jechem.2017.09.009
2095-4956/© 2017 Science Press and Dalian Institute of Chemical Physics, Chinese Academy of Sciences. Published by Elsevier B.V. and Science Press. All rights reserved.
 H. Li et al. / Journal of Energy Chemistry 26 (2017) 1276–1281
ported that a ternary-layered separator of polypropylene/graphene
oxide/nafion was synthesized via a facile vacuum filtration of GO
sheets onto the macroporous PP membrane, followed by the subse-
quent depositing of an ultra-thin electrostatically repulsive Nafion
layer [14]. The resulting ternary-layered separators are effective in
improving the capacity and the coulombic efficiency of Li/S cells.
Herein, we present a facile preparation of a three-dimensional
(3D) reduced graphene oxide/activated carbon (RGO/AC) interlayer
through simple hydrothermal synthesis and convenient mechani-
cal pressing. The introduction of activated carbons effectively miti-
gates the restack of graphene while also serving as anchors points
from which the graphene nanosheets are pinned around them. The
RGO/AC films sandwiched between the cathode and the separator,
show a highly porous network structure and exhibit promising im-
provement for Li/S batteries. We have shown that the introduc-
tion of a RGO/AC interlayer promotes the adsorption of dissolved
lithium polysulfides and improves the reutilization of entrapped
active materials which led to Li/S batteries with high capacity re-
tention and excellent cycle stability.
2. Experimental
2.1. Material synthesis
Graphene oxide (GO) was synthesized from nature graphite us-
ing the modified Hummers method [27]. GO was dispersed in DI
water by sonication for 1 h and centrifuged at 30 0 0 rpm for 30 min
to remove any aggregates.
The activated carbon (AC) with an abundant surface area of
1600 m2/ g was modified by strong oxidizing agents and strong acid
[28]. The activated carbons (150 mg) were slowly added into the
mixture of concentrated H2 SO4 /HNO3 (3:1) (30 mL) and sonicated
in ultrasonic cleaners for 5 h. After diluting by DI water (400 mL),
the obtained solution followed by vacuum filtration through PVDF
membrane and vacuum drying at 60 °C. Subsequently, 10 mg mod-
ified AC was dispersed in 6 mL GO dispersions (2 mg/mL) by ultra-
sonication for 30 min. Then, with 3 mL 1 M sodium ascorbate aque-
ous solution as reductive agent, the suspension was heated in an
oil bath at 100 °C for 2 h without stirring. The resulting RGO/AC
hydrogel was taken out and washed with deionization water at
60 °C three times to remove any impurities. Finally, the 3D RGO/AC
film was obtained via freezing drying (≤20 Pa, −49 °C) and sim-
ple mechanical compression. Each sample with a diameter of about
20 mm and a thickness of about 0.21 mm was obtained.
2.2. Material characterization
The X-ray diffraction patterns of the as-synthesized samples
were recorded using an X-ray diffraction (XRD, SmartLab, Rigaku
Corporation) with Cu Kα radiation source. The morphological
and microstructure characteristics of the as-synthesized samples
were investigated by scanning electron microscopy (SEM, Hitachi
S-4800) and transmission electron microscopy (TEM, JEM2010F),
respectively. N2 adsorption–desorption isotherm measurement
(V-Sorb 2800P) was performed to analyze the specific surface
and porosities of the samples. Raman spectra were acquired from
a Raman spectroscope (Renishaw RM 20 0 0) with a 632.8 nm
wavelength laser. Thermogravimetric analysis (TGA) was carried
out using a NETZSCH STA-409 PC instrument.
2.3. Electrochemical measurements
The S/PPy composites were prepared in accordance with our
previous reports [29,30]. For sulfur electrodes, the S/PPy compos-
ite, super-P and polyvinylidene fluoride (PVDF) at a mass ratio of
8:1:1 were dissolved in N-methyl-2-pyrrolidone (NMP) to form a
1277
slurry. The above-slurry was cast on an Al foil current collector to
obtain the S/PPy composite cathode, which was then dried in vac-
uum oven at 60 °C for 12 h prior to cutting. 2025-type coin cells
were assembled in an Ar (99.9995%) filled glove box. Lithium foil
was used as anode, the S/PPy electrodes after the cutting (diameter
of 10 mm) was used as cathode, and as prepared RGO/AC interlayer
was put between the cathode and a Celgard 2400 separator. The
areal loading of rGO, activated carbon and sulfur in each electrode
are about 1.5 mg/cm, 2.0 mg/cm− and 4 mg/cm. The electrolyte was
a solution of 1 M LiTFSI in a mixed solution of dimethoxy ethane
and 1,3-dioxolane (1:1 v/v) with 0.1 M LiNO3 as additive. The elec-
trolyte amount of 75 μL was dripped on each side of cathode
and anode, respectively. The cyclic voltammetry (CV) test was in-
vestigated at a scan rate of 0.1 MV/s between 1.0 V and 3.0 V via
a potentiostat (VMP3, Biologic). The discharge/charge cycling per-
formances were carried out between 1.0 V and 3.0 V at different
C rates using a multichannel battery test system (BTS-5V20 mA,
Shenzhen Neware Co. Ltd.). All the measurements were conducted
at room temperature.
3. Results and discussion
The fabrication procedure of RGO/AC film is shown in Fig. 1(a).
GO and AC were mixed through ultrasonication, where the AC suc-
cessfully inserted into the layers of GO. Under the oil bath’s el-
evated temperature, GO transformed into RGO while maintaining
AC embedded in between its graphene sheets. Finally, the RGO/AC
interlayer was obtained via freezing drying and simple mechani-
cal compression, which was observed to possess excellent flexi-
bility. The discharge/charge cycling progress of Li/S battery inside
was displayed in Fig. 1(b). The functional interlayer of RGO/AC was
sandwiched between the separator and an S/PPy cathode, consid-
ered as a polysulfides trap. The introduction of RGO/AC interlayer
can contain the polysulfides species at the cathode side and im-
prove the utilization of the active materials.
The structure and composition of this film is shown in Fig. 2,
the film of RGO/AC sample exhibited two characteristic broad
peaks at around 2θ of 22.8° and 42.8°, which we assigned to
the typical (002) and (100) peaks of graphene, respectively [31].
Activated carbon was introduced into the layer of graphene suc-
cessfully through the ultrasonication. Raman characterization of
RGO/AC films are shown in Fig. 3, which indicates two major peaks
of D band (at 1349 cm−1 ) and G band (at 1567 cm−1 ). The D band
stems from the sp3 defects while the G band corresponds to the
in-plane vibration of sp2 carbon atoms [32]. The intensity ratio of
D band and G band (ID /IG of 1.326) suggested a disorder graphene
structure of the RGO/AC, which indicated that the introduction of
AC into the RGO increased the relative content of sp3 defects and
provided more channels for electron transfer [33].
In order to determine the sulfur loading of S/PPy, thermogravi-
metric analysis was conducted under Ar atmosphere with a heat-
ing rate of 10 °C/min. As shown in Fig. 4, with the temperature rise
during the test, the weight loss curve of the sample can be divided
into two regions. There is a rapid weight loss when the temper-
ature was further increase from 200 to 350 °C. The rapid weight
loss is about 58 wt%, due to that the sulfur in the sample was com-
pletely evaporated. With the continued rise of temperature during
the test, the PPy begins to decompose. Therefore, the amount of
sulfur in the composite could be estimated as about 58 wt%.
As shown in Fig. 5(a), the nitrogen adsorption–desorption
isotherm of the RGO, AC and RGO/AC composites were analyzed at
77 K. It can be seen from these figures that the isotherms display
a typical IV-type curve with type-H3 hysteresis loop, revealing the
hierarchical pore structure associated with meso- and macropores
[34]. The BET surface area of the RGO, AC and RGO/AC composite
were measured to be 261.0 m2 /g, 1508.4 m2 /g and 746.9 m2 /g, re-
1278 H. Li et al. / Journal of Energy Chemistry 26 (2017) 1276–1281

Fig. 1. (a) A schematic showing the preparation of the RGO/AC interlayer. (b) Schematic of a Li/S battery with the RGO/AC interlayer sandwiched between the sulfur cathode
and the separator.

Fig. 3. Raman spectra of the RGO/AC interlayer.

Fig. 2. XRD patterns of the RGO/AC interlayer.

spectively. These pore size distribution curves as shown in Fig. 5(b)

present small size mesopores around 4 nm with a broad macrop-
orous distribution.
The morphologies and microstructures of the as-prepared
RGO/AC films are shown in Fig. 6(a–f) using SEM and TEM elec-
tronic imaging. Fig. 6(a) and (b) show the top-view SEM images of
the RGO/AC films, exhibiting a hierarchically dense structure where
the introduced AC was embedded into the graphene nanosheets.
From the cross-sectional view (Fig. 6(c) and (d)), in the as-prepared
film, the activated carbons play the key roles of reducing the de-
gree of restacking of neighboring graphene nanosheets and effec-
tively connecting graphene nanosheets at different orientations.
The TEM images of the RGO/AC sample as shown in Fig. 6(e) and
(f), demonstrate the construction of graphene with a highly exfoli-
ated morphology and the modified AC distributed into the interior
of RGO structure. Fig. 4. TGA curves of S/PPy composite at a heating rate of 10 °C/min.
 H. Li et al. / Journal of Energy Chemistry 26 (2017) 1276–1281 1279

Fig. 5. (a) N2 adsorption–desorption isotherms; (b) Pore size distribution of RGO/AC, AC and RGO composite. Inset: magnification of pore size distribution between 1 and
10.0 nm.

Fig. 7. CV curves of the Li–S cells with the RGO/AC interlayer.

Fig. 6. (a, b) Top-view SEM images and (c, d) cross-section SEM images of the
RGO/AC interlayer with different magnifications; (e, f) TEM images of the RGO/AC
interlayer with different magnifications.

The electrochemical performance of the S/PPy cathode with the

RGO/AC interlayer was investigated in Li–S batteries. Fig. 7 shows
the cyclic voltammetry (CV) of S/PPy cathode with the RGO/AC in-
terlayer between 1.0 V and 3 V vs. Li+ /Li at the first three scanning
cycle at a scan rate of 0.1 mV.s. During the cathodic sweep, the
peaks at ∼2.3 and ∼2.0 V were assigned to the reduction of el-
ement sulfur (S8 ) to soluble lithium polysulfides (Li2 Sn , 4 ≤ n ≤ 8)
and the eventual formation of insoluble insoluble Li2 S2 and Li2 S,
respectively [35]. In the following anodic scan, the distinct sharp
peak centering at about 2.5 V corresponds to the oxidation of Li2 S Fig. 8. Charging/discharging curves of the Li/S batteries with the RGO/AC interlayer
and Li2 S2 to Li2 S8 [36]. at 0.1 °C.
1280 H. Li et al. / Journal of Energy Chemistry 26 (2017) 1276–1281
Fig. 9. Cycling performance of the cells with and without the RGO/AC interlayer at
0.1 °C.
Fig. 10. Rate capability of the Li/S cells with and without the RGO/AC interlayer at
different current densities.
Fig. 8 shows the galvanostatic charging/discharging curves of
the Li/S batteries with the RGO/AC composite interlayer at a scan-
ning rate of 0.1 °C. It can be seen that two main plateaus ap-
pear in the potential profiles during the discharging process, corre-
sponding to the two-step electrochemical reaction between lithium
and sulfur [37]. The CV also confirms that the RGO/AC interlayer
implemented in the Li/S is not electrochemically active. The first
electrochemical reaction is presented by a short discharge plateau
of about 2.4 V and related to the reduction of elemental S8 into
higher order, soluble lithium polysulfides (Li2 Sn , n ≥ 4). The fol-
lowing prolonged plateau around 2.0 V in the discharge profiles
reflects the subsequent reduction of high order polysulfides into
lower order polysulfides and finally to lithium sulfide Li2 S.
To demonstrate the benefits of the RGO/AC composite inter-
layer on electrochemical performance, a series of electrochemical
measurements were carried out. As illustrated in Fig. 9, the cy-
cling performance is conducted for the cells with and without the
RGO/AC composite interlayer measured at 0.1 °C. The initial dis-
charge capacity of the Li/S cell without the RGO/AC interlayer was
1020 mAh/g, while the cell with RGO/AC interlayer reached a dis-
charge capacity of 1078 mAh/g, corresponding to sulfur utiliza-
tion of 64%. Furthermore, the RGO/AC interlayer clearly enhances
the cyclicity of the Li/S cell, retaining 655 mAh/g after 100 cycles,
which is almost twice of the value of the Li/S cell without the in-
terlayer. Furthermore, the coulombic efficiency of the cell with a
RGO/AC interlayer was close to 100%, indicating that the soluble
polysulfides from the cathode are largely blocked by the RGO/AC
interlayer, penetrating only a little to the anode through the mem-
brane pores. This remarkable improvement in sulfur utilization and
cyclability is attributed to the introduction of the RGO/AC inter-
layer, which serves as a polysulfide-diffusion inhibitor, effectively
localizing the migrating polysulfides within the cathode region of
the cell as schematically represented in Fig. 1(b).
Fig. 10 shows the rate capability of the Li/S cells with and with-
out the RGO/AC at different current densities. For the cell contain-
ing the RGO/AC interlayer, the discharge capacity steadily changed
as the current rate increased from 0.2 °C to 1.5 °C, with high re-
versible capacities 768, 617, 470, 348 mAh/g at 0.2 °C, 0.5 °C, 1 °C
and 1.5 °C, respectively. Moreover, the capacity was essentially re-
stored to its original when the current density is switched abruptly
from 1.5 °C to 0.2 °C, indicating at the good stability of the de-
signed cell. By comparison, when a current density of 1.5 °C is ap-
plied to the cell without interlayer, a reversible discharge capacity
of only 232 mAh/g was achieved. This further suggests the positive
effects of the interlayer.
4. Conclusions
In summary, a functional interlayer composed of reduced
graphene oxide and activated carbon is sandwiched between a
sulfur cathode and the separator using a simple method to im-
prove the electrochemical performance of Li/S battery. The RGO/AC
functional interlayer can not only inhibit the shuttle effect dur-
ing charge/discharge, but also promote a higher utilization of ac-
tive materials through the recycling of entrapped active materials.
Moreover, RGO/AC functional interlayer process high specific area
and abundant pores, the volume expansion of the sulfur cathode
is believed to be buffered to some extent, by the porous network
of the RGO/AC films. As a result, our work suggests that RGO/AC
films used as a functional interlayer could be a simple and effective
method to suppress the diffusion of lithium polysulfides and pro-
mote the electrochemical performance of Li/S battery. The promis-
ing strategies of a functional interlayer can be helpful to the com-
mercialization of Li/S battery.
Acknowledgments
The authors acknowledge the financial support from the
National Natural Science Foundation of China (grant no. 21406052),
the Program for the Outstanding Young Talents of Hebei Province
(grant no. BJ2014010), the Scientific Research Foundation for Se-
lected Overseas Chinese Scholars, Ministry of Human Resources
and Social Security of China (grant no. CG20150 030 02).
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