Chinese Chemical Letters 31 (2020) 217–222

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Chinese Chemical Letters

journal homepage: www.elsevier.com/locate/cclet

Communication

Cotton-derived oxygen/sulfur co-doped hard carbon as advanced

anode material for potassium-ion batteries
Baolin Xua , Shihan Qia , Fang Lia , Xiaoxin Pengb , Jinfeng Caib , Jiaojiao Liangc,** ,
Jianmin Maa,d,e,*
a
School of Physics and Electronics, Hunan University, Changsha 410082, China
b
Yiyang Wanjingyuan Electronics Co., Ltd., Yiyang 413000, China
c
College of Traffic Engineering, Hunan University of Technology, Zhuzhou 412008, China
d
Key Laboratory of Materials Processing and Mold (Zhengzhou University), Ministry of Education, Zhengzhou University, Zhengzhou 450002, China
e
State Key Lab of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 China

A R T I C L E I N F O A B S T R A C T

Article history: Hard carbon is regarded as promising anode materials for potassium-ion batteries (KIBs) owing to their
Received 16 August 2019 low price and easy availability. However, the limited rate capability still needs to be improved. Herein, we
Received in revised form 29 August 2019 demonstrate the fabrication of oxygen/sulfur co-doped hard carbon through a facile hydrolyzation-
Accepted 10 October 2019
sulfuration process of skimmed cotton. The simultaneous dopants significantly improve potassium ion
Available online 18 October 2019
diffusion rate. When served as the anode for KIBs, this hydrolyzed hard carbon delivered a high reversible
capacity (409 mAh/g at 0.1 A/g), superior rate capability (135 mAh/g at 2 A/g) and excellent cyclability
Keywords:
(about 120 mAh/g overt 500 cycles at 2 A/g). This work provides a facile strategy to prepare low-cost
Carbon
Doping
doped-hard carbon with superior potassium storage property.
Anode © 2019 Chinese Chemical Society and Institute of Materia Medica, Chinese Academy of Medical Sciences.
Potassium-ion battery Published by Elsevier B.V. All rights reserved.
Biomass

The increasing cost hinders the development of lithium-ion
batteries (LIBs) in stationary power sources, although they have
been regarded as the most promising power source for electric
vehicles (EVs) [1–4]. In recent years, sodium ion batteries (SIBs)
and potassium ion batteries (KIBs) have attracted great attention
for their inexpensive prices and global widespread resources [5–8].
Unfortunately, the commercialization of SIBs and KIBs is sluggish
due to the lack of suitable host electrode materials. Compared with
SIBs, KIBs have two advantages. Firstly, the standard electrochem-
ical potential of K+/K is lower than that of Na+/Na, which brings
higher working voltage and energy density for KIBs. Secondly,
potassium ion has the higher ionic conductivity and mobility in
organic electrolyte than that of lithium and sodium ions, due to its
weak Lewis acidity [9]. Therefore, KIBs are a potential technology
for stationary power sources.
Up to now, some advances have been achieved to find the host
electrode with good potassium storage property in recent few years.
* Corresponding author at: School of Physics and Electronics, Hunan University,
Changsha 410082, China.
** Corresponding author.
E-mail addresses: liangjiaojiao@hnu.edu.cn (J. Liang), nanoelechem@hnu.edu.cn
(J. Ma).
For cathodes, Prussian blue and Prussian white analogues have been
studied widely for the high energy density and low cost [10–12].
Besides, layered transition-metal oxides and organic cathodes have
also been developed for KIBs [13–17]. Meanwhile, several kinds of
materials are regarded as potential anode materials for KIBs,
including metal oxides/chalcogenides [18–22], alloy-type materials
[23,24], organic materials [25] and carbonaceous anodes [26].
Among those candidates, carbonaceous anodes have attracted most
attention due to the low cost and easy availability [27,28]. Graphite
suffers from a large volume expansion of 61% during potassiation
because of the large radius of potassium ion [29]. It can only deliver
very limited cyclic performance and rate capability. Carbonaceous
materials with expanded interlayer spacing are demonstrated to
deliver high electrochemical performance as anode for KIBs, like hard
carbon [30,31]. Ji’s group reported the potassium storage property of
hard carbon [32]. They prepared spherical hard carbon that showed
good cycling stability. However, it delivered inferior rate capability.
The huge capacity loss at high rates is due to the sluggish reaction
kinetics, which is the main challenge for hard carbon. To overcome
this problem, the strategy of heteroatom doping has been developed
[33]. Ding et al. reported a S-doped hollow carbon spheres prepared
by SiO2-template [34]. During potassiation/depotassiation process,
this material showed a high ion diffusion coefficient in the range of
10
10-10-12 cm2/s. Xia and co-workers synthesized a N/O co-doped

https://doi.org/10.1016/j.cclet.2019.10.009
1001-8417/ © 2019 Chinese Chemical Society and Institute of Materia Medica, Chinese Academy of Medical Sciences. Published by Elsevier B.V. All rights reserved.
218 B. Xu et al. / Chinese Chemical Letters 31 (2020) 217–222

mesoporous carbon through carbonizing Cu-BTC MOF precursor counter electrode and a layer of glass fiber (Whatman, grade GF/D)
[35]. The N/O co-doped carbon showed a reversible capacity of played the role of separator. The electrolyte was 1 mol/L KPF6
110 mAh/g at 1 A/g, since the co-doping of N and O elements dissolved in dimethyl ether (DME). The CR2025 type coin cells
remarkably enhanced the electronegativity and electrical conduc- were assembled in a glove box filled with Argon atmosphere.
tivity of hard carbon. Galvanostatic charge/discharge measurements were conducted on
Biomass carbon is considered to be promising materials for a Neware Battery Testing System. The cyclic voltammetry (CV) and
energy storage due to low cost and abundant sources, e.g., like reed electrochemical impedance spectroscopy (EIS) were carried out on
[36], cotton [37], bamboo [38], etc. Some examples on biomass an IVIUM electrochemical workstation.
carbon have been reported in KIBs. For examples, Wang’s group The H

OS

C was prepared through a hydrolyzation reaction,
prepared a loofah-derived carbon to store potassium with a followed by a calcination process. During the hydrolyzation
reversible capacity of about 155 mAh/g over 200 cycles att 100 mA/ process, the cotton was partially hydrolyzed and its color turned
g [39]. Lu and co-workers obtained a porous carbon by using potato into grayish yellow from white. During the calcination process, the
as the precursor [40]. Benefited by the porous structure, it showed cellulose in cotton fiber was carbonized. Meanwhile, the sulphur
a capacity of 152 mAh/g at 1000 mA/g. powder was sublimed to react with the oxygen-group on the
In this work, the cotton-derived O/S co-doped hard carbon was surface of cotton fibers to form O/S- defect sites. At last, the color
prepared through hydrolyzation/sulfuration processes. Benefited turned into black, as displayed in Fig. S1 (Supporting information).
from the simultaneous introduction of S and O co-dopants, the As shown in the SEM image of H

O

C (Fig. 1a), the H

O

C
final product exhibited a good cyclic stability over 500 cycles with fibers have a length of several hundreds of micrometers with the
the high Coulombic efficiencies over 99%. Notably, a high reversible diameter of dozens of micrometers. In Fig. 1b, the surface of
capacity of 135 mAh/g was achieved at 2 A/g, indicating the H

O

C fiber was relatively smooth with some tiny carbon sheet.
superior rate capability. Furthermore, the influences of hydro- For the H

OS

C in SEM images (Figs. 1c and d), although it had
lyzation and sulfuration on the structure and potassium storage the similar length and diameter with H

O

C, its surface was
property were explored. much rougher. The S-doping caused this rough surface, leading to
The used skimmed cotton was bought from a nearby pharmacy increasing its surface area. As can be seen in Figs. 1e and f, there
store (Jianerkang Co., Ltd., Soochow). To prepare the hydrolytic exists no lattice fringes which can be observed, meaning the
cotton-derived oxygen/sulfur co-doped carbon (denoted as H-OS- amorphous structure of these two cotton-derived hard carbons.
C), the hydrolyzation/sulfuration processes are necessary. In a The SEM images of OS

C and O

C are presented in Fig. S2
typical synthesis, the absorbent cotton was immersed into (Supporting information). It can be seen that those carbon fibers
0.5 mol/L HCl aqueous solution for 24 h at 60  C, firstly. Then, had a hollow structure and would break into carbon sheets. The
the partially hydrolytic cotton was washed with deionized water large-size carbon fibers will not lead to the terrible potassium
(DI water) several times to remove residuary HCl. After drying at storage property, because of the rich defect-sites and hollow
80  C overnight, the cottons were calcined with sublimed sulphur structure.
powder at 850  C (hearting rate: 5  C/min) in Argon flow. The mass To obtain the structural information of the cotton-derived
ratio between cotton and sulphur powder was 2:1. At last, the carbon samples, XRD, Raman, BET and FT-IR techniques were
fabricated O/S co-doped carbon was immersed into CS2 to wash carried out, respectively. The XRD patterns in Fig. 2a have two
residuary S out. For comparison, another three samples were also broad peaks located at about 24 and 44 , which can be assigned to
prepared. The hydrolytic cotton-derived O-doped carbon (denoted the planes of (002) and (100) in graphitic carbon (JCPDS No.
as H-O-C) was fabricated by carbonizing hydrolytic cotton without
sublimed Sulphur powder. The O/S-doped carbon (denoted as OS-
C) was synthesized without the hydrolyzation process and the
cotton-derived O-doped carbon (denoted as O-C) was obtained by
carbonizing skimmed cotton in Argon flow directly.
The X-ray powder diffraction (XRD, Rigaku D/max-2500 X-ray
diffractometer) was performed with Cu Kα radiation (l =
0.154056 nm) at a scan rate of 8 /min. The morphologies were
characterized by scanning electron microscopy (SEM, Hitachi
S4800) and transmission electron microscopy (TEM, Tecnai G2
F20). The Raman spectra were carried out by a 532 nm Raman
spectrometer (HORIBA LabRAM HR Evolution Raman spectrome-
ter). The thermogravimetric analysis was conducted in air with a
heating rate of 10  C/min (TGA, STD Q600 thermogravimetric
analyzer). The Brunauer-Emmett-Teller (BET) surface areas and
pore size distributions of the four samples were determined by the
Nitrogen absorption/desorption measurement (Nova 2000e volu-
metric adsorption analyzer). The X-ray photoelectron spectroscope
(XPS, Thermo scientific Kα spectrometer) was conducted by
utilizing Al Kα as the ray source. The Fourier transform infrared
spectrometry (FT-IR, NICOLET NEXUS 470) was also employed.
To fabricate the work electrode, the four cotton-derived carbon
samples were grinded in the agate mortar to form powder firstly.
Then, the carbon powder was mixed with acetylene black and
polyvinylidene fluoride with a mass ratio of 80:10:10, as active
material, conductive agent, and binder, respectively. The above
mixture was stirred in N-methyl pyrrolidone (NMP) to form a
slurry. Lastly, the as-prepared slurry was coated on Cu foil and Fig. 1. (a, b) SEM images of H-O-C; (c, d) SEM images of H-OS-C; (e, f) TEM images of
dried at 80  C overnight. A thin potassium plate was used as the H-O-C and H-OS-C.
 B. Xu et al. / Chinese Chemical Letters 31 (2020) 217–222
Fig. 2. (a) XRD patterns, (b) Raman spectra, (c) Nitrogen adsorption/desorption isotherms and (d) FT-IR profiles of the O-C, OS-C, H-O-C and H-OS-C samples.
26-1079). It should be noted that the (002) peaks of OS

C,
H

O

C, and H

OS

C samples show slight shift to low angles,
compared with that of C sample. This means that the S-doping and
hydrolyzation strategies could broaden the d-spacing of (002)
plane [41,42], which are beneficial to the storage of potassium ions.
The low peak intensity and broad peak width suggest the
amorphous structure, which is corresponding to the TEM image
shown in Figs. 1e and f. As can be seen from the Raman spectra
shown in Fig. 2b, there exist two peaks, namely, D peak (about
1330 cm
1) and G peak (about 1590 cm
1). The D peak is caused by
the disordered aromatic structure of saturated carbons, meaning
the defect-sites, while the G peak is due to the stretching vibration
mode E2g for sp2 carbons [43]. All the four Raman spectra have the
similar sharp, a higher D peak and a lower G peak, suggesting the
low crystallinity and rich defect-sites. The intensity ratios (ID:IG) of
O

C, OS

C, H

O

C, and H

OS

C samples are 1.08, 1.09, 1.13
and 1.11, respectively. It means the H

O

C and H

OS

C have
more defect-sites than OS

C and O

C samples, because the
hydrolyzation will bring more oxygen groups (
OH,
COOH).
Defect sites can play the role of channel for the diffusion of
potassium ions, and more defect sites could bring a better rate
performance for potassium storage. Fig. 2c shows the nitrogen
adsorption/desorption isotherms of the four samples. Obviously,
the H

OS

C has the largest specific surface area of 612 m2/g. The
profiles of OS

C, H

O

C, and H

OS

C three samples present
the same type, the type-IV adsorption/desorption hysteresis,
which suggests the mesoporous structure. On the contrary, the
C sample has the smallest specific surface area of 427 m2/g and the
different type of adsorption/desorption hysteresis. The pore sizes
of the above four samples are centered at about 1.88 nm, indicating
the mesoporous structure, as shown in Fig. S3 (Supporting
information). As shown in Fig. 2d, the FT-IR spectra prove the
existences of C¼C, C–O, and
OH bonds. In detail, all the four
samples have the broad peak at 3480 cm
1 and the small peak at
1640 cm
1, which can be attributed to the stretching vibrations of

OH group and the stretching vibrations of C¼C bond in aromatic
rings. The existence of
OH group means O-defect sites and the
C¼C bonds suggests the successful carbonization. Only the two
hydrolyzed cotton-derived samples have the sharp peaks at about
1105 cm
1.
219
Furthermore, XPS measurements were conducted to determine
the elemental composition. Fig. 3a shows the survey spectrum of
H-OS-C and H-O-C samples. For H-OS-C, there exist four peaks
assigned to S 2s, S 2p, C 1s, and O 1s, located at about 164 eV, 230
eV, 284.6 eV, and 532 eV, respectively. From the relative peak
intensities, it can be known that the content of carbon element is
high. Besides, the survey spectrum of H-O-C only shows the peaks
of C 1s and O 1s. As can be seen from the C 1s spectrum of H-OS-C
(Fig. 3b), the carbon peak can be divided into three different parts,
including C-C peak (284.6 eV), C–O/C-S peak (285.5 eV) and the
broad C

O/O¼ C

O peak (289 eV) [31]. The O 1s spectrum
(Fig. 3c) also reveals the existences of C

O and C¼O peaks, which
corresponded to the FT-IR spectrum of H-OS-C. In Fig. 3d, the S 2p
spectrum is fitted by three peaks. The two peaks assigned to S2

(163.8 eV) and polysulfides (Sn2
, 164.5 eV) indicate the successful
doping of S element enhances the electronic conductivity and
diffusion rates of potassium ions. The peak located at about 169 eV
is the spin-orbit of S 2p1/2 [44]. The atomic contents of C, O, S for H-
OS-C are 93.48%, 4.45% and 2.06%, respectively. The high-
resolution C 1s and O 1s spectra of H-O-C display the similar
shapes with those of H-OS-C, as shown in Fig. S4 (Supporting
information).
To evaluate the potassium storage of the as-prepared cotton-
derived carbon samples, CV and galvanostatic charge/discharge
measurements were carried out. Fig. 4a displays the CV curves of
the H-OS-C in the initial three cycles at a sweeping rate of 0.2 mV/s.
A large cathodic peak at 0.05 V was observed, which was caused by
the insertion of potassium ions. On contrast, as shown in Figs. S5a
and c (Supporting information), the corresponding cathodic peaks
of O-C and OS-C samples were located at 0.2 V. According to some
previous works [26,29,45,46], the intercalation reaction potential
of graphite anode is lower than that of hard carbon anode. Thus,
this difference suggests that O-C and OS-C samples have more
graphite crystallite structures and less defect-sites than H-OS-C
sample, which are corresponding to the results of FT-IR and Raman
spectra. A smaller peak at about 0.7 V was displayed in the first
cycle, which was attributed to the reversible electrochemical
adsorption and the irreversible formation of solid electrolyte
interfaces (SEI) [47]. Correspondingly, two broad peaks at about
0.25 V and higher voltage range were measured, which indicated
220 B. Xu et al. / Chinese Chemical Letters 31 (2020) 217–222

Fig. 3. XPS spectra. (a) Survey spectrum of H-OS-C and H-O-C. High-resolution C 1s spectrum (b), O 1s spectrum (c) and S 2p spectrum of H-OS-C (d).

Fig. 4. Electrochemical performances. (a) CV curves at 0.2 mV/s and (b) galvanostatic charge/discharge curves at 0.1 A/g of H-OS-C. (c) Rate capabilities at various current
densities and (d) cyclic performances at 1 A/g of the O-C, OS-C, H-O-C, and H-OS-C electrodes. (e) Long-term cyclability of H-OS-C at 2 A/g.
 B. Xu et al. / Chinese Chemical Letters 31 (2020) 217–222 221

Table 1 decay between the first and second cycles, all the four samples
Fitted EIS parameters at the states of before galvanostatic test and after the third
showed good cycling stabilities at 1 A/g over 100 cycles. It is
charging process.
believed that the broader d-spacing of (002) plane is attributed to
Samples Before test After 3 cycles this good cyclic performance. Moreover, as shown in Fig. 4e,
R2 (ohm) CPE-P1 CPE-P2 R2 (ohm) CPE-P1 CPE-P2 prolonged charge/discharge measurements were carried out at 2
O-C 2.42 0.875 0.751 5.42 0.632 0.794
A/g to evaluate the cyclic durability of H-OS-C. The initial discharge
OS-C 1.134 0.866 0.722 3.75 0.727 0.748 capacity and Coulombic efficiency were 454 mAh/g and 44.1%,
H-O-C 2.46 0.968 0.820 15.64 0.741 0.822 respectively. Subsequently, the discharge capacity decreased to
H-OS-C 2.36 0.857 0.698 12.90 0.764 0.843 145 mAh/g and became stable and the Coulombic efficiency
gradually increased to about 99.7%. After 500 cycles, a capacity
the extraction of potassium ions and the desorption behavior, of about 120 mAh/g was still maintained. It demonstrates the ultra-
respectively. In subsequent cycles, the CV curves did not change a high cycle stability of the H-OS-C electrode (Table 1).
lot, suggesting the good structure stability of H-OS-C during To understand the kinetics of potassium storage reaction well,
potassiation/depotassiation. The charge/discharge curves in the the EIS measurements were conducted. The fitted Nyquist plots of
first three cycles at 0.1 A/g is shown in Fig. 4b. The H-OS-C those four samples before and after 3 cycles are shown in Fig. 5.
delivered a high initial discharge capacity of 1278 mAh/g with a Generally, the EIS can be divided into three parts: The electrolyte
low Coulombic efficiency of 46.4%, since the large surface area resistance in high frequency region (Rs), charge transfer resistance
needs much electrolyte to form the SEI film, leading to these high in the middle frequency range (Rct), and a straight line in the low
discharge capacity and low Coulombic efficiency. In the subse- frequency area (capacitance-controlled process). Those three parts
quent cycles, there was a significant decrease in discharge capacity can be presented as the fitting circuit in insets. All the EIS patterns
to 428 mAh/g in the second cycle and 409 mA h/g in the third cycle. can be fitted by the same circuit, where resistor 1 (R1) represents
As shown in Fig. S5 (Supporting information), the three samples, the Rs, the parallel-circuit consisting of a CPE unit (CPE1) and
H-O-C, OS-C and O-C showed the same capacity degradation trends another resistor (R2) denotes the Rct, and the other CPE unit
between the first and second cycles, with H-OS-C. However, their symbolizes the capacitance-controlled process. The R2 value of
reversible capacities were lower than H-OS-C, especially the O-C OS

C is smaller than that of O

C, suggesting the better electronic
sample. conductivity, because of the S-doping. The increasing contents of
The outstanding rate capability of the H-OS-C anode was also the C

O and C¼O bonds will decrease the conductivity of
demonstrated at various current density from 0.1 A/g to 2 A/g, as hydrolytic cotton-derived samples. Thus, the H

O

C and
displayed in Fig. 4c. The H-OS-C delivered the high capacities of H

OS

C have the larger R2 values than the other two samples.
409, 322, 255, and 185 mAh/g at 0.1, 0.2, 0.5 and 1 A/g, respectively. After 3 cycles, the all the four R2 values increased because the SEI
At the high current density of 2 A/g, it still maintained a reversible formed. The CPE-P is a parameter of CPE unit and its values of 0.5
capacity of 135 mAh/g, much higher than those of H

O

C, OS

C and 1 suggest the diffusion-controlled process and capacitance-
and O

C samples. Furthermore, when the rate capability was controlled process, respectively [48,49]. Like R2, the value of CPE-P
examined at 0.1 A/g one again, the discharge capacity recovered to decreased after galvanostatic test. It reveals that potassium ions
399 mAh/g. This surprising rate performance could be attributed to show a lower diffusion rate in SEI than that in carbon host. More
the porous structure, rich O/S-defect sites and large reaction importantly, after three cycles, H

OS

C had the largest CPE-P
surface. The cycling performance of the four cotton-derived carbon among four samples, meaning the fastest kinetics of capacitance-
electrodes is shown in Fig. 4d. Although there was large capacity controlled process. The rich O/S-defect sites provide the diffusion

Fig. 5. Fitted EIS patterns at the states of before galvanostatic test and after the third charging process. (a) O-C, (b) OS-C, (c) H-O-C and (d) H-OS-C. The insets show the fitting
circuit.
222 B. Xu et al. / Chinese Chemical Letters 31 (2020) 217–222
channel for potassium ions and play the role of activated reaction
site, leading to this fast kinetics. According to above discussion, it
can be concluded that with enough electronic conductivity, the
rate-limited reason of hard carbon is the potassium ion diffusion
rate. The hydrolyzation and sulfuration strategies can enhance the
ion diffusion rate effectively.
In summary, we have successfully converted cotton into O, S-
co-doped hard carbon by hydrolyzation/sulfuration processes. The
S heteroatom enhance the electronic conductivity and the rich-
defect sites structure improves the diffusion rates of potassium
ions. When this O/S co-doped carbon served as the anode for KIBs,
it exhibited a high reversible specific capacity of 409 mAh/g at low
current density of 0.1 A/g, outstanding rate capability (135 mAh/g
at 2 A/g), and long cyclic stability (120 mAh/g overt 500 cycles at
2 A/g) with Coulombic efficiency closed to 100%. Moreover, the
potassium storage kinetics was also explored. Its superior
potassium storage property was mainly contributed from the
capacitance process, especially at large current densities.
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.
Acknowledgments
This work was supported by the Natural Science Foundation of
Hunan Province (No. 2017JJ1008), the National Natural Science
Foundation of China (Nos. 21905086, 51971090) and the Key
Research and Development Program of Hunan Province of China
(No. 2018GK2031).
Appendix A. Supplementary data
Supplementary material related to this article can be found, in the
online version, at doi:https://doi.org/10.1016/j.cclet.2019.10.009.
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