Electrochimica Acta 230 (2017) 508–513

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Electrochimica Acta
journal homepage: www.elsevier.com/locate/electacta

In situ coating of graphene-like sheets on Li4Ti5O12 particles for

lithium-ion batteries
Lingna Sun, Wei Xiong, Hongwei Mi, Yongliang Li, Haitao Zhuo, Qianling Zhang,
Chuanxin He* , Jianhong Liu*
Shenzhen Key Laboratory of Functional Polymer, College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, PR China

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

Article history:
Received 7 November 2016 Li4Ti5O12 particles are synthesized coated with very thin graphene-like sheets in situ using liquid-
Accepted 28 November 2016 polyacrylonitrile (LPAN) as the carbon source and added utilized conductivity additives to improve the
Available online 28 November 2016 conductivity of the electrode materials. The crystalline structures of Li4Ti5O12 with 20% LPAN and
different conductivity additives composites were examined by XRD. The structure and electrochemical
Keywords: performance of the graphene-like sheets coated Li4Ti5O12, with conductivity additives added, was
Li4Ti5O12 systematically investigated. The electrochemical performance also revealed that the graphene-like
graphene-like nanosheet sheets significantly improved the discharge capacity and cycling stability of Li4Ti5O12. In particular, the
electrochemical performance
coated Li4Ti5O12 with 20 wt% LPAN and 1% acetylene black (CB) reached 166.2 mAh g 1 at 10C. The
solid ball-milled synthesis
performance improvement is a result of the graphene-like nanosheet conformal coating, which creates
an electrically conductive network for the electrode.
© 2016 Published by Elsevier Ltd.

1. Introduction applications [4,5]. Unfortunately, Li4Ti5O12 also suffers from poor

As the environmental problems and energy crisis become more
and more serious, the need for clean and efficient energy sources
has directed a global trend. Recently, lithium ion batteries (LIBs)
have attracted great attention as the potential candidates for the
next generation electronic devices due to their high energy density
and environmental compatibility [1–3]. But to achieve extensive
application, there are several critical disadvantages, including low
power density, short cycling life and safety hazards, which are
highly concerned for LIBs materials. Therefore, the search for
electrode materials with enhanced performance becomes one of
the most important issues. Li4Ti5O12 is regarded as one of the most
promising anode materials due to its unique properties. Compared
with the general graphitic carbons, Li4Ti5O12 has a flat and
relatively high voltage plateau at approximately 1.55 V versus Li+/
Li, thus the formation of the solid electrolyte interface (SEI) layers
and electroplating of lithium is avoiding. Furthermore, the
Li4Ti5O12 exhibits the negligible volume change during the
charge/discharge processes. As a zero-strain material, Li4Ti5O12
with the improved safety and structure stability, contribute to the
excellent cycling performance and great promise for high rate LIB
* Corresponding authors.
E-mail addresses: hecx@szu.edu.cn (C. He), Liujh@szu.edu.cn (J. Liu).
electronic conductivity, which leads to the problem that the
electrochemical properties of Li4Ti5O12 can’t commendably meet
the requirements of the practical application. To solve the problem,
several effective approaches have been proposed, such as
nanosization[6–9], surface modification [10], and doping with
metal or non-metal ions [11,12].
Among various methods, the well-known surface carbon-
coating technique is one of the most effective ways to improve the
rate performance of the electrode material [13]. Li and his
colleagues prepared nitrogen-doped carbon coated Li4Ti5O12
nanocomposite with acetyl glucosamine as carbon source by
pre-coating process combined with ball milling. At the charge-
discharge rate of 10.0C, the discharge capacity of sample is
133.4 mAh g 1 [14]. Graphene, a two-dimensional macromolecular
sheet of carbon atoms with a honeycomb structure, is another
promising carbon source due to its excellent electronic conductiv-
ity and mechanical properties [15]. When electrode materials are
coated or wrapped with graphene, not only the electrical
conductivity but also the capacity and cycling stability of anode
materials may be improved [16]. Our group reported that the uses
of graphene to form composite materials with LiMn2O4 [17] and Si
[18] to improve the capacity and cyclic stability of anode materials.
Several reports detail about graphene-based Li4Ti5O12 materials
[19–24]. For example, Zhu et al. reported graphene-embedded
Li4Ti5O12 anode material showed improved discharging/charging

http://dx.doi.org/10.1016/j.electacta.2016.11.165
0013-4686/© 2016 Published by Elsevier Ltd.
 L. Sun et al. / Electrochimica Acta 230 (2017) 508–513
and cycling properties [25]. Shi et al. prepared a hybrid of lithium
titanate nanoparticles well dispersed on electrical conductive
graphene nanosheets as an anode material for high rate lithium ion
batteries. With 5 wt.% graphene, the hybrid materials deliver a
specific capacity of 122 mAh g 1 even at a very high charge/
discharge rate of 30C [26]. The graphene/Li4Ti5O12 composites
were obtained by in situ hydrolysis of C16H36O4Ti with ultrasonic-
assist in the graphene oxide/ethanol solution. The composites with
uniform distribution of Li4Ti5O12 nanoparticles on the RGO sheets
exhibited superior rate capacities of 154 mAh g 1 (10C) and
149 mAh g 1 (20C), considerably higher than the values found in
the previous reported hybrid structures[27].
In additon, the Li4Ti5O12/G/CNTs hybrid material was synthe-
sized via a facile rheological phase reaction route. At 0.2C, the
initial discharge capacity of the Li4Ti5O12/G/CNTs was 172 mAh/g,
and even at the high rate of 5.0C and 10.0C, it could still remain at
150 mAh/g and 144 mAh/g, respectively [28]. A facile strategy is
developed based on a sol–gel method to prepare lithium titanate–
carbon nanofiber composites as anode in Li-ion batteries [29]. In
addition, Li4Ti5O12 and graphene nanostructure composites were
synthesized and exhibited superior rate capacities [30–32].
However, these graphene-based Li4Ti5O12 usually generate a
hybrid or composite with graphene and Li4Ti5O12. Fewer reports
describe coating Li4Ti5O12 anode materials with graphene in situ.
Here we synthesized Li4Ti5O12 particles coated with very thin
graphene-like sheets in situ using liquid-polyacrylonitrile (LPAN)
as the carbon source and utilized conductivity additives added to
improve the conductivity of the electrode materials.
2. Experimental Methods
2.1. Preparation of Li4Ti5O12
Li2CO3 and TiO2 with stoichiometric ratio were mixed and ball-
milled. The molar ratio of Li and Ti was 0.83, in other words Li2CO3
3.03% excess to compensate for lithium evaporation during
calcination. The mixture was sieved and transferred to a corundum
crucible, and then heated in argon atmosphere at 800  C for 14 h,
heating rate of 5  C/min.
2.2. Preparation of Li4Ti5O12 coated with graphene-like nanosheets
Li2CO3 and TiO2 with stoichiometric ratio were mixed and the
ratio of Li2CO3 was a little excess. The precursor and a liquid
acrylonitrile homopolymer (LPAN) with 1:0.2 weight ratio were
denoted as 20% LPAN. LPAN was dissolved in methanol and the
solution was added to the precursor. Then the mixture was stirred
and the solvent was evaporated. The obtained solid was heated to
70  C for 2 h and then sieved and transferred to a corundum
crucible, and then heated in argon atmosphere at 800  C for 14 h,
heating rate of 5  C/min.
2.3. Preparation of Li4Ti5O12/conductive additive/LPAN composite
electrode material
Li2CO3 and TiO2 with stoichiometric ratio were mixed and the
ratio of Li2CO3 was a little excess. 1% conductive additive of carbon
microtubes (CMTs) was added to form the precursor. LPAN with
20% weight ratio of the precursor was dissolved in methanol and
the solution was added to the precursor. Then the mixture was
stirred and the solvent was evaporated. The obtained solid was
heated to 70  C for 2 h and then sieved and transferred to a
corundum crucible, and then heated in argon atmosphere at 800  C
for 14 h, heating rate of 5  C/min.
The conductive additive was changed to carbon nanotubes
(CNTs) or acetylene black (CB) by the same method.
509
The working electrode was prepared by dispersing 80 wt%
active material, 10 wt% acetylene black and 10 wt% polyvinylidene
fluoride (PVDF) binder in the N-methylpyrrolidione solvent to
form a uniform slurry. The slurry was coated on Al foils and dried in
a vacuum at 110  C for 6 h before assembled into coin cell in an
argon-filled glovebox.
2.4. Characterization and electrochemical measurements
The crystalline structures were obtained by X-ray diffraction
(XRD, Bruker, Germany) using Cu Ka. Transmission electron
microscopy (TEM) images were collected using a FEI-Tecnai G2
(USA, 200 kV) instrument. The galvanostatic charge/discharge
were carried out on a LAND-CT2001A battery test system (China)
between cut-off potentials of 2.00 and 0.01 V. The specific capacity
was calculated based on the total mass of active materials. The
electrochemical impedance measurements were accomplished by
Solartron Impedance analyzer 1260A from 100 kHz to 0.1 Hz.
Raman measurements were carried out at room temperature using
a Jobin Yvon/Atago Bussan T64000 triple spectrometer equipped
with micro-optics.
3. Results and Discussion
During this experiment, a liquid acrylonitrile homopolymer
(LPAN) was used to form a graphene-like coating. The morphology
and structure of the graphene-like sheets was investigated in the
literature [17,18] reported by our group earlier. According to the
analysis of the precursor and the graphene-like sheets, the
Li4Ti5O12 anode materials coated with the graphene-like sheets
were prepared at different calcination temperatures and with
different LPAN contents to optimise the preparation conditions and
composition.
The crystalline structures of Li4Ti5O12 with 20% LPAN and
different conductivity additives composites were examined by
XRD and the patterns are shown in Fig. 1. All the strong peaks can
be assigned to Li4Ti5O12 reported in the literature (JCPDS 49-0207).
It can be considered that Li4Ti5O12 composites have a good
crystallinity when carbon microtubes (CMTs), carbon nanotubes
(CNTs) or acetylene black (CB) were added in the product and no
other impurities were observed in the products. The addition of
CMTs, CNTs, or CB did not affect the crystallographic sturcture of
LTO.
The sample is obtained by LTO and 1% CB composites with 20%
weight ratio of LPAN (LTO-1%CB-20%LPAN). The morphologies of
Fig. 1. XRD patterns of Li4Ti5O12 added different conductivity additives.
510 L. Sun et al. / Electrochimica Acta 230 (2017) 508–513
Fig. 2. (a and b) TEM and HRTEM images of LTO-1%CB-20%LPAN composite, (c and d) Raman spectra and TG curve of LTO-1%CB-20%LPAN composite; (e) XPS spectra of Ti 2p
spectrum; (f) XPS spectra of C 1s spectrum.
LTO-1%CB-20%LPAN were observed by TEM. A typical TEM image of
the as-synthesized product is shown in Fig. 2a. The product
exhibited uniform particles with irregular shape, with average
sizes about 100  200 nm. Moreover, the HRTEM image of the LTO
composites (Fig. 2b) shows that the nanoparticle of LTO is well-
wrapped within the outer graphene-like matrix and the observed
lattice fringes in the core region with an interplanar spacing of
0.25 nm, corresponding to the (311) lattice spacing of LTO. And the
thickness of the graphene-like layers of the LTO composite are
about 3–5 nm and the layers are uniform coating on the surface of
LTO particle. The Raman spectra of the powders shown in Fig. 2c
indicate two main peaks at around 1358 and 1592 cm 1, which
correspond to the D- and G-bands of carbon materials, respective-
ly, and the broad peak at around 2500–3200 cm 1 represents the
2D band of carbon materials. The broad peak and lower intensity of
the 2D band indicate that the graphene in the LTO composites has
several layers, which is consistent with the result of the HRTEM
image. As shown in Fig. 2d, the TG curve of Li4Ti5O12-1%CT-20%
LPAN composite. It can be seen that the sample has clear weight
loss from 280  C. The TG curve almost keeps a constant value above
700  C. Because spinel Li4Ti5O12 was stable in atmosphere, the
composite lost approximately 3.64% weight due to decrease of
carbon in the composite.
As shown in Fig. 2e, the XPS spectrum of the Ti 2p is consisted of
two peaks which can be correspond very well to the Ti 2p1/2
(464.2 eV) and the Ti 2p3/2 (458.2 eV). The difference between the
Ti 2p3/2 and the Ti 2p1/2 is 6 eV, representing a regular state of Ti4+
for the LTO, as well as in TiO2. Moreover, the C 1 s spectrum of the
as-prepared material was fitted with three peaks as shown in
Fig. 2f. The main peak at 284.5 eV could be assigned to sp2
hybridized graphitic carbon bonding (C-C), indicating that most of
C atoms are aromatic carbon. The peak at 285.7 eV is assigned to C-
N bonding and a weak peak at 288.5 eV should be attributed to C-O
bonding, which results from the pyrolysis of raw materials.
 L. Sun et al. / Electrochimica Acta 230 (2017) 508–513
3.1. Electrochemical performance
3.1.1. Effect of the different weight ratio of LPAN on the electrochemical
performance of LTO composite
The electrochemical performance of the fabricated LTO
composite was systematically evaluated using the coin-type cell
configuration. It was found in our experiments that Li4Ti5O12 and
1% carbon microtubes composites with different weight ratio of
LPAN added perform different electrochemical performance. The
cycling behavior of LTO and 1% carbon microtubes composites at
high rates of 10C (1C = 175 mA g 1) within the voltage range of 1–
3 V were shown in Fig. 3a. For comparison, the initial reversible
discharge specific capacities of LTO and 1% carbon microtubes
composites without LPAN are 65.6 mAh g 1 and after 200 cycles
the retained capacities are 30.1 mAh g 1. It can be seen that the
pure addition of 1% carbon microtubes can’t improve the capacities
of LTO, because carbon microtubes could not coat on the surface of
LTO particles. The second reversible discharge specific capacities of
Li4Ti5O12 and 1% carbon microtubes composites with 10%, 20%, 30%
weight ratio of LPAN are 118.6, 116.2, 58.8 mAh g 1, respectively.
The retained capacities for 10%, 20%, 30% weight ratio of LPAN after
200 cycles are 100.1, 113.8 and 56.4 mAh g 1, and the retention
ratios are 84.4, 97.9 and 95.9%, respectively. It should be noted that
the best electrochemistry properties are obtained by LTO and 1%
carbon microtubes composites with 20% weight ratio of LPAN
(LTO-1%CMTs-20%LPAN).
Fig. 3b compared the rate performance between LTO-1%CMTs
and LTO-1%CMTs-20%LPAN. It is clear that the LTO-1%CMTs-20%
LPAN sample exhibits improved rate performance than the LTO-1%
CMTs sample. At a high rate of 10C, a specific capacity of
116 mAh g 1 can be retained for LTO-1%CMTs-20%LPAN composite
sample. In contrast, for LTO-1%CMTs, the specific capacity decline
quickly to 38.4 mAh g 1 at a rate of 10C. These results confirmed
that the lithium titanate coated by graphene-like sheets here own
high specific capacity and excellent cycling stability at high rate
charge/discharge.
3.1.2. Effect of the different conductivity additives on the
electrochemical performance of LTO composites
It was found that Li4Ti5O12-20% LPAN composites with 1 wt%
different conductivity additives added, such as CB, CMTs, and CNTs
respectively, perform different electrochemical performance.
Fig. 4a presents the capacities of these new anode materials at
various rates from 0.1C to 10C. The first coulombic efficiency of
Li4Ti5O12-1%CB-20%LPAN is 90.5% with a current density of 0.1C, as
shown in Fig. 4a. It is clear that the LTO-1%CB-20%LPAN sample
exhibits best rate performance than the other two samples. With
the addition of 1 wt% CB into the Li4Ti5O12-20% LPAN electrode, the
capacities of Li4Ti5O12-1%CB 20%LPAN electrodes were signifi-
cantly improved at most current rates than the capacities of
Fig. 3. (a) The cycle performance of added 1% CMTs Li4Ti5O12 with different content of LPAN at 10C, (b) The rate performance of Li4Ti5O12-1%CMTs-0%LPAN and Li4Ti5O12-1%
CMTs-20%LPAN composites.
511
Li4Ti5O12-1%CMTs-20%LPAN. The reason maybe that CB exhibits
excellent electronic conductivity and disperses homogeneously in
the electrode materials, and contacts with Li4Ti5O12 particles to
reduce the contact resistance between the particles. In addition, it
should be noted that when the current rate is reduced back to 0.1C
again, a capacity of the LTO-1%CB-20%LPAN sample higher than
140 mA h g 1 can be resumed. The perfect electrochemical
performance may result from the carbon content and the
graphene-like layers of the Li4Ti5O12 particles.
The cyclic performance of the Li4Ti5O12-20%LPAN composites
with 1 wt% different conductivity additives added, such as CB,
CMTs, and CNTs, were evaluated at a high current rate of 10C, as
shown in Fig. 4b. As it can be seen, the initial reversible discharge
specific capacities of LTO-1%CB-20%LPAN, Li4Ti5O12-1%CMTs-20%
LPAN, and Li4Ti5O12-1%CNTs-20%LPAN at 10C are 166.2, 130.8 and
124.9 mAh g 1, respectively. The capacity of LTO-1%CB-20%LPAN
remained high at 141.9 mA h g 1 after 200 cycles, which
corresponds to 85% retention of the first discharge capacity. After
2000 cycles, the capacity of LTO-1%CB-20%LPAN remained at
94.8 mA h g 1, higher than the capacities of Li4Ti5O12-1%CMTs-20%
LPAN and Li4Ti5O12-1%CNTs-20%LPAN. Nevertheless, all electrode
materials exhibited excellent cyclability. These results confirmed
that the lithium titanate tailored by CB and LPAN here own high
specific capacity and excellent cycling stability at high rate charge/
discharge.
Electrochemical impedance spectra (EIS) of the as-prepared
materials are measured, respectively, as shown in Fig. 4c. The plots
of all the four samples exhibit the commonness that the plots
consist of a semicircle in the high-frequency region, followed by a
straight line in the low-frequency region. The semicircles in the
high-frequency region for the LTO electrode are related to surface
charge-transfer process, and straight line in the low-frequency
region corresponds to a semi-infinite Warburg diffusion process
[33]. The diameter of the semicircle for the LTO-20%LPAN electrode
is larger than that of the other three samples, indicating that the
LTO-20%LPAN composite electrode possess higher resistance.
Therefore, the addition of conductive additive is very important
for improving the electrical conductivity of LTO electrode.
However, different conductive additives have different effects on
the electrical conductivity. CB is the best conductive additive
among the three samples. The diameter of the semicircle for the
LTO-1%CB-20%LPAN electrode is the smallest in the four samples,
indicating that the LTO-1%CB-20%LPAN electrode possesses lower
resistance, which is due to the stable structure and the improved
conductivity.
3.1.3. Effect of the different additive amount of CB on the
electrochemical performance of LTO composites
The different additive amount of CB has important influence
on the electrochemical performance of LTO composites. The cyclic
512 L. Sun et al. / Electrochimica Acta 230 (2017) 508–513

Fig. 4. (a) The cycle performance of Li4Ti5O12 added with different conductivity additives at different discharge rate, (b) The cycle performance of added 20%LPAN Li4Ti5O12
with 1% different conductivity additive at 10C, (c) Nyquist plots of Li4Ti5O12-20%LPAN added with different conductivity additives.

Fig. 5. (a) The cycle performance of Li4Ti5O12-20%LPAN with different content CB at 10C, (b) Nyquist plots of Li4Ti5O12-1%CB added with different content LPAN.

performance of the Li4Ti5O12-20%LPAN composites, and Li4Ti5O12-
20%LPAN with 1 wt%, or 2 wt% CB, were evaluated at a high
current rate of 10C, as shown in Fig. 5a. This observation verifies
that the best additive amount of CB is 1 wt%. As shown in Fig. 5a,
the initial reversible discharge specific capacity of LTO-1%CB-20%
LPAN at 10C is 166.2 mAh g 1. But the first discharge capacity of
LTO-2%CB-20%LPAN is only 136 mAh g 1, lower than the capacity
of LTO-1%CB-20%LPAN, which remained at 141.9 mA h g 1 after
200 cycles. The electrochemical performance of Li4Ti5O12-20%
LPAN without CB is obviously poorer than the other samples.
Fig. 5b shows the EIS results of the LTO-1%CB composites with
various amount of LPAN. The large semicircles observed for the
LTO electrode are indicative of high interfacial charge-transfer
resistance (Rct), which can be attributed to the poor electrical
conductivity of the LTO. The diameters of the semicircles for the
LTO-1%CB-LPAN composites are smaller than that of the LTO-1%
CB electrode, indicating that the LTO-1%CB-LPAN composite
electrodes possess lower resistance, which is due to the improved
conductivity by the uniform coating of graphene-like nanosheets
on the LTO particles. Compared to the LTO-1%CB-20%LPAN
composite, the Rct of the LTO-1%CB-10%LPAN and LTO-1%CB-
30%LPAN composites are higher, indicating that LTO-1%CB coated
with 20% LPAN has higher electrical conductivities than the other
two composite anode.
4. Conclusions
In conclusion, we have developed a facile approach to obtain
Li4Ti5O12 particles coated with graphene-like layer and conductiv-
ity additives added by a solid ball-milled process. The structure and
electrochemical performance of the graphene-like membrane
coated Li4Ti5O12, with conductivity additives added, was system-
atically investigated. The electrochemical performance also
revealed that the graphene-like membrane significantly improved
the discharge capacity and cycling stability of Li4Ti5O12. In
particular, the coated Li4Ti5O12 with 20 wt% LPAN and 1% CB
reached 166.2 mAh g 1 at 10C. The EIS analyses also demonstrated
that the graphene-like membrane did not influence the insertion
or desertion of Li+. LTO-1%CB-20%LPAN composites possess
excellent electrochemical properties especially at high rate, which
is due to the improved conductivity by the uniform coating of
graphene-like nanosheets on the LTO particles.
 L. Sun et al. / Electrochimica Acta 230 (2017) 508–513 513

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