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A Journal of
Accepted Article
Title: Recent development of all-solid-state lithium secondary batteries
with sulfide inorganic electrolytes
Authors: Ruochen Xu, Shengzhao Zhang, Xiuli Wang, Yan Xia, Xinhui
Xia, Jianbo Wu, Changdong Gu, and Jiangping Tu
This manuscript has been accepted after peer review and appears as an
Accepted Article online prior to editing, proofing, and formal publication
of the final Version of Record (VoR). This work is currently citable by
using the Digital Object Identifier (DOI) given below. The VoR will be
published online in Early View as soon as possible and may be different
to this Accepted Article as a result of editing. Readers should obtain
the VoR from the journal website shown below when it is published
to ensure accuracy of information. The authors are responsible for the
content of this Accepted Article.
To be cited as: Chem. Eur. J. 10.1002/chem.201704568
Link to VoR: http://dx.doi.org/10.1002/chem.201704568
Supported by
10.1002/chem.201704568
Chemistry - A European Journal
Table of content
Due to the increasing demand of security and energy density, all-solid-state batteries
have become the promising next-generation energy storage devices to replace the
traditional batteries with flammable organic electrolytes. In this review, we focus on the
recent developments of sulfide inorganic electrolytes in all-solid-state batteries, and the
challenges of assembling bulk-type all-solid-state batteries for industrialization are
discussed.
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TOC graphic
10.1002/chem.201704568
Chemistry - A European Journal
Recent development of all-solid-state lithium secondary batteries
with sulfide inorganic electrolytes
Ruochen Xu [a], Shengzhao Zhang [a], Xiuli Wang *[a], Yan Xia [a], Xinhui Xia [a],
[a] Dr. R. Xu, S. Zhang, Y. Xia, Prof. X. Wang, X. Xia, C. Gu, J. Tu
State Key Laboratory of Silicon Materials, Key Laboratory of Advanced Materials and
Applications for Batteries of Zhejiang Province, and School of Materials Science and
Engineering, Zhejiang University
Hangzhou 310027, China
E-mail: wangxl@zju.edu.cn; tujp@zju.edu.cn, tujplab@zju.edu.cn
[b] Prof. J. Wu
College of Physics & Electronic Engineering, Taizhou University
Taizhou 318000, China
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Jianbo Wu [b], Changdong Gu [a], and Jiangping Tu *[a]
10.1002/chem.201704568
Chemistry - A European Journal
Abstract
Due to the increasing demand of security and energy density, all-solid-state lithium
ion batteries have become the promising next-generation energy storage devices to
replace the traditional liquid batteries with flammable organic electrolytes. In this
solid-state batteries. The challenges of assembling bulk-type all-solid-state batteries for
industrialization are discussed, including low ionic conductivity of the present sulfide
electrolytes, high interfacial resistance and poor compatibility between electrolytes and
electrodes. Many efforts have been focused on the solutions for these issues. Despite
some progresses have been achieved, it is still far away from practical application. The
perspectives for future research on all-solid-state lithium ion batteries are presented.
Keywords: All-solid-state; Sulfide inorganic electrolyte; Lithium secondary battery.
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review, we focus on the recent developments of sulfide inorganic electrolytes for all-
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Chemistry - A European Journal
1. Introduction
Rechargeable lithium ion batteries (LIBs) are rapidly developing to meet the
increasing requirements of energy storage with high energy and power density in recent
years, which have become extremely significant in portable electronics and electric
bring safety issues, including flammable organic electrolytes, thermal instability and
toxic chemicals [4]. However, LIBs have the irreplaceable position in large-scale energy
storage devices which almost conquer the electronics market [5, 6]. For these reasons,
bulk-type all-solid-state LIBs (ASSLIBs) without organic liquid electrolytes are a good
choice to replace the traditional liquid batteries
[7]
. ASSLIBs made up of
negative/positive electrodes, and solid electrolyte have high energy density due to the
compressed structure. In addition, solid-state ionic electrolytes are inert toward metallic
lithium and can resist the growth of lithium dendrite
[8]
, and also have excellent
temperature stability and a wide stable electrochemical window that enables high
voltage cathodes [9]. Generally, solid electrolytes can be divided into inorganic solid
electrolytes, solid polymer electrolytes and composite solid electrolytes
[10]
. In this
review, we primarily discuss the classification of inorganic solid electrolytes, focusing
on sulfide electrolytes [11].
The study of ASSLIBs was started in the middle of the 20th century with the
development of high-conductivity solid-state electrolytes [12]. One of the most important
properties of sold electrolytes is the lithium ionic conductivity. Ionic conduction in
ceramic electrolytes is realized by movement of ions through vacancies or defects, thus
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vehicles nowadays [1-3]. In particularly, the conventional LIBs with liquid electrolytes
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Chemistry - A European Journal
the ionic conductivities of electrolytes increase with temperature
[13]
. The ionic
conductivities of sulfide inorganic electrolytes conform to the Arrhenius equation: ? =
A exp (?Ea/kT), where Ea is the activation energy, T is the absolute temperature, k is the
Boltzmann constant, and A is the pre-exponential factor
[14]
. To achieve fast ionic
vacancies or defects for the mobile ions to occupy is larger than that of mobile species;
(2) the barrier energies are lower than the transition energies from one site to another;
(3) suitable size of mobile ions to fit the conduction channels; (4) the transition of ions
can be connected to form a continuous diffusion pathway [15].
To realize bulk-type ASSLIBs, solid electrolytes should have high lithium ionic
conductivity at room temperature, low activation energy, stable wide electrochemical
window, thermal stability without volume change, chemical stability versus anode and
negligible electron conductivity [16]. However, most of the existing solid electrolytes
have not achieved the requirement of ionic conductivity for ASSLIBs [17], which is the
main obstacle to limit their large-scale application. Recently, various attempts have
been made to improve the ionic conductivities of sold electrolytes and some progress
has been achieved. Sulfide inorganic compounds have been widely studied as solid
electrolytes for ASSLIBs because they have higher ionic conductivities than other
inorganic electrolytes at room temperature [11,18,19]. However, the most serious drawback
of sulfide inorganic electrolytes is that their chemical stability is very poor in air [20].
Sulfide electrolytes are sensitive to moisture and easy to react with the water contained
in air, leading to generation of harmful H2S gas and destruction of electrolytes [21]. The
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conduction, the electrolyte should meet the following conditions: (1) the number of
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Chemistry - A European Journal
effective way to reduce H2S generation and improve chemical stability in air is to
substitute oxides in electrolytes [22]. The poor chemical stability strongly limits the
application of sulfide electrolytes despite it can be improved by the substitution.
An all-solid-state battery is comprised of cathode, anode and solid-state electrolyte,
[23]
. The solid electrolyte in ASSLIBs not only serves as lithium-ion conduction but also
act as battery separator. Sulfide electrolytes are developed for ASSLIBs because of their
high ionic conductivities and non-flammability
[24]
. In addition, sulfide inorganic
electrolytes generally have a wide stable electrochemical window, which enables the
ASSLIBs to be operated over a wide voltage range [25]. Although the sulfide electrolytes
have almost reached the demand of ASSLIBs, there are still many critical challenges to
be overcome for large-scale application, including large interfacial resistance between
electrolyte and electrodes, low ionic conductivity of electrode materials, volume change
of cathodes during cycling and instability in contact with anodes [12, 26, 27]. Furthermore,
the fabrication technology of ASSLIBs is under developing, and the interfacial contact
during the assembly process is an extremely important factor for ASSLIBs. Therefore,
suitable approaches of solving the issues mentioned above should be developed to
achieve high-performance ASSLIBs. We shall discuss the current progress and
potential of sulfide electrolytes in ASSLISs in detail.
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as shown in Figure 1, and the compact structure leads to high energy density for battery
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Chemistry - A European Journal
Carbon
Solid
Electrolyte
Figure 1. Schematic diagram of a typical bulk-type all-solid-state battery.[28]
2. Sulfide solid electrolytes
Inorganic solid electrolytes can be divided into oxide and sulfide electrolytes.
Compared to oxide-based solid electrolytes, sulfide-based electrolytes have smaller
binding force with Li ions due to the lower electronegativity and the ionic radius of S2?
in sulfide-based electrolytes is larger than that of O2? in oxide-based electrolytes,
leading the ionic migration channel of the former is larger than that of the latter [19, 29].
Therefore, sulfide electrolytes have higher ionic conductivities than oxide electrolytes.
And the sulfide electrolyte shows small grain boundary resistance even in cold-pressed
pellet, which is superior to oxide one [12]. To date, sulfide solid electrolytes have been
extensively studied for ASSLIBs and they have a high room temperature conductivity
over 0.1~1 mS cm?1. Table 1 lists the ionic conductivities of existing sulfide
electrolytes. Except the high ionic conductivity, sulfide electrolytes have several
advantages, including wide electrochemical window, excellent thermal stability and
good mechanical properties [30-35].
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Active
Materials
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Chemistry - A European Journal
Structure
Conductivity
(25 癈 /mS cm?1)
Reference
Li7P3S11
Glass-ceramic
17
[36]
Li7P2S8I
Crystal
0.63
[37]
Li6PS5Cl
Crystal
0.7
[38]
70Li2S�P2S5
Glass-ceramic
3.2
[39]
70Li2S�P2S5�2S3
Glass-ceramic
5.4
[40]
70Li2S�P2S5�i3PO4
Glass-ceramic
1.87
[41]
75Li2S�P2S5�2O5
Glass-ceramic
0.8
[42]
Crystal
0.16
[9]
Li3.25P0.95S4
Glass-ceramic
1.3
[43]
Li9.6P3S12
Glass-ceramic
1.2
[44]
70Li2S�P2S5
Glass
0.054
[38]
75Li2S�P2S5
Glass
0.2
[45]
80Li2S�P2S5
Glass
0.17
[46]
Li10GeP2S12
Crystal
12
[47]
Li10.35Ge1.35P1.65S12
Crystal
14.2
[48]
Li3.25Ge0.25P0.75S4
Crystal
2.2
[49]
Li10SnP2S12
Crystal
4.0
[50]
Li10SiP2S12
Crystal
2.3
[51]
Li9.54Si1.74P1.44S11.7Cl0.3
Crystal
25
[44]
Composition
Li3PS4
To data, sulfide electrolytes are usually synthesized by three methods, including
melt-quenching [36, 52], mechanical ball-milling [53, 54] and liquid-phase method [55, 56].
Most of the sulfide electrolytes are prepared by mechanical ball-milling method and the
ionic conductivity increases with the precipitation of crystalline phase by heattreatment. Eom et al.[11] quantitatively examined the crystallization kinetics of
mechanically milled 70Li2S�P2S5 glass to enhance the crystallinity of the solid
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Table 1. Ionic conductivities of different sulfide solid electrolytes
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Chemistry - A European Journal
electrolyte and they found the enhancement in conductivity for the 78Li2S-22P2S5
glass-ceramics accomplished by using two-step heat treatment of 170 癈 for 30 min
(nucleation stage) and 230 癈 for 3 h (crystal growth stage). As for the method of meltquenching, the preparation conditions are harsh and it is easy to produce impurities
melt quenching technique under various melting conditions. The conductivity of the
glass?ceramics was enhanced by the precipitation and growth of Li7P3S11 crystal.
However, the Li7P3S11 crystal changed into the thermodynamically stable phase of low
conductive Li4P2S6, with further increasing the heat treatment temperature and holding
time. In addition, the liquid-phase method enables sufficient reaction of raw materials
and produces homogenous precursor. And the ionic conductivities of solid electrolytes
made by liquid-phase method are affected by the organic solvent
[57]
. Ito et al.[58]
synthesized a crystal phase of Li7P3S11 electrolyte by a liquid phase method using 1,2dimethoxyethane solvent. The impurity or amorphous phase easily formed at the grain
boundaries, resulting in high activation energy and low ionic conductivity.
Research into sulfide-type solid electrolyte started in 1986 with the Li2S-SiS2
system [59]. In 2001, Kanno et al.[49] first reported the crystalline thio-lithium conductor
Li3.25Ge0.25P0.75S4 with an ionic conductivity of 2.2 mS cm?1. Li7P3S11 glass-ceramic
was found in the Li2S-P2S5 system in 2005, which had high ambient temperature ionic
conductivity of 3.2 mS cm?1 with low activation energy, greatly promoting the
development of sulfide electrolytes [39]. Recently, a new sulfide crystal Li10GeP2S12 was
synthesized. It exhibited an extremely high lithium ionic conductivity of 12 mS cm ?1,
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during the cooling process. Hayashi et al.[52] prepared the 70Li2S�P2S5 glasses by a
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Chemistry - A European Journal
exceeding even those of liquid electrolytes [47]. The Li10GeP2S12 electrolyte also showed
high stability and wide potential window [60-62]. More recently, Kato et al.[44] reported a
lithium superionic conductor of Li9.54Si1.74P1.44S11.7Cl0.3 (Figure 2) with an
exceptionally high conductivity of 25 mS cm?1. In addition, the ASSLISs based on
electrochemical stability, exhibiting high power density and ultrafast charging
performance.
(b)
(c)
(a)
Figure 2. (a) Arrhenius conductivity plots. (b) Crystal structure of Li9.54Si1.74P1.44S11.7Cl0.3. (c)
Nuclear distributions of Li atoms in Li9.54Si1.74P1.44S11.7Cl0.3 at 25 癈.[44]
Despite much progress has been achieved, there are still fundamental problems in
sulfide solid electrolyte: (1) low lithium ionic conductivities of most existing sulfide
electrolytes; (2) poor chemical stability in air; (3) low electrochemical stability at
electrolyte/electrode interface; (4) high cost of partial sulfide electrolytes. The ionic
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Li9.54Si1.74P1.44S11.7Cl0.3 electrolyte possessed excellent ionic conductivity and
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Chemistry - A European Journal
conductivities of solid electrolytes can be enhanced by changing composition or
optimizing preparation method. Huang et al.[41] reported on a 70Li2S-30P2S5 system
with substitution of Li3PO4. The glass-ceramics substituted with 1 mol % Li3PO4
exhibited the high conductivity of 1.87 mS cm?1 and enhanced its stability. Moreover,
al.[36] reported that the hot pressed Li7P3S11 showed high ionic conductivity of 17 mS
cm?1 because of the reduced boundary resistance during heat treatment (Figure 3). As
for the chemical stability of sulfide electrolytes, changing the component of electrolyte
is an effective way. Ohtomo et al.[63] prepared the Li2O-Li2S-P2S5 glass through the
replacement of Li2S by Li2O, which was effectively in the suppression of H2S gas
generation. The electrochemical stability at interface can be improved by anion doping
in electrolytes. Rangasamy et al.
[37]
prepared Li7P2S8I from LiI and Li3PS4 that
demonstrated high electrochemical stability with metallic lithium anode. To realize
industrialization, the price of raw materials is an important factor. As for Li10GeP2S12,
the cost of Ge is very high. Bron et al.[50] reported the synthesis of Li10SnP2S12 instead
of Li10GeP2S12, showing the ionic conductivity of 4 mS cm?1 and one-third of the cost
for the Ge analogue. The Si could also replace the Ge atom and Li11Si2PS12 was recently
reported with extremely high ionic conductivity [64].
In a word, enhancing the ionic conductivities of solid electrolytes can be achieved
by doping of the existing system or optimizing the preparation method. The stability
can be improved by the addition of oxygen atoms or anion doping. The researchers now
devote to find new solid electrolyte system with high stability/ionic conductivity and
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the preparation method also greatly affects the property of solid electrolytes. Seino et
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Chemistry - A European Journal
(a)
(c)
(b)
(d)
Figure 3. SEM images of 70Li2S-30P2S5 glass-ceramic: (a) cold-pressed sample, (b) heat-treated
sample at 280 癈, (c) Complex impedance plots for 70Li2S-30P2S5 glass-ceramic at ?35 癈, (d)
after cold pressing and heat treatment at 280 癈.[36]
3. Development of all-solid-state batteries
A bulk-type ASSLIB is comprised of compressed cathode/anode and solid
electrolyte layer. The electrolyte is the key component of ASSLIBs, which decides the
migration of lithium ions in batteries. Generally, a cathode of ASSLIBs composes of
active material, solid electrolyte and conductive additive, which form continuous
lithium ion and electron conducting paths to active material to ensure both high ionic
and electronic conductivities of the electrode. Because the sulfide electrolyte layer is
easy to decrease grain-boundary resistance by conventional cold-press of electrolyte
powders, the ASSLIBs can be assembled through simple fabrication processes.
3.1 Cathode
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low cost.
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Chemistry - A European Journal
3.1.1 Sulfur and lithium sulfide
Lithium-sulfur batteries (LSBs) with a high theoretical energy density (2600 Wh
Kg?1) are regarded as one of the most promising candidates to meet the growing
application demands [65-70]. However, despite great progress, their extensive application
effect leads to low active material utilization and poor cycling stability [71]. Although
new structures and technologies [72,73] have been explored, the shuttling problem is not
fundamentally solved. Replacement of liquid electrolytes with solid electrolytes is an
excellent solution [74-76]. Solid electrolytes can not only completely prevent polysulfide
diffusion, but also block dendrite growth, resulting in high stability and safety [77-79]. In
addition, sulfur is suitable to be employed as cathodes for ASSLSBs with sulfide
inorganic electrolytes because sulfur is more compatible with the electrolytes than
others.
However, sulfur has poor electronic and ionic conductivities, which is
unsatisfactory for the cathode of ASSLSBs [80, 81]. Therefore, sulfur incorporating with
electronic conductive materials and solid electrolytes to form a composite cathode is a
useful strategy to enable both high electronic and ionic conductivities. Nagao et al.[82]
developed sulfur-composite cathodes in ASSLSBs. The cathodes were prepared by
mechanical milling of sulfur particles with acetylene black and Li2S-P2S5 glass-ceramic
electrolyte at high temperature. Because of the large contact area among sulfur,
acetylene black and solid electrolyte, the ASSLSBs fabricated using the composite
electrodes exhibited excellent cycling stability (1050 mAh g?1 for 50 cycles) and good
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is still restrained by the shuttle effect of soluble polysulfide intermediates. The shuttle
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Chemistry - A European Journal
rate capability. In addition, reducing the sulfur particle size is able to improve the
contact area with electronic and ionic conductive materials. Nagao et al.[83] found that
a reduction in particle size of composite electrode materials could be controlled by
mechanical milling. The small particles improved the contact among the electrode
another problem that is the volume expansion. Because the contact at interface in
ASSLSBs is solid-to-solid, the volume change during cycling easily leads to poor
contact, resulting in fast capacity deterioration. Recently, Yao et al.[84] reported a unique
sulfur cathode fabricated by deposition on reduced graphene oxide (rGO) to improve
the electronic conduction and reduce the stress/strain from volume change. The
ASSLSBs with rGO/S cathode show a high initial discharge capacity of 1629 mAh g?1
at 0.05 C and excellent cycling stability (830 mAh g?1 after 750 cycles at 1 C) (Figure
4). They further investigated the reaction mechanism of sulfur electrode in ASSLSBs.
Unlike the traditional liquid LSBs, ASSLSBs conforms the direct electrochemical
reaction S + 2Li+ + 2e
?
Li2S during the discharge process, without producing
polysulfide intermediates through the analysis of CV curves. Lack of comparable
system studies of the reaction mechanism in ASSLSBs, further work is needed to clarify.
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components to enhancement of the capacities of ASSLSBs. Also, sulfur cathode has
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Chemistry - A European Journal
(a)
(b)
(d)
(e)
Figure 4. (a) Cyclic voltammogram of rGO@S-40 composite in all-solid-state cell at 60 癈. (b)
Galvanostatic discharge/charge profiles for rGO@S-40 composite in all-solid-state cell at different
rates at 60 癈. (c) Cycling performances of rGO@S-40 composites at 1.0 C and corresponding
Coulombic efficiencies at 60 癈. Photograph of the Li?S full cells (d) before and (e) after 750 cycles
at 1.0 C and 60 癈.[84]
Li2S is also regarded as a promising material for LSBs due to its high theoretical
capacity of 1168 mAh g?1 without volume expansion. In addition, it can be used as an
anode that does not have lithium sources [85]. However, Li2S has low electronic and
ionic conductivities same as sulfur. Han et al. [81] reported a novel bottom-up method to
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(c)
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Chemistry - A European Journal
synthesize
a
nanocomposite
by dissolving
Li2S
as
the
active
material,
polyvinylpyrrolidone (PVP) as the carbon precursor, and Li6PS5Cl as the solid
electrolyte (Figure 5). The addition of carbon black and Li6PS5Cl in the cathode forms
multiscale electronic/ionic conducting networks, thus the cathode delivers a high
investigated the performance of ASSLSBs based on the small particle size of Li2S
electrodes. Reducing the particles size was effective for improving their reversible
capacity and rate performance.
(a)
(b)
(c)
Figure 5. (a) Schematic illustration of the bottom-up synthesis of the mixed conducting Li2S
nanocomposite. (b) Cycling performances of Li2S?C and Li2S?Li6PS5Cl?C nanocomposite
electrodes at 50 mA g?1. (c) Charge/discharge profiles of Li2S?Li6PS5Cl?C nanocomposite
electrode at various current densities from 50 mA g?1 to 400 mA g?1.[81]
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reversible capacity (830 mAh g?1 for 60 cycles at 50 mA g?1). Nagao et al.[86]
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In order to improve the performance of ASSLSBs based on sulfur or lithium sulfide,
the effective ways are to combine electronic-conductive additive and ionic-conductive
additive in cathodes, decrease the particle size of active materials, and build 3-D carbon
3.1.2 Metal sulfides
Recently, metal sulfides have been attracted much attention in application of
ASSLIBs because of their high electrochemical activity, excellent electronic
conductivity, high theoretical capacities and mild operating voltages [87, 88]. Moreover,
metal sulfides show superior compatibility combined with sulfide electrolytes and
exhibit a highly reversible intercalation reaction with lithium. For example, the
nanocomposite electrodes prepared by ball-milling of TiS2 and Li2S-P2S5 electrolyte
for ASSLIBs exhibited a high initial discharge capacity of 840 mAh g?1 at 50 mA g?1,
benefiting from the formation of an amorphous Li-Ti-P-S phase, size control of
electrodes, and homogeneous distribution of solid electrolyte and TiS2 during the
controlled ball-milling process [89]. Chen et al.[90] mixed MoS2 with Li6PS5Br and super
P carbon to form a composite cathode. The resulting ASSLIBs displayed a capacity of
270 mAh g?1 up to 700 cycles at 0.2 C at 70 癈 with a high Coulombic efficiency.
However, the large particle size of MoS2 is the limiting factor to enhance the reversible
capacity. Recently, Co9S8 nanoparticles synthesized by a solution-based precipitation
exhibited a capacity of 151 mAh g?1 at 0.38 mA?1 cm2 after 50 cycles [91]. To improve
cycling stability and rate performance, the Co9S8-Li7P3S11 nanocomposites were
prepared by anchoring Li7P3S11 electrolyte particles on Co9S8 nanosheets. As a result,
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structure to accommodate volume change.
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Chemistry - A European Journal
the ASSLIBs showed a high capacity of 421 mAh g?1 at 1.27 mA?1 cm2 after 1000
cycles.
As mentioned above, metal sulfides have good electronic conductivity so that they
do not need extra electronic-conductive additive in cathodes. The only problems for
solid-electrolyte in cathode and designing suitable interfacial architecture can lead to
advances in the development of ASSLIBs with metal sulfides.
3.2 Anode
3.2.1 Lithium metal
Metallic lithium has an extremely high theoretical specific capacity of 3860 mAh
g?1 and the lowest negative electrochemical potential. However, the metallic lithium is
active and easy to form lithium dendritic, leading to the internal short circuits. Many
works to form protective films on the surface of metallic lithium have been reported in
liquid batteries
[92-95]
. Although the protective films restrain the growth of lithium
dendritic, the security of batteries with lithium metal anodes is still very low. ASSLIBs
with solid electrolytes can use lithium metal anodes directly, greatly improving their
security and energy density. However, there are many chemical, electrochemical and
mechanical stability issues at the interface between lithium metal and solid electrolyte.
Certainly, the electrochemical stability of solid electrolyte can be affected by its
composition. Tao et al.[42] investigated the substitution of P2O5 for P2S5 in 70Li2S30P2S5 glass-ceramic. The 70Li2S-29P2S5-1P2O5 shows higher electrochemical
stability than 70Li2S-30Li2S and it is completely compatible with metallic lithium, as
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metal sulfides are the poor ionic conductivity and interface issue. Therefore, adding
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Chemistry - A European Journal
shown in Figure 6. Therefore the assembled ASSLIBs with 70Li2S-29P2S5-1P2O5
exhibited better electrochemical performances than those with the pristine electrolyte.
Sun et al.[96] reported the oxygen substitution effects in Li10GeP2S12 electrolytes. The
partial substitution of oxygen for sulfur (Li10GeP2S12-xOx) not only improves the ionic
metal electrodes in ASSLIBs, Kato et al.[97] developed a modification method by
depositing Au thin film between lithium metal and Li2S-P2S5 electrolyte. The insertion
of Au film improved the utilization of lithium metal and ensured the stability of metallic
lithium with sulfide electrolyte.
3.2.2 Lithium alloys
Due to the instability of lithium with sulfide electrolytes, researchers use lithium
alloys instead of lithium metal in ASSLIBs. Lithium alloys, such as Li-In [98], Li-Al [99],
Li-Si [100] are good candidates for negative electrodes because of their high capacities
and safety. Despite indium is included in the rare metal, Li-In is the most commonly
used alloy because its potential is almost constant (0.62 V vs. Li/Li+) and the
electrochemical reaction is reversible. Nagata et al. used Li-In alloy as anode in
ASSLSBs and the molar ratio of Li-In is 0.79 [101]. The cells showed a high initial
capacity of 1096 mAh g?1 with excellent cycling stability in the voltage range of 0.5?2.5
V. Employing lithium alloys is an effective method to dramatically improve the
interfacial stability between anodes and solid electrolytes.
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conductivity but also enhances the electrochemical stability. To further protect lithium
(a)
(b)
(c)
(d)
Figure 6. (a) Cyclability of 75Li2S-25P2S5 glass-ceramics. (b) Cyclability of 75Li2S-24P2S5- 1P2O5
glass-ceramics. (c) Charge-discharge curves and (d) Cycling performance of all-solid-state cell
Li/75Li2S-(25-x) P2S5-xP2O5/LiCoO2 (x = 0% and 1%) at 25 癈.[42]
The interfacial stability between electrolytes and anodes is a significant factor to
achieve high-performance ASSLIBs. Modifying the composition of solid electrolytes
or employing lithium alloys as anodes are useful ways to enhance the stability of sulfide
electrolyte versus lithium metal.
3.3 Interface
3.3.1 Interface phenomena
Due to the solid-solid contact between electrode material and electrolyte, the large
resistance exists at the interface, which limits the transport of lithium ions [102-105]. In
addition, the stress/strain at interface dramatically increases because of volume change
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Chemistry - A European Journal
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of some electrodes during cycling, loose contact or interface separation occurs. As a
result, the ASSLIBs show poor cycling stability or even become damaged. Recently,
there are several methods developed to intimate the interfacial contact between
electrode and electrolyte: (1) Reduce the particle sizes of active material and electrolyte;
cathode; (4) Construct reasonable interfacial architecture.
3.3.2 Interface modification
Modification of the interface between solid electrolyte and electrode can
effectively imitate the interfacial contact and decrease the interfacial resistance. (1) As
for the particle size, Hayashi et al.[106] prepared nanosized NiS electrode via a
mechanochemical reaction and the nanointerface was formed between the electrode and
electrolyte. This method obtained a good solid-solid interface for fast transport of
lithium ions due to the reduced size of NiS. The ASSLIBs with the nanocomposite
electrode exhibit high capacity and good cycling stability. (2) ASSLIBs employed
sulfide electrolytes are ordinarily assembled by cold-pressing. Although this method is
very convenient, it still exists space at interface, resulting large interfacial resistance.
Busche et al.[107] reported that the interfacial resistance could be lowered considerably
by hot-pressing during the preparation procedure of ASSLSBs. By introduction a hotpressing process, the grain boundary and interfacial resistance could be significantly
reduced, enabling a continuous transport channel in batteries. The assembled ASSLSBs
achieved a high sulfur utilization (1370 mAh g?1) in the first cycle and showed a good
cycling stability. This study provides an effective method to reduce interfacial
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(2) Introduce hot-pressing during preparation; (3) Add ionic-conductive materials in
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resistance and intimate the contact between sulfur cathode and electrolyte for the
construction of high-performance ASSLSBs. (3) In addition, cathodes need to possess
high contact area with electrolyte to arrive high utilization of active materials. Many
electrodes have low ionic and electronic conductivities thus efforts have been done to
solid electrolyte and carbon materials. Certainly, the way for mixing of solid electrolyte,
carbon and active materials affects the combination of the three ingredients. Hakari et
al.[108] compared the electrochemical performance of composite electrodes prepared by
hand grinding and ball milling. The electrode prepared by milling showed much higher
performance than that by grinding, due to the intimate contact and the increase in
lithium ion paths at interface. Now the strategy of mixing active materials, electronicconductive additive and solid electrolytes by ball milling has been widely applied in
the preparation of cathodes for ASSLIBs. (4) Recently, interfacial architecture has been
developed to further optimize interface. To achieve interface contact, the sulfide
electrolyte is directly coated on the surface of active materials. Aso et al.[109] reported
that a highly conductive 80Li2S-20P2S5 electrolyte was coated on NiS-VGCF
composite by pulsed laser deposition to form intimate solid-solid contacts between the
cathode and electrolyte (Figure 7). The electrolyte coating gave the favorable lithium
ion conduction paths in the working electrode. As a result, the SE-coated NiS-VGCF
composite showed a high initial discharge capacity of 300 mAh g?1, and much better
cycling stability than the counterpart without NiS-VGCF coating.
22
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improve both the contact area and the ionic/electronic conductivity by incorporating
(a)
(b)
(c)
(d)
Figure 7. (a) Schematic illustration of SE-coated NiS-VGCF composite. (b) Cycle performance of
all-solid-state cell using uncoated or SE-coated NiS-VGCF composites. Charge?discharge curves
of all-solid-state cell using (c) uncoated or (d) SE-coated NiS-VGCF composite.[109]
ASSLIBs with sulfide solid electrolytes are on their way toward achieving small
interfacial resistance and high stability/compatibility. Present studies mainly focus on
the contact modification between electrolyte and cathode by reducing particle size,
introducing hot-pressing, adding ionic-conductive materials and construction
reasonable interfacial architecture, which expand fundamental understanding and guide
the design of ASSLIBs. As for the future research direction, more attention can be paid
on the interface between electrolyte and anode and how to realize the ASSLIBs in largescale applications.
23
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4. Conclusions and perspectives
To summarize, all-solid-state battery becomes a promising candidate for next
generation of energy storage devices due to its improved safety, high energy density
and wide operating temperatures. However, there still exist many challenges for
conductivities and poor stability with lithium/air, and large interfacial resistance
between cathodes and electrolytes, large volume change in electrodes for ASSLIBs
during cycling. Many efforts have been done to improve ionic conductivities of
electrolytes and overcome the problems mentioned above in ASSLIBs. (1) Enhancing
the ionic conductivities of solid electrolytes can be achieved by doping of the existing
system or finding new solid electrolytes; (2) Modifying the composition of solid
electrolytes or employing lithium alloys as anodes can be improve stability of sulfide
electrolytes versus lithium metal; (3) Overcoming the large interfacial resistance at
solid/solid interface between electrodes and electrolyte is a huge challenge. It would be
useful to solve the interface issues by reducing particle size, introducing hot-pressing,
adding ionic-conductive materials and construction reasonable interfacial architecture;
(4) Building 3-D construction of cathodes is an effective way to accommodate the
volume change in electrodes and decrease stress/strain during cycling. It is necessary
to ensure the imitate contact and chemical/electrochemical compatibility at solid-solid
interface, and fast/continuous lithium ion transport in ASSLIBs in order to realize high
utilization of active materials and excellent cycling stability.
The research for future directions on the exploration of advanced ASSLIBs with
24
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application of ASSLIBs employed sulfide inorganic electrolytes, such as low ionic
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Chemistry - A European Journal
sulfide electrolytes are as follows: (1) Synthesis of new sulfide electrolytes with
improved ionic conductivities for meeting the requirements of application; (2)
Enhancement of chemical stability of sulfide electrolytes in air in order to simplify
production condition; (3) Improvement of the compatibility between solid electrolyte
resistance; (5) Fabrication of novel composite cathodes with high ionic/electronic
conductivities; (6) Modification Li metal anode to decrease the resistance; (7)
Investigation of the electrochemical reaction mechanisms in ASSLIBs to guide the
design of high-performance solid batteries; (8) Exploration of novel cell configuration
design to further improve the energy density and realize high power density; (9)
Optimization of the preparation/assembly process for all-solid-state batteries. As the
most promising candidate for the energy storage devices, ASSLIBs provide advanced
safety, high energy density and long cycling stability. The future developments of
overcoming the challenges are expected to realize large-scale applications of ASSLIBs.
Acknowledgements
This work is supported by the National Natural Science Foundation of China
(51271167) and the Program for Innovative Research Team in University of Ministry
of Education of China (IRT13037).
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[104] Z. Bai, Z. Ju, C. Guo, Y. Qian, B. Tang, S. Xiong, Nanoscale 2014, 6, 3268-3273.
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