Facile synthesis of nanostructured TiNb2O7 anode materials with superior performance for high-rate lithium ion batteries

Article abstract of DOI:10.1039/c5cc07052j

One-dimensional nanostructured TiNb₂O₇ was prepared by a simple solution-based process and subsequent thermal annealing. The obtained anode materials exhibited excellent electrochemical performance with superior reversible capacity, rate capability and cyclic stability.

Full text of DOI:10.1039/c5cc07052j

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Facile synthesis of nanostructured TiNb O anode materials with
2
7
superior performance for high-rate lithium ion batteries
Received 00th January 20xx,
Accepted 00th January 20xx
a
a,b
a
a
a
a
a
Shuaifeng Lou , Yulin Ma , Xinqun Cheng , Jinlong Gao , Yunzhi Gao , Pengjian Zuo , Chunyu Du
a
and Geping Yin *
DOI: 10.1039/x0xx00000x
www.rsc.org/
+
6
2 7 2 7
One-dimensional nanostructured TiNb O was prepared by a ionic channels of TiNb O are favorable for Li mobility, leading to a
simple solution-based process and subsequent thermal annealing. good rate capability. Most important of all, the theoretical specific
-
1
The obtained anode materials exhibited excellent electrochemical capacity is much higher than Li
4 5
Ti O12, reaching 387 mA h g with a
4
+
3+
5+
4+
performance with superior reversible capacity, rate capability and 5 electron transfer process involving Ti /Ti , Nb /Nb and
4
+
3+ 16
cyclic stability.
2 7
Nb /Nb . In addition, the voltage profile of TiNb O shows a slow
rise/drop near the end of the charge/discharge processes, which is
helpful for state of charge (SOC) estimation, often based on the
open-circuit voltage, and is especially important for battery pack
Lithium-ion batteries with high energy density and power density
are promising power sources for electric devices, especially for
1
,2
electric vehicles (EVs) and hybrid electric vehicles (HEVs).
4 5
management in EV applications. In contrast, Li Ti O12 generally
Graphite is extensively used as the anode material in commercial
lithium ion batteries, but it cannot meet the demanding
requirements for high energy and high power applications due to
the low specific capacity, poor rate performance, and safety
shows a very flat voltage followed by an abrupt rise/drop near the
end of the charge/discharge processes, leading to great challenges
in estimating SOC, especially when it is combined with a cathode
3
material exhibiting
Li Ti 12/LiFePO battery system. For these reasons, TiNb
expected to replace Li
for power lithium ion batteries.
In practice, however, TiNb
a
similar behavior, such as in the
concerns. Hence, it is imperative to develop electrode materials
4
5
O
4
2 7
O
is
with superior performance including high storage capacity and rate
capability.
4
5
Ti O12 as a next-generation anode material
17,18
Over the past decade, spinel Li
4 5
Ti O12 has been widely studied as an
2
O
7
also suffers from the drawback of
alternative anode material in power LIBs because of its high
+
4+
3+
poor electronic conductivity and ionic conductivity, which restricts
the electrochemical kinetics. Therefore, the great challenge now is
operating voltage of 1.55V (vs. Li /Li) from the Ti /Ti redox couple.
This avoids the formation of solid electrolyte interface (SEI) layer,
4
,5
2 7
to improve the kinetic performance of TiNb O . Recently, much
and leads to a excellent rate performance and long cycle life. In
particular, the high lithium storage potential prevents the formation
of lithium dendrites, hence ensuring a high safety level. However,
work has devoted to solve the problem, thereinto, the construction
of nanostructure and porous structure are effective methods to
improve the kinetic performance by shortening the diffusion
-
1
the theoretic specific capacity of Li
4
Ti
5
O
12 is only 175 mA h g and,
+
distance of Li and increasing the contact area between electrode
therefore, the energy density is reduced relative to graphite. As a
19,20
7
and electrolyte. Electrospinning tehchnology,
template method ,
consequence, the practical application of the Li
seriously limited.
4
Ti
5
O12 anode is
8
12
self-assembly method and hydrothermal method have been
2 7
introduced to prepare the nanostructured TiNb O , such as
TiNb
Li Ti
attracts much research interest and has been extensively
2 7
O was first proposed as a novel anode material to replace
6
nanoporous structure, ordered mesoporous structure and micro-
nano hierarchical structure etc, resulting in an enhanced
electrochemical performance. However, these methods generally
need complex preparation process or strict synthesis conditions, so
4
5
O12 by Goodenough and coworkers in 2011. It subsequently
7
-15
investigated recently. Similar to Li
4
Ti
5
O12, safety is also enhanced
with an operating voltage of 1.64V in TiNb
2 7
O
. Additionally, The 2D
2 7
the synthesis of nanostructured TiNb O with more simple method
is expected.
In this communication, a simple Sol-Gel method is used to obtain
the 1D rod-shape TiNb nanomaterials (the experimental details
2 7
O
are presented in the ESI†). It has been demonstrated that 1D
nanostructures possess direct one-dimensional electronic pathways
21
for efficient charge transport. Moreover, it also can further
improve the fast transference of lithium ion in virtue of the large
22
2 7
effective contact area between the TiNb O and electrolyte. The
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Journal Name
(a)
(b)
3d (5/2 3/2)
5+
Nb
07.4eV
2
(
110)
(
003)
PDF No. 77-1374
(002)
(602)
(
113)
(
512)
(020) (1113)
005)
(
10
20
30
40
50
60
70
80
204 205 206 207 208 209 210 211 212 213
Degree (2 Theta)
Fig.1 (a) XRD pattern of nanostructured TiNb
nanostructured TiNb
Binding energy (eV)
2 7
O , (b) XPS spectra of Nb element in
2 7
O .
as-synthesized products serving as an anode for LIBs exhibit
superior rate capability and cyclability. Electrochemical results
demonstrate that the TiNb
capacity as high as 140.4 and 83.9 mA h g at charge/discharge
rates of 20C and 50C, respectively, indicating that 1D TiNb could
be a promising candidate for LIBs with high-power capability.
Fig. 1a shows the X-ray diffraction (XRD) pattern of the as-
synthesized nanostructured TiNb and its standard pattern
JCPDS: #77-1374). All of the diffraction peaks are in good
agreement with the standard XRD pattern of TiNb , confirming
the good crystallinity of the TiNb phase, which crystallizes in a
ReO structure’ and belongs to a monoclinic system (space group
C2/m) with the lattice constants a = 20.351 Å，b = 3.801 Å, c =
2 7
O could deliver an average reversible
-
1
2
O
7
2
O
7
(
2 7
O
2
O
7
‘
3
1
1.882 Å, and β =120.19° from Cava et al and Goodenough et al’s
6,23,
work.
The TiNb
2
O
7
with ReO
3
structure consists of 3×3×∞ blocks
(M=Ti, Nb) octahedra, where the
Ti and Nb atoms arrange in random order (Fig. S1a, ESI†), and each
of these blocks contains nine MO (3×3) octahedra forming straight
of edges and corners shared MO
6
6
2 7
Fig.2 (a) SEM and (b) TEM images of the nanostructured TiNb O , (c) TEM image
of the single nanorod, (d) the HRTEM image of the selected area (white box in
Fig.2c), (e) selected area electron diffraction (SAED) and (f) the simulated SAED
columns along the b-axis with columns connected by
crystallographic shear planes. Fig. S1b (ESI†) shows the bc plane of
2 7
the crystal structure. The atomic arrangements of every layer along image of TiNb O at [-110] zone axis.
the b-axis are staggered, forming a A-B-A type structure within the
unit cell. The Li ion sites are located in the (001) crystal planes as phase was indeed produced after thermal annealing.
1
6
shown in the work by Lu et al. X-ray photoemission spectroscopy The morphology and microstructure of TiNb
XPS) was employed to determine the oxidation state of the Nb, Ti using scanning electron microscopy (SEM), transmission electron
and O element in TiNb O , and the results are shown in Fig. 1b and microscopy (TEM) and high resolution transmission microscopy
2 7
O were examined
(
2
7
S2 (ESI†). It can be seen that the Nb 3d5 peak is located at (HRTEM) measurements. As shown in Fig. 2a and S4a (ESI†), the
/2
5
+
approximately 207.4 eV corresponding to Nb , in good agreement TiNb
2
O
7
mainly consists of short nanorods with 100-300 nm in
24
with the binding energies in Nb O , indicating that all of the Nb in diameter and 300-600 nm in length. The TEM images in Fig.2b and
2
5
TiNb O7 is pentavalent. The binding energies at approximately S4b (ESI†) further confirm the rodlike features. It is worth noting
2
4
63.4 eV and 459.6 eV (Figure S2a, ESI†) correspond to Ti 2p 1/2 that similar phenomenon (rodlike materials) also appears in other
4
+
28-30
and Ti 2p 3/2 respectively, indicating a normal state of Ti in the niobium based materials, such as V
x y Z 2
Nb O and Ti Nb10O29, etc,
TiNb O . The main peak of O 1s (Figure S2b, ESI†) is centered at suggesting a specific growth mechanism associated with these Nb
2
7
5
29.7 eV, which is attributed to the oxygen species in the TiNb O
containing oxides. Generally, the growth direction is concerned with
2
7
phase. The other small peak at 531.1 eV can be ascribed to oxygen the surface energy of crystal plane, which maybe decide the
2
5,26
31,32
species in hydroxyl.
To further confirm the formation of TiNb O phase, FT-IR the target for HRTEM and selected area electron diffraction (SAED)
orientation feature.
2 7
A typical TiNb O nanorod was chosen as
2
7
spectroscopy was used to reveal the bonding characteristics of the analysis to further investigate the structure and preferred
-1
-1
products (Fig. S3, ESI†). The bands at 3450 cm and 1650 cm are orientation in the particles. As shown in Fig. 2c and 2d, the whole
associated with the stretching vibrations of hydroxyl groups from rod appears to a uniform single orientation, and the axial direction
-
1
absorbed water on the surface of particles. The bands at 924 cm
of the rod is parallel to a set of carystal planes. The same structure
-
1
and 530 cm can be assigned to the stretching vibrations of the Nb- has been shown in all other rods (Fig. S5, ESI†), suggesting a
O bonds and the Nb-O-Nb bridging bonds, respectively. Finally, the consistency growth results in our products. The SAED pattern of the
bands at 694 cm and 839 cm arise from the stretching vibration of area boxed in red image (Fig. 2d) is shown in Fig. 2e along the [-110]
-1
-1
2
7
Ti-O-Ti bonds. Therefore, it is further confirmed that the TiNb O
zone axis. There is good consistency between the experimental and
2
7
2
| J. Name., 2012, 00, 1-3
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0
.20
reactions taking place at the electrodes. The initial three cycles (Fig.
3
.0
(a)
1st cycle
nd cycle
rd cycle
(b)
1st cycle
2nd cycle
3rd cycle
-1
2
3
0.15
0.10
2 7
3b) for TiNb O were recorded at a scan rate of 0.1 mV s . It can be
2.5
seen that one pair of sharp redox peaks are located at around 1.61
and 1.67 V, corresponding to the oxidation and reduction reaction
0
.05
0.00
0.05
0.10
0.15
0.20
2.0
-
5+
4+
34
of Nb /Nb couples. In addition, there is one pair of shoulder
peaks at about 1.52 and 1.56 V, which probably stems from the two
1.5
-
-
1.0
-
different niobium positions in TiNb
2
O
7
6
,
namely edge-shared
0
50
100
150
200
250
1
300
1.00 1.25 1.50 1.75 2.00 2.25 2.50 2.75 3.00
1
-
octahedral and corner-shared octahedral. The other pair of broad
Specific Capaity (mAh g )
Potential (V)
4
+
3+
5
00
50
00
50
00
50
00
50
00
120
00
350
00
250
00
50
redox peaks at 1.76 and 1.80 V can be assigned to the Ti /Ti
couple, and the broad bump in the range of 1.0–1.4 V may be
(
c)
(d)
4
3
1
4
1C
4+
3+
34
3
2C 5C 10C
Charge capacity
1C
assigned to the Nb /Nb
redox couples.
Notably, the
8
0
20C 50C
3
2
100C
phenomenon that the location of peaks in the initial cycle differs
from that in the subsequent cycles can be explained by electronic
2
60
1
2
4
0
1
100
50
0
Chargecapacity
Coulombic efficiency
2 7
structural changes of TiNb O , corresponding to the migration of
1
Diccharge capacity at 1C
2
0
5
0
Fermi level and major distortion of the Nb (Ti)-oxygen octahedrons
0
0
16
0
5
10
15
20
25
30
35
40
0
5
10
15
20
25
30
35
40
upon the insertion of lithium ions. Moreover, both the two curves
Cycle number
Cycle number
after the first cycle almost overlap completely, indicating excellent
cyclability and good kinetics of the electrode.
Fig.3 (a) Charge/discharge curves of the initial three cycles, (b) Cyclic
voltammograms of the cell containing a TiNb electrode in the potential
2 7
O
-1
window of 1.0-3.0 V at a scan rate of 0.1 mV s (c) Cycling performance and The cycling performance of TiNb
Coulombic efficiency of cells containing TiNb electrodes at 0.1C, and (d)
Capacity retention of TiNb electrodes at various rate (1 C, 2 C, 5 C, 10 C, 20 C,
0 C, 100C): discharge rate was fixed at 1C.
2
O
7
at 0.1C is shown in Fig. 3c. It is
found that the specific capacity of TiNb electrodes after 40
cycles is 229.1 mA h g , corresponding to a capacity retention of
6.6%. To further investigate the fast lithium ion transport and
capacity restoration of TiNb electrodes, we measured the
2 7
O
2
O
7
2
O
7
-1
5
8
2 7
O
simulated results (Fig. 2f). In addition, the SAED shows very sharp
diffraction spots, suggesting that the short nanorod is a single-
crystal with d-spacings of 0.342 nm and 0.374 nm, corresponding to
capacity at various rates ranging from 1 C to 50 C and then returned
to 1 C (Fig. S6, ESI†). The average charge capacities for 5 cycles are
-
1
2
26.0, 207.4, 183.3, 166.2, 140.4 and 83.9 mA h g , corresponding
the (003) and (110) crystal planes of TiNb
crystal planes have been marked in Fig. 2d, indicating that the
growth direction of the TiNb nanorod is along the (003) plane.
The electrochemical performance of the TiNb sample was
analyzed in lithium half cells. Fig.3a shows the charge/discharge
curves of TiNb during the initial three cycles at 0.1 C (C: the
2 7
O , respectively. These
to the charge/discharge rates of 1 C, 2 C, 5 C, 10 C, 20 C and 50 C,
respectively. When the rate was returned to 1 C, the average
2 7
O
-1
charge capacity recovered to 225.8 mA h g , which is nearly the
2
O
7
-
1
same as the initial charge capacity of 226.0 mA h g at 1 C,
indicating the superior electrochemical reversibility of the TiNb
electrode.
2 7
O
2 7
O
current value outputing the nominal capacity in stipulated time,
where 0.1C corresponds to the rate at which the material is fully
In order to better understand the remarkable electrochemical
performance of the TiNb O electrodes, rate tests at a fixed
-
1
2
7
discharged in 10 hour, 38.7 mA g ) between 1.0-3.0 V. The initial
-
1
-1
discharge rate of 1C were also performed, as shown in Fig. 3d.
discharge and charge capacity is 290.7 mA h g and 264.6 mA h g ,
respectively, corresponding to an initial Coulombic efficiency of
-1
Reversible capacities as high as 210.7 and 198.0 mA h g were
achieved at a charge rates of 20C and 50 C, respectively. Even at a
9
1.1%. In addition, the discharge profiles present three different
-1
higher charge rate of 100 C (38.7 A g ), a high capacity of 159.1 mA
regions: the two sloping regions (3.0→1.7 V and 1.5→1.0 V)
indicating a solid-solution reaction and one plateau region (~1.6 V)
-1
h g was still obtained. Fig. 4 shows the long-term cycling
performance of the TiNb O electrode at a charge/discharge rate of
3
3
2
7
suggestive of
characteristics are also observed on the charge profiles.
The lithium ion storage mechanism in TiNb is much more
complex than that in the simple oxides (TiO and Nb ). Cyclic
voltammetry (CV) was performed to better understand the redox
a
two phase transformation region.
Similar
1
0C after 5 cycles at 0.1 C. The capacity retention was excellent
-1
with a high reversible capacity of 123.2 mA h g retained after 500
cycles.
2 7
O
2
2 5
O
In summary, TiNb
lengths of 300-600 nm have been successfully synthesized by a
2 7
simple sol-gel method. By virtue of its unique structure, the TiNb O
2 7
O nanorods with diameters of 100-300 nm and
5
4
3
2
1
00
00
00
00
00
0
120
1
8
6
4
2
0
00
0
-
1
material exhibits high reversible capacity of 264.6 mA h g at 0.1 C,
Charge capacity
Coulombic efficiency
-1
and even achieves 140.4 and 83.9 mA h g at the charge/discharge
0
rate of 20 C and 50 C, respectively. It maintains a high capacity of
-1
10 C
1
23.2 mA h g at 10 C rate after 500 cycles. Such superior
0
2 7
performance makes TiNb O materials a highly promising candidate
0
as anode materials for lithium ion batteries with high energy and
power density.
0
50 100 150 200 250 300 350 400 450 500
This work was supported by National Natural Science Foundation of
China (No. 51472065). We thank the Center of Analysis and
Measurement of Harbin Institute of Technology. Y.M. and S.L.
Cycle number
Fig.4 Cycling performance and Coulombic efficiency of TiNb
2 7
O anode at 10 C
after 5 cycles at 0.1 C.
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would like to thank Drs. Guoying Chen and Marca. M. Doeff (LBNL) 33 B. Guo, X. Yu, X.-G. Sun, M. Chi, Z.-A. Qiao, J. Liu, Y.-S. Hu, X.-
Q. Yang, J. B. Goodenough and S. Dai, Energ. Environ. Sci.,
for discussion.
2
014, 7, 2220.
3
4. M. Wei, K. Wei, M. Ichihara and H. Zhou, Electrochem.
Commun., 2008, 10, 980.
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