Electrochemistry Communications 131 (2021) 107119

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Electrochemistry Communications
journal homepage: www.elsevier.com/locate/elecom

Full Communication

Enhanced rate capability of Li4Ti5O12 anode material by a photo-assisted

sol–gel route for lithium-ion batteries
Chuanbao Wu a, *, Yunwei Wang b, Guangqiang Ma b, Xingwen Zheng c
a
College of Vanadium and Titanium, Panzhihua University, Panzhihua 617000, China
b
School of Biological and Chemical Engineering, Panzhihua University, Panzhihua 617000, China
c
Key Laboratory of Green Catalysis of Sichuan Province, Sichuan University of Science & Engineering, Zigong 643000, China

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

Keywords: Photo-assisted sol–gel route was developed to prepare nanostructured Li4Ti5O12 anode materials. Resulting
Lithium titanate Li4Ti5O12 powders were characterized by phase analysis, microscopic morphology observation, and cyclic
Anode charge/discharge tests. As lithium-ion battery electrode, synthesized Li4Ti5O12 material by using the photo-
Lithium-ion batteries
assisted sol–gel route shows specific capacity of 120 mAh g− 1 at 10C discharge rate. Furthermore, this mate­
Rate capability
rial retains 98% of its initial specific capacity at 0.2C after 50 charge/discharge measurements. Outstanding rate
Photo-assisted sol–gel route
capability and cycling stability of this Li4Ti5O12 material are mainly derived from grain refinement induced by
ultraviolet photo-irradiation. Therefore, this photo-assisted sol–gel route is attractive alternative method for
preparing electrode materials for high-power lithium-ion battery applications.

1. Introduction strain” structure [14].

Spinel LTO is considered the best anode material for LIBs because of
Lithium-ion batteries (LIBs) have the characteristics of high energy the high level of safety and long cycling lifetime , which are both
density, fast charging capacity, high reliability, and long life, and are attributed to its minimal volume change (<0.2%) during charge/
therefore widely used in portable electronics and electric vehicles [1–3]. discharge processes [15,16]. Moreover, spinel LTO anodes can prevent
Due to the demands of modern electronics and electric vehicle devel­ lithium dendrites from forming on their surfaces due to their higher
opment, next-generation LIBs with fast charging/discharging capacity lithiation potential (~1.55 V) [8]. However, the intrinsic kinetics of LTO
and long cycling life are increasingly desirable [4,5]. These next- significantly limit its rate capacity due to its low electrical and lithium
generation LIBs require ultra-stable electrode materials with excellent ion conductivity [16–18].
electrochemical performance [6]. Much research has been done to improve the rate performance of
Graphite is a widely used anode material in commercial LIBs on lithium titanate, including methods such as optimizing its size and
account of its cost effectiveness and eco-friendliness [7]. However, morphology, surface modification, and introduction of impurity phases
during charge/discharge cycles, uncontrollable lithium dendrite growth [15,16]. Among these methods, optimizing the size and morphology is
on the anode can puncture the membrane, causing short circuits and an important strategy to enhance the rate capability of LTO anodes. In
safety issues in batteries [8]. Moreover, the large volume change of fact, reducing the LTO grain size to the nanoscale is a very important
graphite anodes under rapid charge/discharge cycles results in a rapid strategy for high-rate applications because nanostructured LTO reduces
decline in capacity and significantly reduced cycle life because of the the transmission distance of Li+ and electrons. It is well known that there
emergence of unstable solid–electrolyte interphase [6,9]. Recently, are many ways to prepare nanostructured materials, including sol–gel,
several alternative anode ceramics such as TiO2, SnO2, Fe2O3/Fe3O4, hydrothermal, solution–combustion, and microwave irradiation
and Li4Ti5O12 have been widely studied for LIBs [10–14]. These oxide methods [19,20]. These different preparation methods significantly
ceramics have shown outstanding electrochemical performance [10]. affect the structure and morphology of their resulting electrode mate­
Particularly, the spinel lithium titanate (Li4Ti5O12; LTO) presents superb rials, affecting electrochemical performance.
stability even under rapid charge and discharge due to its unique “zero- Photo-assisted sol–gel processes can quickly decompose the organic

* Corresponding author.
E-mail address: wuchuanbao@pzhu.cn (C. Wu).

https://doi.org/10.1016/j.elecom.2021.107119

Available online 3 September 2021

1388-2481/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
C. Wu et al. Electrochemistry Communications 131 (2021) 107119

components in precursor materials to produce uniform metal–oxygen into carbon dioxide and water by ozone molecules derived from UV-
network structures, beneficial for reducing the subsequent firing tem­ irradiated oxygen, so a relatively rapid thermal decomposition process
perature, modulating material morphology, and improving the material was expected to occur. For comparison, precursor powder samples were
performance compared with traditional sol–gel processes [21,22]. placed on the heating plate in air at room temperature or at 200 ◦ C for 2
Recently, photo-assisted sol–gel methods have been successfully carried h without UV irradiation. Lastly, the precursor powders with and
out in synthesizing InGaZnO [23], YBa2Cu3O7-x [24], TiO2 [25], and without UV irradiation were fired in air at 800 ◦ C for 2 h in one batch to
LiCoO2 [26]. However, photo-irradiation in these syntheses was mainly obtain spinel LTO powders.
carried out on the precursor film or liquid phase states, and there are few
reports on photo-irradiation of powders or LTO anode materials. In this 2.2. Characterization of LTO
paper, an LTO anode was fabricated by a photo-assisted sol–gel route
and characterized as an anode material for LIB applications. It was A D8 Advance (Bruker, Germany) (Cu target) was used to detect the
verified that photo-irradiation reduced the LTO grain size and that the phases of the resulting LTO powders by powder X-ray diffraction (XRD).
UV-irradiated LTO obtained an excellent rate capability and cycle Scanning electron microscopy (SEM) experiments were performed on a
stability. Sigma 500 (ZEISS, Germany), and rough statistical analysis of grain sizes
was carried out on a SEM analysis software (Nano Measurer 1.2). A
2. Experimental Nicolet iS20-type (Thermo Fisher, America) Fourier-transform infrared
spectrometer (FTIR) was employed to detect the chemical bonding
2.1. Preparation of LTO structures in the precursor powders treated with and without UV
irradiation.
LTO precursor solution was synthesized using lithium acetate dihy­ The rate performance and cycle stability of the LTO powders were
drate and tetrabutyl titanate as raw materials, acetylacetone as a tested by using coin-type half cells (LIR2016) with LTO as the cathode,
chelating agent, and absolute ethanol as the solvent in a photo-assisted lithium metal as the anode, microporous polypropylene films (Cel­
sol–gel process. In brief, tetrabutyl titanate was added to a mixture of gard2400) as separators, and commercial 1 mol L-1 LiPF6 in EC/DMC/
acetylacetone and absolute ethanol, with tetrabutyl titanate and acety­ EMC as the electrolyte [20]. To prepare the anode electrodes, a slurry
lacetone in a molar ratio of 1:1. After briefly magnetic stirring, 1 mol% was prepared with LTO powder as the active material, acetylene carbon
excess lithium acetate dihydrate was added to offset the volatile loss of black (ACET) as the conductive agent, polyvinylidene fluoride (PVDF) as
lithium during the firing process. The solution was then stirred for 2 h at the binder (8:1:1 in weight for LTO/ACET/PVDF), and N-methyl-2-
room temperature to obtain a yellow clear LTO precursor solution. Next, pyrrolidone (NMP) as the solvent. The slurry was then uniformly blade-
the LTO sol was stirred at 70 ◦ C until the formation of the gel and then coated onto a carbon-coated aluminum current collector (40 μm in
baked at 70 ◦ C to obtain precursor powder. The precursor powders were thickness) to form an electrode using a scraper with a gap of 100 μm. The
photo-irradiated by UV light for 2 h under a low-pressure mercury lamp electrode was vacuum dried at 60 ◦ C for 12 h and then cut into discs
in air at room temperature (25 ◦ C) or at 200 ◦ C. A schematic diagram of using an eyelet machine with diameters of 15 mm. With the LTO-coated
the UV irradiation process for decomposing the organic compounds in discs as the cathode, coin-type cells were assembled in a glovebox filled
the LTO precursor powders is shown in Fig. 1. The wavelengths of the with argon gas. The rate performance and cycle stability were evaluated
UV light source (Philips TUV-8 W) were 185 nm (10%) and 254 nm by a NEWARE CT-4008 T battery testing system under different current
(90%), and the output intensity was about 14 mW/cm2. The distance densities with upper and lower cut-off voltages of 2.5 V and 1.0 V,
between the lamp and sample was 15 cm. With UV radiation, long-chain respectively.
organic groups in the precursor powder will be cleaved to short-chain
small molecules, and the short-chain small molecules will be oxidized

Fig. 1. Schematic diagram of UV irradiation process for decomposing the organic compounds in LTO precursor powders.

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C. Wu et al. Electrochemistry Communications 131 (2021) 107119

3. Results and discussion After firing at 800 ◦ C for 2 h, the LTO precursor powders, which are
amorphous, were converted to spinel LTO crystal, and their phase
To investigate the chemical bonding structure of the LTO precursor structures are shown in the XRD patterns reported in Fig. 3. The
powders, the powders were characterized by FTIR test. FTIR provides diffraction peaks of the LTO powder samples treated with and without
both qualitative and quantitative information about functional groups. UV radiation appear in the diffraction angle range of 10–70 ◦ . They are
The FTIR spectra of the precursor powders obtained under different consistent with the characteristic peaks of LTO (JCPDS Card No.
conditions are shown in Fig. 2. When the LTO precursor powder was 49–0207) and are verified as belonging to the Fd3m space group.
treated at room temperature (25 ◦ C) without UV irradiation, the bands [31,32]. No diffraction peaks of other impurity phases such as common
observed in FTIR at about 1587 and 1531 cm− 1 are ascribed to C– –O rutile TiO2 are visible, indicating that the phase purity of these LTO
symmetric and asymmetric vibration [27]. The C– – O bond chelates to samples is high. The diffraction peak intensities of the LTO powder
the metal element through a coordination bond, inhibiting the treated with UV irradiation (UV-LTO) are lower than those of the LTO
condensation of the precursor powder [27]. Therefore, this bond needs powder treated without UV irradiation (non-UV-LTO). Furthermore, the
to be decomposed to promote condensation. After 1 h of UV irradiation full widths at half maximum of the highly intense (1 1 1) and (4 0 0)
at 25 ◦ C, the peak intensity of this bond significantly decreases. The peak peaks of the UV-LTO diffraction pattern are slightly larger than those of
intensity further decreases after UV irradiation at 200 ◦ C, indicating that the non-UV-LTO diffraction pattern. These results suggest that it is likely
UV irradiation can effectively decompose the C– – O bonds in the LTO that the grain size of UV-LTO is smaller than that of non-UV-LTO due to
precursor powders. the homogeneous growth of LTO grains under UV-assisted pyrolysis.
The transmission bands at 1437, 1380, 1282, 1026, and 932 cm− 1 Fig. 4 shows the morphology and particle-size distribution of the
are attributed to CH2 bending, CH3 stretching, C–H second overtone, LTO powders fired at 800 ◦ C for 2 h. Fig. 4(a) shows that the LTO crystal
C–O asymmetric stretching, and C–O symmetric stretching, respectively grains synthesized without UV irradiation are irregularly granular and
[28,29]. The intensities of these peaks also decrease after UV irradiation. have distinct angles, indicating that this spinel LTO sample is fully
Furthermore, the peaks at 1587, 1531, and 1437 cm− 1 slightly shift crystallized when fired at 800 ◦ C for 2 h. Its average crystal grain size is
toward lower wavenumbers after UV irradiation (as denoted by the red 448.8 nm and the standard deviation is 172.5 nm, as shown in Fig. 4(c),
arrows in Fig. 2) due to the formation of disordered carbon [30]. This according to the statistical analysis of the randomly-selected 60 grains in
indicates that the long-chain organic compounds decompose to short- the SEM image. In comparison, the LTO crystal grains synthesized with
chain organic compounds after UV irradiation. Furthermore, the short- UV irradiation are dispersed small particles with an approximately
chain organic compounds are easily oxidized to CO2 and H2O, which spherical shape, as shown in Fig. 4(b). Its average crystal grain size is
leads to a decrease in the peak intensity of the C–H and C–O bonds. UV 87.7 nm and the standard deviation is 42.9 nm, as shown in Fig. 4(d),
irradiation of air converts O2 into O3, as shown in Fig. 1. During the according to the statistical analysis of the randomly-selected 100 grains
irradiation process, UV light decomposes ligands containing C– – O and in the SEM image, which shows that crystal grain growth was signifi­
C–H bonds, and O3 then reacts with and removes the decomposed cantly inhibited. This microstructure can shorten the transport pathway
components [28]. Under the combined effect of ultraviolet decomposi­ of lithium ions during the LIB charge/discharge process, which is
tion and ozone oxidation, organic species are almost completely beneficial for improving its rate capability. According to the above
decomposed under UV irradiation for 1 h at 200 ◦ C, as shown in Fig. 2. infrared analysis, grain refinement is closely related to the UV irradia­
This low-temperature thermolysis of organic species is highly signifi­ tion process. The UV irradiation will promote the formation of a uniform
cant. At low thermolysis temperatures, the precursor powder can M− O− M (metal–oxygen–metal) network, which is conducive to
maintain its amorphous state and uniform metal distribution, beneficial obtaining fine grains due to the activation of metal and oxygen atoms
for the homogeneous growth of Li4Ti5O12 grains in the subsequent firing after photodecomposition of the organic groups [24].
process. To characterize the electrochemical performance of both LTO sam­
The results of our experiments have confirmed that UV irradiation at ples, coin-type half cells were assembled with LTO as the cathode. Their
room temperature does not fully decompose organic matter, so this electrochemical performance was tested through a galvanostatic
process does not significantly improve the morphology or performance method, as shown in Fig. 5. Fig. 5(a) and (b) present the first charge/
of the resulting LTO powder. Therefore, in the remainder of the paper, discharge behavior at different rates for the non-irradiated and UV-
the changes to the structure and properties of LTO synthesized under UV irradiated LTO. A long charge/discharge platform around 1.6 V
irradiation at 200 ◦ C are investigated.

Fig. 2. FTIR spectra of LTO precursor powders treated with and without UV Fig. 3. XRD patterns of non-UV-LTO and UV-LTO powders fired at 800 ◦ C for
irradiation at different temperatures. 2 h.

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C. Wu et al. Electrochemistry Communications 131 (2021) 107119

Fig. 4. SEM images of (a) non-UV-LTO and (b) UV-LTO powders fired at 800 ◦ C for 2 h. Statistical analysis of the grain sizes for (c) non-UV-LTO and (d) UV-LTO
based on the corresponding SEM images.

Fig. 5. First charge/discharge voltage profiles at different rates for (a) non-UV-LTO and (b) UV-LTO. (c) Rate performance and (d) cycling performance of non-UV-
LTO and UV-LTO.

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C. Wu et al. Electrochemistry Communications 131 (2021) 107119

appears for both materials, corresponding to the reversible phase tran­ Sichuan Province (2020YFG0214).
sition derived from intercalation/deintercalation behavior of lithium
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