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Volume 28 Issue 1
Jan.  2021
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Article Contents
Abstract
1.   Introduction
2.   Experimental
3.   Results and discussion
4.   Conclusion
Acknowledgements
References
Yue-quan Su, Xin-yue Zhang, Li-meng Liu, Yi-ting Zhao, Fang Liu, and Qing-song Huang, Optimization of battery life and capacity by setting dense mesopores on the surface of nanosheets used as electrode, Int. J. Miner. Metall. Mater., 28(2021), No. 1, pp.142-149. https://dx.doi.org/10.1007/s12613-020-2088-y
Cite this article as: Yue-quan Su, Xin-yue Zhang, Li-meng Liu, Yi-ting Zhao, Fang Liu, and Qing-song Huang, Optimization of battery life and capacity by setting dense mesopores on the surface of nanosheets used as electrode, Int. J. Miner. Metall. Mater., 28(2021), No. 1, pp.142-149. https://dx.doi.org/10.1007/s12613-020-2088-y
shu
Research Article

Optimization of battery life and capacity by setting dense mesopores on the surface of nanosheets used as electrode

Author Affilications

  • School of Chemical Engineering, Sichuan University, Chengdu 610065, China

Funds: This work was financially supported by the National Natural Science Foundation of China (No. 51771125). We thank S.L. Wang for her help with the TEM characterization
  • Corresponding author:

    Fang Liu E-mail: sculiuf@scu.edu.cn

    Qing-song Huang E-mail: qshuang@scu.edu.cn

  • Received: 09 February 2020; Revised: 02 May 2020; Accepted: 05 May 2020; Available Online: 08 May 2020
    Graphical Abstract
    • Abstract

  • Nanosheets with mesopores on the surface have been prepared using molybdenum trioxide (α-MoO3). The effect of mesopores on the performance of the electrode remains elusive. The MoO3 nanosheets obtained in this study exhibited great battery performance, including good capacity, prolonged recycling life cycles, and excellent rate performance; e.g., 780 mAh/g when charged under a super high current-density of 1000 mA/g. These nanosheets demonstrated excellent stability, maintaining a capacity of 1189 mAh/g after 20 cycles, and 1075 mAh/g after 50 cycles; thus preventing the capacity to decrease to values under the scanning rate of 100 mA/g. These high-purity MoO3 nanosheets are well-ordered and have dense mesopores on the surface; these micropores contribute to the excellent electrode performance of the host electrode materials; the performance parameters include prolonged battery life and capacity. Setting mesopores or active sites on the electrode surface can be an alternative way to obtain stable electrodes in the future.

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  • Lithium-ion batteries (LIBs) have been a trending research subject worldwide [1]. A LIB is typically composed of several key parts, such as shell, electrolyte, diaphragm, and electrode materials. The electrode material continues to be the limiting factor in determining the performance of LIBs. The structural instability of the electrode material hinders the development of LIBs. The electrode material with a highly stable, layered structure undergoes a highly reversible structural change during the ion intercalation–deintercalation process [2]. LIB electrodes should facilitate the Li-ion’s charging–discharging, as well as sufficiently harvesting the energy storage to support the prolonged life of the device. To this end, the layered material with underlying layer thickness down to atomic layer, e.g., two-dimensional (2D) material sheet, is the most desired material thickness. Previous studies [3–6] have proposed the theoretical capability of graphene to act like negative material with anode specific capacity CA of 372 mAh/g, thus suggesting that graphene can be used commercially as electrode material [7]. Recently, most of the layered materials [8–11], including 2D materials, have been adopted as electrode materials [12–14]. The pores of the layered structure are conducive to rapid ion diffusion [15]. Due to their large theoretical specific capacity, transition metal oxides with a layered structure have become attractive anode materials for LIBs [16–17]. MoO3 can be considered for economical and extensive use in future owing to its low cost, environmental friendly characteristic, and chemical stability in air. As a typical layered structure material, MoO3 comprises two sublayers [18]. These sublayers are stacked layer by layer along the [010] orientation as α-MoO3 type [19]. The tetrahedral and octahedral holes in the lattice structure are regarded as a host material to improve the properties of LIB [19–20].

    α-MoO3 is a stable 2D layered material [6,8]. It can achieve high electrochemical stability and capacity owing to its large surface area [14,21–22] and layered structure [5,9,23–27], which benefits Li-ion’s charging–discharging. MoO3 has been studied as an electrode material for a long time [21,28–32]; its capacity can reach 1000 mAh/g under the density of 100 mA/g with a life cycle of <50. However, a method to increase the capacity beyond 1000 mAh/g and simultaneously prolong the life cycle remains elusive.

    In this research, a new α-MoO3 electrode has been presented to promote the capacity to 1075 mAh/g at the scanning rate of 100 mA/g and life span to 50 cycles by introducing micropores in the MoO3 electrode nanosheets (M–MO) and by heating molybdenum sheet super-quickly (HMSQ) to ~950–1000°C within 20 s in atmospheric environment. The layered structure obtained by the HMSQ method (widely applied in the field of metallurgy) provides a channel redounded to charging and discharging of lithium ions [4,12,33–35]. By using the obtained stable layered structure as electrode material, we can provide a solid configuration for Li+ transmission [12,35], which proves that MoO3 nanosheets are very promising battery material [13–14,21–22,25,36]. So, this type of layered structure can replace traditional battery materials [37]. Therefore, we can conclude that the method proposed in this study is better than most of the traditional preparation methods, which are commonly obtained by water-bath heating method [19,21,28–29,31–32, 38–40], and the traditional preparation process is also more complicated and time-consuming [18,29,33,38].

    2.1   Material preparation

    α-MoO3 nanosheets with rich active sites on the surface are prepared via the magnetic suspension rapid heating method. The Mo sheet (17 mm × 17 mm × 1 mm, purity 99%) was placed in a high-frequency magnetic induction melting furnace (GP-35AB). Then, it was rapidly heated for 20 s and oxidized with 30 kW power in air. With increase in the reaction time and heating power, the product yield also increased.

    2.2   Characterizations

    The crystalline structure of α-MoO3 was analyzed using X-rays diffraction (XRD, Bruker D8 ADVANCE). The surface chemical constituents of the MoO3 nanosheets were analyzed via Raman spectra (Andor SR-500i). The surface morphology and microstructure of MoO3 nanosheets were observed via scanning electron microscope (SEM, JSM-7500F, JEOL Japan). The rich active sites on the surface of MoO3 nanosheets were further observed via high resolution transmission electron microscope (HRTEM, Tecnai G2 F20 S-TWIN).

    2.3   Electrochemical test

    The CR2032 button cell was used to test the electrochemical performance of active materials. The active material (α-MoO3), acetylene black, and polyvinylidene fluoride were mixed uniformly in a mass ratio of 8:1:1. In the next step, the mixture was coated with a copper foil and then dried under vacuum at 80°C for 12 h. The battery was assembled in an argon-filled glove box. Lithium metal was used as the counter electrode, and Celgard 2400 was used as the electrode separator. The electrolyte LIB315 (Hua Rong Chemical Co., Ltd.), which is a standard 1 mol/L LiPF6 solution composed of EC (Ethylene carbonate), DMC (Dimethyl cabnate), and DEC (Diethyl carbonate) (1:1:1 by volume). A Neware battery tester (Shenzhen, China) was used to perform constant-current charge–discharge performance tests at different rates on platforms of 0.01 and 3.0 V according to the mass of the active material. The zeta potential of the material was measured using a Malvern Zetasizer Nano ZS90 instrument. Simultaneously, a LIB was assembled with MoO3 powder (Guang Fu Chemical Co., Ltd., 99.99vol% Ar) under the same conditions, and the same measurements were performed.

    Lamellar MoO3 structures can be obtained by showcasing the MoO3 nanosheets of width 24.7 µm and length in centimeter (Figs. 1(a) and 1(b), and inset (a1)). The lamellar configuration can be viewed from the side, suggesting that the strips are stacked layer by layer (Fig. 1(c)). The thickness of each of these well-organized layers is ~20 nm, and the surface is full of mesopores (Fig. 1(d)). The size of the pores, which are the most probable aperture, is ~5–10 nm and known as meso-sized pores (Fig. 1(e)). The densely distributed pores can be viewed via polarized optical microscopy (POM), as shown in Fig. 1(f), by scattering different colored lights because of variation in the size and density of the pores on the surface and the varying thickness of the MoO3 nanosheets. The meso-sized pores are illustrated in Fig. 1(g), where the pores can be viewed as defective pots (circled in red in Fig. 1(g), and in insets (g1) and (g2)). Furthermore, it is found that the surface (nano-level) of the MoO3 nanosheets is uneven and has fuzzy, light-and-dark streaks, which illustrates that the material surface possesses holes (molecular-level), namely mesopores, as shown in Fig. 1(d). The MoO3 molecular layers with holes are stacked one by one. After introducing a large number of mesoporous structures on the surface of the electrode material, its cycle stability, charge–discharge capacity, and other electrochemical properties significantly improved [41–44]. Hence, it is the uneven surface of M–MO nanosheets prepared via this method having numerous active sites that may provide more access for intercalation of lithium ions during battery charging–discharging [5,9,23–27].

    Fig. 1.  Microstructure and morphologies of MoO3 nanosheets. (a, a1) The lamellar structure of MoO3 nanosheets shown via SEM. (b) Image of MoO3 nanosheets width distributions shows the width in magnitude of 24.7 µm, where the n is sample number, the x is average width, and the σ is the standard variance. (c) The layered structure can be seen from the edge via SEM, which indicates that the strips are stacked layer by layer. (d) The schematic diagram shows that the surface of sheets is full of mesopores. This figure also shows that the slices grow layer by layer, so the defects are inherited in each layer. (e) The size of the hole on this surface is concentrated at 5–10 nm and is called a medium-sized hole. V is the pore volume, and D is the pore diameter. With the pore diameter varying, the nitrogen adsorption capacity for each gram changes correspondingly. (f) The holes on the surface scatter different colors of light. These densely distributed holes can be observed by a polarizing optical microscope (POM). (g) The size of the pores (circled in red) are illustrated through the HRTEM image of the MoO3 and the holes (g1, g2) can be viewed more intuitively using the inverted fast Fourier transformation (FFT) (cross-correlation processing) method.
    DownLoad: Full-Size Img PowerPoint

    The MoO3 nanosheets are highly oriented along the [010] direction, and the peak intensities along other directions look very tiny (Fig. 2(a)), implying that the layers are stacked along [010] and have developed fully. Moreover, the curves demonstrate three main peaks with very thin full width at half maxima (FWHM), which shows that the nanosheets are well-organized. In comparison with the standard curve in Fig. 2(a), the impurity peaks can hardly be identified, which proves that α-MoO3 nanosheets are pure and thus can be used as battery electrode. Furthermore, Raman scattering characterization confirmed the pure phase of α-MoO3 (Fig. 2(b)). All the positions of Raman peaks were consistent with those of the pure phase of α-MoO3, where the main peaks at 996, 819, and 667 cm−1 are well-defined with very thin FWHM and Lorentz-fit. This shows that the α-MoO3 nanosheets are pure and well-organized. The peaks in the range of 100–400 cm−1 correspond to various phonon mode and crystal properties of α-MoO3 [30].

    Fig. 2.  Characterization of MoO3 nanosheets. (a) XRD pattern demonstrates three highest-intensity peaks arising from stacking layer by layer along [010], suggesting the high-purity and layered α-MoO3 (standard PDF # 05-0508). (b) Raman spectra showing the fingerprint of α-MoO3 with symmetric stretching mode (996 and 819 cm–1) of Mo=O and asymmetric stretch mode (667 cm−1) of O–Mo–O. (c) MoO3 XPS full-spectrum, (d) Mo 3d XPS peak fitting, and (e) O 1s XPS peak fitting.
    DownLoad: Full-Size Img PowerPoint

    The chemical properties of nanosheets and their valence state can be analyzed via X-ray photoelectron spectroscopy (XPS) (Figs. 2(c)–2(e)). The elemental structure of O and Mo are detected via full-spectrum scanning (Fig. 2(c)). The valence state can be judged via single elemental scanning. For example, Mo 3d spectrum has been adopted to index the peaks centered at 232.31 and 235.34 eV to Mo(VI) 3d5/2 and Mo(VI) 3d3/2 (Fig. 2(d)), respectively [45–46], and 235.16 and 232.58 eV to Mo(V) 3d3/2 and Mo(IV) 3d5/2 (Fig. 2(d)), respectively, which conform the oxidation state (Mo6+) of MoO3. For O 1s (Fig. 2(e)), the peak with binding energy at 530.2 eV belongs to Mo–O bond [45] and the peak at 531.1 eV (Fig. 2(e) implies adsorption oxygen or water in air [21].

    Fig. 3(a) shows the charge–discharge cycle test results of MoO3 nanosheets cell under a scanning rate of 100 mA/g, where the discharge capacity was 1075 mAh/g after 50 cycles. After a long cycle, its capacity began to decline, and it was 856 mAh/g after 90 cycles. The ideal charge–discharge cycle is a reversible process; however, in practice, due to the generation of irreversible capacity in each cycle, the coulomb efficiency (CE) is less than 100%. The coulomb efficiency of the battery in the test was higher than 94%. The cycled battery was consequently disassembled after 90 cycles, and the surface structure of the electrode was analyzed [47]. As shown in Fig. 3(a1), no obvious layered structure was observed, and the electrode surface became agglomerated [2,48–49]. Furthermore, the MoO3 nanosheets cell was also tested 50 times at scanning rates of 200, 400, and 1000 mA/g. In addition, to elucidate the effect of mesopores on the nanosheets surface, commercial-grade MoO3 powder (Guang Fu Chemical Co., Ltd., 99.99vol% Ar) was used (Fig. 4(b)). According to the lithium-ion conversion formula MoO3 + xLi+ + xe– →LixMoO3, LixMoO3 + (6 – x)Li+ + (6 – x)e− ↔ Mo + 3Li2O [21,39], the theoretical capacity can reach 1117 mAh/g [5]. As shown in Fig. 3(b), during the first 10 rounds at 100 mAh/g, the capacity is 1100 mAh/g. Then, at 200, 400, and 1000 mA/g, the capacity is 1010, 910, and 780 mAh/g, respectively. After 50 cycles, when the density is set to the initial value of 100 mA/g, its capacity can still return to 1091 mAh/g. It is worth noting that when cycling at 200 mA/g, its capacity does not decrease significantly compared to 100 mA/g (less than 50 mAh/g). This shows that when charging–discharging within 200 mA/g, the battery can still maintain a higher capacity. In comparison to MoO3 nanosheets, if the purchased MoO3 powder cells are charged at 100 mA/g, their capacity decreases dramatically, from 1470 to 315 mAh/g after 10 cycles, and maintains 166 mAh/g after 50 cycles (Fig. 4(b)), Moreover, as the SEM image shows (Fig. 4(b1)), there is a considerable difference between the structure of the purchased MoO3 powder and the structure of the MoO3 nanosheets. The purchased MoO3 powder is not like the nanosheets that are formed by stacking thinner nanosheets. Fig. 4 shows the test image of the zeta potential of MoO3 nanosheets and purchased MoO3 powder, which is obtained by dispersing 10 mg sample in 10 mL of distilled water, ultrasonic treatment for 0.5 h, and by testing using a Malvern Zetasizer Nano ZS90 equipment. The zeta potential of MoO3 powder is only −1.29 mV, whereas the value for MoO3 nanosheets is −41.0 mV. The M–MO sheets show a much higher absolute zeta potential value than that of the powder, which indicates that a higher electrode activity is obtained on surface of the sheet. In addition, the high absolute zeta potential value benefits the migration of Li-ions in the electrolyte solution [50–51] by enhancing the battery’s charge–discharge cycle stability [11,50–51]. This method provides a new idea for rapidly preparing metal oxide nanosheets so that these can be widely used in the preparation of power batteries, super capacitors, catalysts, and sensors.

    Fig. 3.  Electrochemical properties of MoO3 nanosheets. (a) Charge–discharge cycle performance and coulomb efficiency of MoO3 nanosheets (0.01–3.0 V). (a1) Surface morphology of MoO3 nanosheet electrode after 90 cycles shown via SEM. (b) Rate performance of MoO3 nanosheets (0.01–3.0 V). (c) Charge–discharge curves of MoO3 nanosheets at 100 mA/g (0.01–3.0 V). (d) Nyquist plots of MoO3 nanosheets and MoO3 powder electrodes at the open circuit voltage of 3.0 V.
    DownLoad: Full-Size Img PowerPoint
    Fig. 4.  (a) Zeta potential classes of MoO3 nanosheets and MoO3 powder. (b) The charge–discharge cycle capacity curve of MoO3 powder at 100 mA/g. (b1) SEM shows that the structure of the purchased MoO3 powder is different from the structure of the MoO3 nanosheets. It can be seen from the edge of the powder sheet that it is not a stack of thinner nanosheets.
    DownLoad: Full-Size Img PowerPoint

    Fig. 3(c) shows the charge–discharge curve of the MoO3 nanosheets battery at 100 mA/g, which shows the first five cycles and the 45th to 50th (0.01–3.0 V) cycles. In the first cycle, Li+ enters the internal structure of Mo–O layer and the van der Waals gap between the double layers of MoO6 [52–53]. During this reaction, disordered Mo metal form and Li+ from Li2O inserts into LixMoO3 [52] by enabling a high discharge capacity of 1600 mAh/g. Its capacity finally stabilized after the fifth cycle at 1100 mAh/g, which is consistent with the capacity of 1091 mAh/g at 50th cycle. Electrochemical impedance spectroscopy reflects the intrinsic interface charge transfer between the electrode–electrolyte interface [52]. Fig. 3(d) shows the Nyquist curves of MoO3 nanosheets and purchased MoO3 powder electrodes. In the high-frequency region, the diameter of the semicircle curve of MoO3 nanosheets is significantly smaller than that of the purchased MoO3 powder, which reflects much lower resistance between electrolyte solution and electrode surface for MoO3 nanosheets. At the low frequency area, slope of the curve of MoO3 nanosheets is also greater than the slope of the curve of MoO3 powders, which indicates that the diffusion ability of Li-ions in MoO3 layered structure is better than the diffusion ability of Li-ions in MoO3 powder [54–55].

    The M–MO nanosheets obtained in this study demonstrated the best life and capacity, approaching even theoretical values (Table 1) [5]. The nanosheets exhibit the best morphology among all the listed ones, demonstrating the best battery capacity. Meanwhile, the battery life increased from 20 to 100 cycles (Table 1), with capacity decreasing from 1189 to 817 mAh/g, around 69% of the original first-circle capacity.

    Table  1.  Comparison of the capacity and cycling performance based on active materials of some reported MoO3-based electrode material and as-prepared electrode materials
    Electrode Capacity / (mAh·g−1) Cycled number (current density / (mA·g−1)) Ref.
    MoO3/carbon nanobelts 1100 50 (100) [32]
    MoO3 nanoparticles 1050 20 (100) [29]
    α-MoO3/graphene 869.2 80 (50) [56]
    MoO3-x nanowire 630 20 (50) [31]
    MoO3 nanosheets 1110 30 (100) [5]
    MoO3 nanosheets 1189/1148/1075 20/30/50 (100) This work
    Note: Under a scanning rate of 100 mA/g, the capacity of the battery is 1189 mAh/g from 20 cycles, 1148 mAh/g from 30 cycles, and 1075 mAh/g from 50 cycles.
     | Show Table
    DownLoad: CSV

    Fig. 4 shows the test image of zeta potential of MoO3 nanosheets and MoO3 powder, which is obtained by dispersing 10 mg sample in 10 ml of distilled water by ultrasonic treatment for 0.5 h and by testing using a Malvern Zetasizer Nano ZS90 equipment. The zeta potential of MoO3 powder is only −1.29 mV as against −41.0 mV for the MoO3 nanosheets. The M–MO sheets show a much higher absolute zeta potential value than that of the powder, which indicates that higher electrode activity has been obtained on the sheet surface. Moreover, the high absolute value of zeta potential benefits the migration of Li-ions in the electrolyte solution [50–51] by enhancing the battery’s charge–discharge cycle stability [11,50–51].

    α-MoO3 nanosheets exhibiting micropores were grown into quasi-2D materials by heating molybdenum sheet super-quickly (HMSQ), which exhibiting micropores in the MoO3 electrode nanosheets. The MoO3 nanosheets show well-organized 2D layered morphology. As the anode of LIBs, this electrode can provide a reversible capacity of >1075 mAh/g during the first 50 cycles, even at 1000 mA/g, the capacity is 780 mAh/g. The dense mesopores on the surface behave as active sites, contributing to good lithium storage and long electrode life. This is a meaningful attempt and an important step in the exploration to achieve longer battery life and more capacity without increasing costs. Our finding provides a new idea for optimizing the electrode performance.

    This work was financially supported by the National Natural Science Foundation of China (No. 51771125). We thank S.L. Wang for her help with the TEM characterization.

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