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Free-standing SnNb2O6@CSN film as flexible anode for high performance sodium-ion batteries
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Xuemin Yina, Tao Liua, Xiuping Yina, Xiaochen Fenga, Yiming Liua, Qinhao Shia, Xingli Zoub, Yufeng Zhaoa, *
Chinese Chemical Letters | 2023, 34(7) : 107840
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Chinese Chemical Letters | 2023, 34(7): 107840
• Communication •
Free-standing SnNb2O6@CSN film as flexible anode for high performance sodium-ion batteries
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Xuemin Yina, Tao Liua, Xiuping Yina, Xiaochen Fenga, Yiming Liua, Qinhao Shia, Xingli Zoub, Yufeng Zhaoa, *
Affiliations
  • aInstitute for Sustainable Energy and College of Sciences, Shanghai University, Shanghai 200444, China
  • bDepartment of Materials Science and Engineering, Shanghai University, Shanghai 200072, China
Published: 2023-07-15 doi: 10.1016/j.cclet.2022.107840
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Free-standing electrodes are promising candidates for flexible rechargeable batteries, toward the application of flexible energy storage devices, due to their merits of additive-free, lightweight, and high energy density. Herein, we report a free-standing SnNb2O6@CSN flexible film with SnNb2O6 encapsulated in 3D carbon skeleton nanofibers by electrospinning and carbonization processes as flexible anode for sodium-ion batteries (SIBs). The 3D carbon skeleton nanofibers serve as ion/electron transport pathway to improve the electrochemical reaction kinetics and meanwhile alleviate the volume changes of SnNb2O6 during charge-discharge processes. The as-constructed half-cell (SnNb2O6@CSN‖Na) exhibits excellent cycling stability of 99.2 mAh/g at 0.5 A/g after 950 cycles (coulombic efficiency of ~100%) and a high rate performance of 108.6 mAh/g at 10 A/g. In addition, the pouch cell can light up the LEDs at different bending angles (0°, 90°, 180°). This research shows a promising anode material for flexible energy storage electronics.

Free-standing  /  SnNb2O6@CSN  /  Anode  /  Sodium-ion batteries  /  Flexible material
Xuemin Yin, Tao Liu, Xiuping Yin, Xiaochen Feng, Yiming Liu, Qinhao Shi, Xingli Zou, Yufeng Zhao. Free-standing SnNb2O6@CSN film as flexible anode for high performance sodium-ion batteries[J]. Chinese Chemical Letters, 2023 , 34 (7) : 107840 - . DOI: 10.1016/j.cclet.2022.107840
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In recent years, environmental pollution and fossil energy crisis have triggered the rapid development of cost-effective energy storage devices. Sodium-ion batteries (SIBs) are considered as promising candidates to lithium-ion batteries (LIBs) due to their low cost and abundant resources [1-6]. Nevertheless, due to the ion radius of Na+ (1.02 Å) is larger than that of Li+ (0.76 Å), the electrode materials of SIBs exhibit sluggish kinetics and large volume changes during Na+ intercalation/deintercalation processes [7-10].
To date, the reported anode materials for SIBs include carbon-based materials [11,12], alloys [8,13], titanium-based materials [14-16] and organic materials [17]. Among them, niobium-based layered oxides (e.g., TiNb2O7, CuNb2O6, BiNbO4, SnNb2O6, ZnNb2O6 and SbNbO4) are considered as the promising anode materials due to the high theoretical capacity and excellent safety [18-21]. In particular, SnNb2O6 with forsterite structure has been widely used in the field of photocatalytic degradation due to its suitable energy band structure, special crystal structure and excellent chemical stability. In addition, SnNb2O6 is a typical layered oxide with large interlayer spacing, which can provide abundant channels for the transport of Na ions, so it is expected to be applied in Na-ion batteries [22,23]. For instance, we have previously fabricated SnNb2O6@C materials with carbon coating, which displays an outstanding electrochemical performance (67 mAh/g@10 A/g, 102.6 mAh/g@0.5 mA/g after 800 cycles) in SIBs [24]. Huang and co-workers [21] prepared SnNb2O6/amino-functionalized graphene composite by self-assembly method as anode material for SIBs, which presents a high rate performance of 118 mAh/g at 0.8 A/g and excellent cyclability of 106 mAh/g at 0.5 A/g after 1900 cycles.
However, these electrodes were prepared by slurry coating method, in which binders, conductive agents and active materials were dissolved in organic solvent and then coated on copper current collector. The preparation process is complicated, and the active materials are easily detached from the current collector after multiple folds. To solve above issues, additive- and binder-free flexible electrodes were designed. Flexible electrode is a free-standing film that integrates current collector and active materials, which is not only easy to prepare, but also can be used in flexible electronic energy storage devices. Many flexible substrates, such as graphene [25], carbon cloth [26-28], carbon nanofibers/nanotubes and so forth [7,29-34], have been investigated for flexible electrodes. For example, we have previously reported a free-standing FeP@NPC electrode with FeP nanoparticles wrapped in nanofibers for flexible anode, which can be stable working under different folding conditions [29]. Liang and co-workers [35] prepared a self-supporting composite with NiSe2 encapsulated in nanotubes as anode material, which displays significantly improved electrochemical performance. Some studies have reported that free-standing electrodes can effectively improve the electrochemical performance of batteries, but there are still some problems in the practical application of flexible energy storage devices. Therefore, designing and developing more kinds of flexible electrodes can provide more candidates for the development of flexible electronic devices. As a promising anode material, SnNb2O6 has not been reported as a flexible electrode for SIBs.
Herein, we report a free-standing 3D carbon skeleton nanofiber-encapsulated SnNb2O6 (SnNb2O6@CSN) film as anode material for SIBs by facile electrospinning and carbonization processes. The 3D carbon skeleton can not only shorten the transmission paths of electron/ion, improve the electrochemical reaction kinetics, but also prevent the active material from falling off the current collector during the charge and discharge processes. As expected, the as-synthesized free-standing SnNb2O6@CSN electrode exhibits high rate performance of 108.6 mAh/g at 10 A/g, and the pouch cell can still light up the LEDs after being folded several times, displaying that it is a promising anode material for flexible electronic devices.
As shown in Fig. 1 and Fig. S1 (Supporting information), the SnNb2O6@CSN film was prepared via multi-steps including solvothermal process, electrostatic spinning, and high temperature carbonization (Fig. S2 in Supporting information). Firstly, SnNb2O6 material was synthesized by a classical solvothermal method, and its color is yellow (Fig. S3a in Supporting information). The morphology of SnNb2O6 presents irregular lamellar structure, the average thickness of SnNb2O6 nanosheet is about 40 nm (Figs. 2a and b, Fig. S4 in Supporting information). Subsequently, the SnNb2O6 nanosheets were dissolved in polyacrylonitrile (PAN) solution to obtain SnNb2O6@PAN nanofiber film by electrospinning (Fig. S3b in Supporting information). Finally, SnNb2O6@PAN film was calcined at 700 ℃ in argon atmosphere to obtain the final products (SnNb2O6@CSN). As shown in Fig. 2c, the diameter of SnNb2O6@CSN nanofiber is 300–400 nm, and the SnNb2O6 were encapsulated inside carbon nanofibers. The optical images of SnNb2O6@CSN film in Fig. 2d exhibit the excellent flexibility at different states, indicating that the obtained SnNb2O6@CSN film possesses good self-supporting flexibility.
The microstructures of the resulting materials were characterized in detail. Figs. 2e and f show the TEM and HRTEM images of the SnNb2O6. It can be seen that there are distinct fringes with lattice spacing of about 0.36 nm, corresponding to the (111) lattice plane of SnNb2O6 [36]. Figs. 2g–i illustrate the TEM and HRTEM images of the SnNb2O6@CSN nanofiber, and it can be clearly seen that the SnNb2O6 were encapsulated in nanofibers. Moreover, the lattice fringe of SnNb2O6@CSN sample can be observed in Fig. 2i, which is consistent with the structure of SnNb2O6 nanosheet. Energy dispersive spectroscopy (EDS) mapping test was shown in Figs. 2j–o, it can be seen that carbon, oxygen, niobium and stannum are distributed in the nanofiber, manifesting that the SnNb2O6 nanosheets were encapsulated in the nanofiber.
As displayed in Fig. 3a, the XRD pattern shows that all diffraction peaks of SnNb2O6 are good matched with the foordite structured SnNb2O6 (with a typical layered structure, JCPDS No. 84-1810) and no other impure signals are detected, indicating the SnNb2O6 has high crystallinity. Nevertheless, the diffraction peaks of SnNb2O6@CSN are relatively weak, which is attributed to the carbon coating. In addition, the surface elemental composition and elemental valence states of SnNb2O6@CSN were characterized by XPS. The survey spectrum of SnNb2O6@CSN film (Fig. 3b) displays characteristic peaks of carbon, oxygen, niobium and stannum, indicating that there is no impurity in SnNb2O6@CSN. Notably, the peak intensity of C 1s is significantly stronger than that of other elements, indicating a higher carbon content in SnNb2O6@CSN film. Fig. 3c shows that the Sn 3d XPS spectrum was split into two peaks at 495.3 and 486.7 eV, which could be assigned to the Sn 3d3/2 and Sn 3d5/2 of SnNb2O6, respectively [36,37]. The Nb 3d XPS spectrum in Fig. 3d presents two characteristic peaks located at 209.9 and 207.2 eV, which can be attributed to the spin-orbit peaks of Nb 3d3/2 and Nb 3d5/2, respectively, indicating that the chemical valence state is Nb5+ [23,38]. The O 1s spectrum displays three peaks at 530.6, 531.8, and 533.5 eV, corresponding to the Nb-O/Sn-O, C-O, and C=O bonds, respectively (Fig. 3e) [39]. Fig. 3f shows that the C 1s spectrum at 284.8, 285.9, and 289.9 eV can be ascribed to the C-C, C-O and C=O bonds, respectively, which is consistent with the O 1s results [40]. The XPS spectra of the SnNb2O6 nanosheets are shown in Fig. S5 (Supporting information). In addition, the SnNb2O6 content in SnNb2O6@CSN (~44.7 wt%) was calculated by thermogravimetric analysis (TGA) in Fig. S6 (Supporting information).
The electrochemical performance of free-standing SnNb2O6@CSN electrode for sodium-ion storage behavior was investigated, half-cell was assembled using sodium metal as the counter electrode (Fig. 4a). The cyclic voltammetry (CV) tests were performed in a range of 0.01–3.00 V at 0.1 mV/s. Fig. S7a (Supporting information) shows the first three CV profiles of the SnNb2O6@CSN electrode, the reduction peaks at 0.22 V and 0.40 V in the first discharge cycle should be attributed to the decomposition of SnNb2O6 to Sn and Nb2O6 and the establishment of the solid electrolyte interface (SEI), respectively [41,42]. The two cathodic peaks located at 0.24 and 0.78 V correspond to the dealloying process of NaxSn [42]. The peaks at 1.29 V and 1.54 V are attributed to the extraction/insertion of Na+ in the Nb2O5 [43]. It is worth noting that the following CV profiles are almost coincided, demonstrating the excellent electrochemical reversibility of the SnNb2O6@CSN electrode. The CV profiles of SnNb2O6 electrode were shown in Fig. S7b (Supporting information), it is clear that some peaks are present in the CV profiles of SnNb2O6 but not in the CV profiles of SnNb2O6 @CSN. For example, a pair of peaks around 0.05–0.1 V are in good agreement with redox peaks of super P [21,44]. In addition, it can be seen that there are two weak oxidation peaks around 2.1 V and 2.4 V in the CV profiles of SnNb2O6, which should be attributed to the reaction between sodium ion and Cu2O and CuO thin layer on the surface of the copper current collector [45,46].
The electrochemical performance of the free-standing SnNb2O6@CSN electrode was investigated. The discharge-charge profiles of SnNb2O6@CSN at the voltage range from 0.01 V to 3.00 V (vs. Na/Na+) under a current density of 0.05 A/g are shown in Fig. S7c (Supporting information). The SnNb2O6@CSN electrode displays discharge and charge capacities of 570.0 and 339.1 mAh/g, respectively, with a coulombic efficiency (CE) of 59.5% in the initial cycle. A good electrochemical reversibility was achieved in the following charge-discharge cycles. However, the SnNb2O6 delivers discharge and charge capacities of 520.0 and 291.1 mAh/g, respectively, with a CE of only 56.0% in the initial cycle (Fig. S7d in Supporting information). The irreversible capacity loss could be ascribed to the formation of solid electrolyte interface (SEI) and the irreversible reduction of SnNb2O6.
To investigated the cycling stability of SnNb2O6@CSN electrode and SnNb2O6 electrode, the cycle testing was carried out at a current density of 0.05 A/g. As shown in Fig. 4b, both materials exhibit large capacity loss in the first 30 cycles, which may be related to the formation of solid electrolyte interface (SEI), the volume change of the electrode material and the irreversible reduction of the SnNb2O6 during charging and discharging [47]. The reversible capacity of SnNb2O6@CSN electrode maintains at 175.1 mA/g after 240 cycles. While the reversible capacity of SnNb2O6 is only 111.1 mAh/g after 240 cycles. Significantly, the cycling stability of SnNb2O6@CSN electrode is superior to that of SnNb2O6. The long-term cycling stability of SnNb2O6@CSN was tested at a high current density of 0.5 mA/g. As shown in Fig. 4c, the reversible specific capacity is 99.2 mAh/g with a CE of ~100% after 950 cycles, indicating excellent cycling stability of the SnNb2O6@CSN electrode. In addition, the corresponding charge-discharge profiles of SnNb2O6@CSN at the 5th, 20th, 100th, 200th and 500th cycles are shown in Fig. S8a (Supporting information). While for SnNb2O6 electrode, the reversible specific capacity remains at 62.1 mAh/g after 950 cycles (Fig. 4c and Fig. S8c in Supporting information). The rate performance and cycling stability of the pure carbon nanofibers are shown in Fig. S9 (Supporting information). Furthermore, the SnNb2O6 electrode material was obviously detached from the copper current collector after 50 cycles (Fig. S10 in Supporting information). The cross-sectional thickness changes of SnNb2O6 and SnNb2O6@CSN electrodes were calculated in Fig. S11 (Supporting information). It can be seen that the expansion rate for the SnNb2O6 is 36.1%. while the thickness of the SnNb2O6@CSN electrode after 50 cycles is smaller than that of the initial electrode, which is mainly because the initial SnNb2O6@CSN film is relatively fluffy, the SnNb2O6@CSN film becomes thinner under certain pressure during cell assembly. In addition, the SnNb2O6@CSN electrode is loose and porous (Fig. 2c), which provides a certain space for the volume change of SnNb2O6 during charge-discharge processes.
The rate performances of the SnNb2O6@CSN and SnNb2O6 materials at various current densities were displayed in Fig. 4d. The SnNb2O6@CSN demonstrates the reversible specific capacities of 335.5, 283.9, 265.6, 234.7, 207.4, 174.3, 127.7 and 108.6 mAh/g at current densities of 0.05, 0.1, 0.2, 0.5, 1, 2, 5 and 10 A/g, respectively. In addition, when the current density was returned to 0.05 A/g, the specific capacity of the SnNb2O6@CSN was restored to 308.3 mAh/g. In comparison, the SnNb2O6 exhibits the reversible specific capacities of 277.8, 218.8, 159.8, 113.3, 81.1, 56.7, 36.9 and 37.6 mAh/g at current densities of 0.05, 0.1, 0.2, 0.5, 1, 2, 5 and 10 A/g, respectively. Subsequently, the specific capacity was restored to 216.9 mAh/g when the current density was returned to 0.05 A/g (Fig. 4d and Fig. S8d in Supporting information). Notably, the rate capacities of SnNb2O6@CSN are obviously higher than that of SnNb2O6. Particularly, the rate performance of the free-standing SnNb2O6@CSN and other reported niobium-based oxides are compared in Fig. 4e, and the detailed data are summarized in Table S1 (Supporting information). The SnNb2O6@CSN material exhibits comparable and/or even better specific capacities than that of other niobium-based oxides [21,48-55]. The excellent electrochemical performance of SnNb2O6@CSN may be attributed to the following characteristics: (1) The 3D network conductive carbon skeleton (the carbon nanofiber has a large π-conjugated system, which can improve the electrical conductivity of the SnNb2O6@CSN) can shorten the transmission paths of ion/electron and improve the electrochemical transport kinetics. (2) 3D network structure provides abundant internal spaces to alleviate the volume expansion of SnNb2O6 upon cycling.
To better understand the differences in electrochemical kinetics and charge storage mechanism between SnNb2O6 and SnNb2O6@CSN, the CV experiments were performed between 0.01 V and 3.00 V. Fig. 4f shows the CV curves of SnNb2O6@CSN at different scanning rates. The anodic and cathodic peaks are basically stable when the scan rate increases to 1.2 mV/s. On contrast, the reduction/oxidation potentials of SnNb2O6 are slightly offset as the scanning rate increases (Fig. S12a in Supporting information). The current (i) and scanning rate (υ) obey the following formula [51,56]:
where a and b are adjustable parameters. the b-value of 0.5 indicates a diffusion-controlled process, whereas b-value of 1 denotes the surface capacitance process. As shown in Fig. 4g, the b-values of the anodic and cathodic peaks for SnNb2O6@CSN electrode are 0.92 and 0.94, showing a dominated surface capacitive behavior. While the b values of the cathodic and anodic peaks for SnNb2O6 are 0.99 and 0.66, respectively, manifesting that the charge storage mechanism is co-controlled by capacitance and diffusion process (Fig. S12b in Supporting information). To quantitatively determine the contribution ratio of capacitance and diffusion-controlled in SnNb2O6@CSN, the following equation was used [24,57-59]:
where i is the total current at a fixed voltage, and k1 and k2 are adjustable parameters. As shown in Fig. S12c (Supporting information), the CV curve was quantitatively divided into surface capacitance (k1υ) and diffusion-controlled process (k2υ1/2). Based on this, Fig. 4h shows the contribution ratio of capacitance and diffusion-controlled of SnNb2O6@CSN at different scanning rates. It can be seen that 73% of the total capacity comes from the capacitance contribution at a scan rate of 0.1 mV/s, which gradually increases from 73% to 92% as the scan rate increases from 0.1 mV/s to 1.2 mV/s. While for SnNb2O6, the capacitance contribution is only 27% at 0.1 mV/s (Fig. S12d in Supporting information), which increases up to 59% when the scan rate increases to 1.2 mV/s (Fig. S12e in Supporting information). Obviously, the capacitance contribution of SnNb2O6@CSN is significantly higher than that of SnNb2O6. The results indicate that the 3D carbon skeleton can improve the capacitive process of SnNb2O6@CSN, which is beneficial to accelerate the electron/ion transport kinetics.
Electrochemical impedance spectroscopy (EIS) measurement was carried out to further investigate the charge transfer kinetics of SnNb2O6 and SnNb2O6@CSN. As shown in Fig. 4i, the Nyquist plots of SnNb2O6 and SnNb2O6@CSN both consist of a semicircle in a high frequency region and a straight line in a low frequency region. The semicircle in the high frequency region corresponds to the charge transfer resistance (Rct), which is associated with the electrode reaction, and the straight line at the low frequency region represents the Warburg impedance (ZW), which is associated with the diffusion of sodium ions. Notably, the Rct of SnNb2O6@CSN (~35.3 Ω) is significantly lower than that of SnNb2O6 (~53.2 Ω), which indicates that the 3D carbon skeleton can improve the conductivity of SnNb2O6@CSN material.
GITT measurements were used to investigated the electrochemical kinetics. The Na+ diffusion coefficients (DNa+) were calculated according to the following formula:
where τ stands for the relaxation time, s. nB is the mole number of the active material, mol. VM denotes the molar volume of the active material, cm3/mol, S stands for the area of electrode, m2/g. ΔEs and ΔEt can be obtained from the GITT curves. As shown in Fig. 4j, the DNa+ values of the SnNb2O6@CSN are stable between 10−12 and 10−13 cm2/s. While the DNa+ values of SnNb2O6 (10−13–10−14 cm2/s) are obviously lower than that of SnNb2O6@CSN. This further confirms that the SnNb2O6@CSN with 3D carbon structure can effectively promote the Na+ transmission.
Inspired by the excellent flexibility of the free-standing SnNb2O6@CSN electrode, the pouch cell was prepared with NaMNNb as cathode and the as-prepared SnNb2O6@CSN as anode. Figs. S13a and b (Supporting information) display the discharge-charge curves and the cycling performance of NaMNNb//SnNb2O6@CSN pouch cell at 0.05 A/g with a voltage range from 1.5 V to 3.9 V. In order to verify the practical application of the SnNb2O6@CSN electrode in SIBs, as shown in Figs. 4k–m and Movie S1 (Supporting information), the pouch cell can maintain light up LEDs at different bending angles (0°, 90°, 180°), which exhibits that the free-standing SnNb2O6@CSN electrode has great development potential in flexible electronic devices.
In summary, the free-standing SnNb2O6@CSN film with 3D carbon skeleton was successfully prepared as anode material by electrospinning and high temperature carbonization. The 3D carbon skeleton structure can shorten the transmission paths of ion/electron, improve the electrochemical reaction kinetics, as well as solve the issue of active materials detaching from the current collector during charging/discharging. Consequently, the as-prepared free-standing SnNb2O6@CSN exhibits excellent electrochemical performance (108.6 mAh/g at 10 A/g). The pouch cell can light up multiple LEDs at different blending angles. The remarkable electrochemical performance indicates that the free-standing SnNb2O6@CSN flexible electrode has great development potential in flexible electronic devices.
Declaration of competing interest
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The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgments
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This work was financially supported by the National Natural Science Foundation of China (Nos. 51774251, 22179077), the Natural Science Foundation in Shanghai (No. 21ZR1424200), the Shanghai Science and Technology Commission's "2020 Science and Technology In-novation Action Plan" (No. 20511104003), the Hebei Natural Science Foundation for Distinguished Young Scholars (No. B2017203313), and the Scientific Research Foundation for the Returned Overseas Chinese Scholars (No. CG2014003002).
Supplementary materials
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Supplementary material associated with this article can be found, in the online version, at doi:10.1016/j.cclet.2022.107840.
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doi: 10.1016/j.cclet.2022.107840
  • Receive Date：2022-08-05
  • Online Date：2025-11-21
  • Published：2023-07-15
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  • Received：2022-08-05
  • Revised：2022-09-13
  • Accepted：2022-09-20
Affiliations
    aInstitute for Sustainable Energy and College of Sciences, Shanghai University, Shanghai 200444, China
    bDepartment of Materials Science and Engineering, Shanghai University, Shanghai 200072, China
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表12种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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