Mitigating the dissolution of V2O5 in aqueous ZnSO4 electrolyte through Ti-doping for zinc storage

Mitigating the dissolution of V₂O₅ in aqueous ZnSO₄ electrolyte through Ti-doping for zinc storage

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Zihe Wei^a^,^b^,^c, Xuehua Wang^c, Ting Zhu^b, Ping Hu^b^,^d^,^*, Liqiang Mai^a^,^b^,^d, Liang Zhou^a^,^b^,^d^,^*

Chinese Chemical Letters | 2024, 35(1) : 108421

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Chinese Chemical Letters | 2024, 35(1): 108421

• Communication •

Mitigating the dissolution of V₂O₅ in aqueous ZnSO₄ electrolyte through Ti-doping for zinc storage

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Zihe Wei^a^,^b^,^c, Xuehua Wang^c, Ting Zhu^b, Ping Hu^b^,^d^,^*, Liqiang Mai^a^,^b^,^d, Liang Zhou^a^,^b^,^d^,^*

Affiliations

^a Hubei Longzhong Laboratory, Wuhan University of Technology (Xiangyang Demonstration Zone), Xiangyang 441000, China

^b State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China

^c School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430205, China

^d Foshan Xianhu Laboratory of the Advanced Energy Science and Technology Guangdong Laboratory, Xianhu Hydrogen Valley, Foshan 528200, China

Published: 2024-01-15 doi: 10.1016/j.cclet.2023.108421

Outline

Abstract

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Aqueous zinc-ion batteries (AZIBs) have become a hotspot for electrochemical energy storage owing to the high safety, low cost, environmental friendliness, and favorable rate performance. However, the serious dissolution of cathode materials in aqueous electrolytes would lead to poor cyclability, which should be addressed before commercialization. Herein, we designed a Ti-doped V₂O₅ with yolk-shell microspherical structure for AZIBs. The Ti doping stabilizes the crystal structure and relieves the dissolution of V₂O₅ in aqueous ZnSO₄ electrolyte. The optimized sample, Ti_0.2V_1.8O_4.9, delivers a high capacity (355 mAh/g at 0.05 A/g) as well as good capacity retention (89% after 2500 cycles at 1.0 A/g). This work provides an effective strategy to mitigate the dissolution of cathode material in aqueous ZnSO₄ electrolyte for cyclability enhancement.

Key words

Aqueous zinc-ion batteries / V₂O₅ cathode materials / Aqueous ZnSO₄ electrolyte / Yolk-shell structure / Ti doping

Cite this Article

Zihe Wei, Xuehua Wang, Ting Zhu, Ping Hu, Liqiang Mai, Liang Zhou. Mitigating the dissolution of V₂O₅ in aqueous ZnSO₄ electrolyte through Ti-doping for zinc storage[J]. Chinese Chemical Letters, 2024 , 35 (1) : 108421 - . DOI: 10.1016/j.cclet.2023.108421

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Gradual replacement of fossil fuels with renewable energy is an inevitable trend for alleviating energy depletion and environmental pollution. However, most renewable energy such as solar and wind are intermittent. Developing reliable energy storage technologies is able to overcome the intermittency issue [1,2]. Aqueous zinc-ion battery (AZIB) represents a competitive technology for large scale energy storage because of the high theoretical capacity (820 mAh/g) as well as low redox potential (−0.76 V vs. standard hydrogen electrode) of Zn [3]. The mild and near-neutral aqueous electrolytes enable unique advantages of non-flammability, low cost, environmental friendliness, fast charging/discharging capability, and easy assembly of AZIBs [4–7].

A series of cathode materials have been proposed for AZIBs, including manganese oxides [8–12], vanadium oxides [13–18], prussian blue analogs [19,20], and organic compounds [21,22]. Among these materials, vanadium oxides attract special attentions due to the high capacity, rich crystal structures, and variable valence states. Take the layered vanadium pentoxide (V₂O₅) as an example, it possesses an ultrahigh theoretical capacity of 589 mAh/g [23]. However, it suffers from poor cycling stability due to the dissolution of vanadium oxide in aqueous ZnSO₄ electrolytes [24,25]. To improve the cyclability, efforts have been devoted to morphology engineering, electrolyte modification, and intercalating foreign ions/molecules into the layered structure, which are able to reduce the dissolution and stabilize the crystal structure [26–28]. For example, Yang et al. found that V₂O₅ hollow spheres outperformed commercial V₂O₅ in cyclability and rate performance due to the higher surface area of V₂O₅ hollow spheres [29]. Temple-free yolk-shell V₂O₅ demonstrated a high capacity and ideal reversibility owing to the volume expansion alleviating ability of yolk-shell structure [30–32]. Pre-intercalating various metal ions (Na⁺, Mg²⁺, Ni²⁺, Zn²⁺, etc.) and crystalline water into layered V₂O₅ could enlarge the interlayer spacings for Zn²⁺ transfer and storage [33–37]. For example, with an enlarged interlayer spacing for Zn²⁺ transfer, Ca²⁺-preintercalated V₂O₅ manifests high capacity, decent rate performance, and long cycling life [38]. In most of these studies, the improved electrochemical performances were achieved with high-price Zn(CF₃SO₃)₂ or Zn(TFSI)₂ electrolytes. Improving the electrochemical performance of V₂O₅ in low-cost aqueous ZnSO₄ electrolyte has been rarely reported [39–41].

Herein, we synthesize Ti-doped V₂O₅ yolk-shell microspheres (TVO) with tunable Ti content by a spray-drying method. 3.0 mol/L ZnSO₄ is used as the electrolyte to explore the effects of Ti doping on electrochemical performance. The yolk-shell TVO mitigates the dissolution of vanadium in aqueous electrolyte and buffers the volume change during Zn²⁺ intercalation/de-intercalation. The yolk-shell Ti_0.2V_1.8O_4.9 delivers a high capacity of 355 mAh/g at 0.05 A/g. When cycled at 1.0 A/g, 89% of the reversible capacity (211 mAh/g) can be retained after 2500 cycles. The in-situ and ex-situ characterizations reveal that the doping of an appropriate amount of Ti into the lattice of vanadium pentoxides stabilizes the crystal structure. Further increasing the Ti amount lowers the specific capacity due to the reduce of active material content. AZIB pouch cells based on the Ti_0.2V_1.8O_4.9 cathode and 3.0 mol/L ZnSO₄ electrolyte demonstrates good cyclability under deep charging and discharging conditions. Our research offered an effective means to extend the service life of AZIBs with low-cost aqueous ZnSO₄ electrolyte.

The TVO samples with different Ti contents are produced by a simple spray drying method with subsequent annealing in air. The Ti_0.2V_1.8O_4.9 displays an X-ray diffraction (XRD) pattern resembled to that of V₂O₅ (Fig. 1a). The characteristic peaks at 15.3°, 20.2°, 21.6°, 26.1°, 30.9°, 32.3°, 33.2° and 34.2° are associated with the (200), (010), (110), (101), (400), (011), (111) and (301) diffractions of the orthorhombic phase V₂O₅ (PDF No. 96–901–2221). For Ti_0.5V_1.5O_4.75, besides the diffractions from the V₂O₅ phase, additional obvious diffractions at 25.3° and 27.4° associated with the (101) plane of anatase TiO₂ (PDF No. 96–900–9087) and (110) plane of rutile TiO₂ (PDF No. 96–900–4143) can also be detected. The results indicate that doping a low content of Ti (Ti/(Ti + V) ≤ 10%) does not change the crystal structure of V₂O₅, while doping too much Ti (25%) leads to the formation of residue phases. The diffraction peaks located at 19.5°–21° are enlarged in Fig. 1b. For V₂O₅, the (010) diffraction peak is located at 20.17°. When 10% Ti is doped, the diffraction shifts to 20.29°, while it shifts back to 20.23° when the Ti content is increased to 25%. It should be mentioned that although the Ti⁴⁺ (61 pm) has a larger ionic radius than the V⁵⁺ (54 pm), both the Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 show a reduced (010) lattice spacing compared to V₂O₅, indicating the existence of tensile stress in the Ti-doped samples [42,43]. According to the Bragg equation (d = nλ/2sinθ), the (010) lattice spacing of V₂O₅, Ti_0.2V_1.8O_4.9, and Ti_0.5V_1.5O_4.75 are calculated to be 4.40, 4.37 and 4.38 Å, respectively (Table S1 in Supporting information). The grain size of the samples can be determined by Scherrer equation (D = Kλ/βcosθ). The grain sizes for V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 are determined to be 26.3, 17.9 and 22.7 nm, respectively. The XRD Rietveld refinement results of Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 are provided in Fig. S1, Tables S2 and S3 (in Supporting information). From the Rietveld refinement results, one can know that the doped-Ti occupies the V sites.

Fig. 1c presents the X-ray photoelectron spectroscopy (XPS) spectra of the samples. Both V⁴⁺ (515.9 and 523.8 eV) and V⁵⁺ (517.4 and 525.0 eV) exist in the three samples. The V⁴⁺ content is 12.43% in V₂O₅ and it increases with the increasing of Ti amount. For Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75, the V⁴⁺ contents are 18.14% and 22.69%, respectively. The existence of V⁴⁺ suggests the formation of oxygen vacancies in the TVO samples to keep charge neutrality [44]. The V₂O₅, Ti_0.2V_1.8O_4.9, and Ti_0.5V_1.5O_4.75 show almost identical Raman spectra (Fig. 1d). The characteristic peaks at 478 and 697 cm⁻¹ are corresponded to the bending vibration and stretching vibration of V-O-V bond. And the peaks at 405 and 994 cm⁻¹ are associated with the V=O bonds [42,45]. To further study the effects of Ti doping, electron paramagnetic resonance (EPR) has been conducted. All three samples present a peak at g = 2.002 (Fig. 1e), suggesting the presence of oxygen vacancies. The signal increases obviously with Ti doping amount, demonstrating that the substitution of V⁵⁺ with Ti⁴⁺ is accompanied by the introduction of oxygen vacancies for charge compensation [46].

N₂ adsorption-desorption isotherms of the three samples (Fig. S2 in Supporting information) all match with IV-type isotherm with H3 hysteresis loop [47]. The V₂O₅ shows a pore size centered at ~2.4 nm, while the Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 show a bimodal pore size distribution (Fig. 1f). Table S4 shows the BET surface areas of the samples. The Ti_0.2V_1.8O_4.9 possesses the highest surface area (27.05 m²/g), while the V₂O₅ and Ti_0.5V_1.5O_4.75 show surface areas of 18.54 and 15.85 m²/g, respectively. As for the pore volume, the V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 show pore volumes of 0.10, 0.08 and 0.04 cm³/g, respectively.

Scanning electron microscope (SEM) images show that the obtained V₂O₅ (Fig. 2a and Fig. S3a in Supporting information) has a porous spherical structure built up with interconnected nanoparticles with sizes of 50–100 nm. Between the interconnected nanoparticles, there are rich large pores with sizes of tens of nanometres. From a broken microsphere, a porous yolk can be observed below the porous shell, demonstrating the yolk-shell structure. Transmission electron microscopy (TEM, Fig. 2b) further verifies the yolk-shell structure of V₂O₅. High-resolution TEM (HRTEM, Fig. 2c) image shows clear lattice fringes from the (010) planes of orthorhombic V₂O₅. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) image and the corresponding elemental mappings show that the yolk of yolk-shell V₂O₅ contains a hollow cavity in the center. Energy dispersive X-ray spectroscopy (EDS) elemental mappings (Fig. 2d) show that the V and O elements distribute homogeneously in the yolk-shell microspheres.

With the introduction of 10%–25% of Ti, the yolk-shell structure of the samples can be well maintained (Figs. 2e,f,i and j), while the large mesopores on the surface disappear. With the introduction of 10% Ti, the grain size of the sample decreases noticeably (Fig. S3b in Supporting information), agreeing well with the XRD results. Further increasing the Ti content from 10% to 25%, the grain size increases obviously (Fig. S3c in Supporting information), which is responsible for the decrease of surface area. Different from the yolk-shell V₂O₅ which possesses a hollow cavity in the yolk (Fig. 2b), both the Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 possess a solid spherical yolk (Figs. 2f and j). HRTEM confirms the high crystallinity of both Ti_0.2V_1.8O_4.9 (Fig. 2g) and Ti_0.5V_1.5O_4.75 (Fig. 2k). EDS elemental mappings (Figs. 2h and l) show that the Ti distribute homogeneously in the yolk-shell microspheres, demonstrating the successful doping.

To study the effect of Ti doping on the electrochemical performance, charge-discharge tests were performed in CR-2025 type coin cell with mild 3.0 mol/L ZnSO₄ electrolyte. Representative cyclic voltammetry (CV) curves of the samples are presented in Fig. S4 (Supporting information). The non-overlapping feature of CV profiles and gradual increasing of enclosed CV area indicate that all three samples experience a similar activation process. The transformations in peak position and peak intensity can be ascribed to the structure evolution of V₂O₅ to Zn_xV₂O₅⋅nH₂O during the cycling, which is common for vanadium oxide based cathode materials [48–50]. After five CV cycles, all three samples show two pairs of redox peaks at ~0.58/0.78 V and 0.87/1.15 V (Fig. 3a).

The galvanostatic charge discharge (GCD) curves of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 at 0.2 A/g are presented in Fig. 3b and Fig. S5 (Supporting information), and the cyclic performances of V₂O₅, Ti_0.2V_1.8O_4.9, and Ti_0.5V_1.5O_4.75 are presented in Fig. 3c. Agreeing with the CV profiles, all three samples experience an activation process during cycling (Fig. 3c). The activation process is caused by the gradual structural evolution from layered V₂O₅ to layered Zn_xV₂O₅·H₂O with expanded interlayer spacings [51–53]. After the activation process, the Ti_0.2V_1.8O_4.9 displays two discharge plateaus at ~0.6 and 0.9 V, corresponding to the Zn²⁺ intercalation. Upon cycling, the capacity of Ti_0.2V_1.8O_4.9 increases gradually until it reaches at ~250 mAh/g after ~25 cycles, after which the capacity decreases slightly. After 200 cycles at 0.2 A/g, the capacity retains at 211 mAh/g. Both the Ti_0.5V_1.5O_4.75 and V₂O₅ show quicker capacity fading after the activation process. When cycled at 1.0 A/g for 2500 cycles, the capacity retention of Ti_0.2V_1.8O_4.9 reaches 89.4% against the highest capacity, which is much higher than those of V₂O₅ (27.9%) and Ti_0.5V_1.5O_4.75 (43.9%) (Figs. 3d and e, Fig. S6 in Supporting information).

The GCD curves of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 under a serious of current densities (0.05–2.0 A/g) are shown in Fig. 3f and Fig. S7 (Supporting information). The discharge capacities of Ti_0.2V_1.8O_4.9 reach 341, 309, 282, 249, 222 and 187 mAh/g at 0.05, 0.1, 0.2, 0.5, 1.0 and 2.0 A/g, respectively. When the current density returns to 0.05 A/g, the capacity can be recovered to 298 mAh/g (Fig. 3g). Compared to the Ti_0.2V_1.8O_4.9, the V₂O₅ and Ti_0.5V_1.5O_4.75 exhibit lower capacities at the same current densities. The above results suggest that a proper amount of Ti doping can boost the cyclability as well as rate performance of V₂O₅.

Fig. 3h presents the electrochemical impedance spectroscopy (EIS) plots and the equivalent circuit is shown in Fig. S8 (Supporting information). The R_s and R_ct stands for the solution resistance and the charge transfer resistance between the electrode/electrolyte interface, respectively. The R_ct values of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 are 54, 85 and 119 Ω, respectively.

Vanadium oxide based cathode materials generally suffer from serious dissolution in aqueous electrolytes, which causes rapid capacity decay upon cycling. To study the dissolution of active materials in electrolyte, the cathode slices are immersed in 3.0 mol/L ZnSO₄ aqueous solution, where the dissolution of vanadium based oxides can be told from the color change of the electrolyte (Fig. S9 in Supporting information). After 14 days, the solution with V₂O₅ change into light yellow, suggesting the dissolution of V₂O₅ in aqueous ZnSO₄. However, the solution with Ti_0.2V_1.8O_4.9 shows a lighter color, suggesting its mitigated dissolution.

Figs. 4a-c show the CV curves of V₂O₅, Ti_0.2V_1.8O_4.9, and Ti_0.5V_1.5O_4.75 at different scan rates. According to power law equation about the relationship between the current (i) and the scanning rate (v) [54–57]:

(1)

(2)

where a and b are adjustable parameters. When the value of b is close to 0.5, the electrochemical reaction is diffusion-controlled, while if b is close to 1.0, it indicates a capacitive-controlled process [58,59]. The b values of the four redox peaks for V₂O₅ are in the range of 0.83–1.04, while the b values for Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 are in the ranges of 0.78–0.94 and 0.69–0.90, respectively (Figs. 4d-f). The high b values (closed to 1) of all three samples suggest the capacitive-controlled electrochemical processes. With the introduction of Ti, the b value displays a decreasing trend, demonstrating that the Ti doping enhances the diffusion contribution.

To further study the structure transformation of Ti_0.2V_1.8O_4.9 during the charge and discharge process, ex-situ XPS, in-situ XRD, and in-situ Raman are conducted (Fig. 5). In discharged state, the high-resolution V 2p spectrum present three components from V(Ⅴ), V(Ⅳ) and V(Ⅲ) [60,61], with percentages of 23.68%, 61.91%, and 14.36%, respectively. In charged state, only V(Ⅴ) and V(Ⅳ) exist in the sample and their percentages are 49.01% and 50.91%, respectively (Fig. 5a). For the high-resolution Zn 2p spectra, the sample in discharged state show much stronger peaks than that in charged state (Fig. 5b). The results indicate that the Zn²⁺ is inserted into the Ti_0.2V_1.8O_4.9 accompanied by the reduction of V species during discharge and the Zn²⁺ is extracted from the material accompanied by the oxidation of V species during charge process.

Fig. 5c presents the in-situ XRD pattern, from where the (101), (011) and (301) diffractions are observed at 25.9°, 32.9° and 34.9°. During the discharge/charge processes, the diffraction peaks vary in intensity periodically, while the peak position shows negligible change. The in-situ XRD results demonstrate that the Zn²⁺ is intercalated into and extracted from the Ti_0.2V_1.8O_4.9 highly reversibly. Fig. 5d presents the in-situ Raman spectra. The O-V-O (193, 283 cm⁻¹), V₃-O (303, 524 cm⁻¹) and V-O-V (478, 697 cm⁻¹) bands weaken gradually during discharge and almost disappear when the potential reaches ~0.87 V and below. During charge, the V₃-O and V-O-V bands reappear when the voltage reach over ~1.2 V. For the V=O bands (994 cm⁻¹), it shows a same regular intensity change and shift towards lower wavenumber slightly during discharge and moves back during charge. The periodic change in the in-situ Raman spectra demonstrates the excellent reversibility of Ti_0.2V_1.8O_4.9 upon Zn²⁺ intercalation/extraction.

To verify the application potential, a pouch cell was assembled with Ti_0.2V_1.8O_4.9 cathode and 3.0 mol/L ZnSO₄ electrolyte. It shows a capacity of 236 mAh/g and 95.7% capacity retention after 100 cycles at 0.1 A/g (Fig. S10 in Supporting information). These results demonstrate that doping an appropriate amount of Ti effectively enhances the cycling stability of V₂O₅ cathode materials in aqueous ZnSO₄ electrolyte. Considering the good zinc storage performances in both coin cells and pouch cells, the Ti_0.2V_1.8O_4.9 cathode material shows a bright application prospect in AZIBs.

In conclusion, we synthesized a series of yolk-shell structured titanium vanadium oxides with different Ti content by a simple spray drying method. Doping 10% of Ti reduces the lattice spacing of V₂O₅ but does not alter the crystal structure. Introducing 25% of Ti leads to the formation of anatase/rutile residue phases. With the doping of an appropriate amount of Ti, the dissolution of V₂O₅ in aqueous ZnSO₄ electrolyte can be alleviated, leading to improved cyclability. When employed as the cathode material for ZIBs, the optimized material, Ti_0.2V_1.8O_4.9, demonstrates not only high capacity (355 mAh/g) but also ideal cyclability (89% after 2500 cycles, 1.0 A/g) in aqueous ZnSO₄ electrolyte. Ex-situ XPS, in-situ XRD, and in-situ Raman characterizations demonstrate the Zn²⁺ intercalation/de-intercalation is highly reversible in the Ti_0.2V_1.8O_4.9. This work provides an effective strategy to mitigate the dissolution issue of cathode material in aqueous electrolytes by transition metal doping.

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 supported by the National Natural Science Foundation of China (No. 52102299), the Independent Innovation Project of Hubei Longzhong Laboratory (No. 2022ZZ-18), the Guangdong Basic and Applied Basic Research Foundation (No. 2021A1515110059), and the Foshan Xianhu Laboratory of the Advanced Energy Science and Technology Guangdong Laboratory (No. XHT2020-003).

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.2023.108421.

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Year 2024 volume 35 Issue 1

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doi: 10.1016/j.cclet.2023.108421

Receive Date：2023-02-03
Online Date：2025-11-20
Published：2024-01-15

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Received：2023-02-03
Revised：2023-03-20
Accepted：2023-04-02

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^a Hubei Longzhong Laboratory, Wuhan University of Technology (Xiangyang Demonstration Zone), Xiangyang 441000, China

^b State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070, China

^c School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430205, China

^d Foshan Xianhu Laboratory of the Advanced Energy Science and Technology Guangdong Laboratory, Xianhu Hydrogen Valley, Foshan 528200, 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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Fig. 1 (a, b) XRD patterns, (c) XPS spectra, (d) Raman spectra, (e) EPR spectra, and (f) pore size distributions of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75.

Fig. 2 (a) SEM image, (b) TEM image, (c) HRTEM image, and (d) EDS mappings of V₂O₅. (e) SEM image, (f) TEM image, (g) HRTEM image, and (h) EDS mappings of Ti_0.2V_1.8O_4.9. (i) SEM image, (j) TEM image, (k) HRTEM image, and (l) EDS mappings of Ti_0.5V_1.5O_4.75.

Fig. 3 (a) The 5^th cycle CV curves of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 at 0.1 mV/s. (b) GCD profiles of Ti_0.2V_1.8O_4.9 at 0.2 A/g. (c) Cycling performance of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 at 0.2 A/g. (d) GCD curves of Ti_0.2V_1.8O_4.9 at 1.0 A/g. (e) Cycling performances of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75 at 1.0 A/g. (f) GCD curves of Ti_0.2V_1.8O_4.9 at different current densities. (g) Rate performances of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75. (h) EIS plots of V₂O₅, Ti_0.2V_1.8O_4.9 and Ti_0.5V_1.5O_4.75.

Fig. 4 The CV curves of (a) V₂O₅, (b) Ti_0.2V_1.8O_4.9 and (c) Ti_0.5V_1.5O_4.75 at different scan rates. log(i) vs. log(v) plots of (d) V₂O₅, (e) Ti_0.2V_1.8O_4.9, (f) Ti_0.5V_1.5O_4.75.

Fig. 5 (a) V 2p and (b) Zn 2p ex-situ XPS spectra of the Ti_0.2V_1.8O_4.9 recorded at different electrochemical states. (c) In-situ XRD pattern and (d) in-situ Raman spectra of the Ti_0.2V_1.8O_4.9 recorded at 0.1 A/g.

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