Direct synthesis of vanadium pentoxide powder with carbon recombination as aqueous zinc-ion battery cathode

doi:10.21203/rs.3.rs-2584580/v1

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Direct synthesis of vanadium pentoxide powder with carbon recombination as aqueous zinc-ion battery cathode

https://doi.org/10.21203/rs.3.rs-2584580/v1

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Advanced energy storage technologies have been prompted by the benefits of safe, high-capacity, and stable cathode materials for aqueous Zn-ion batteries (ZIBs). Vanadium oxide has lately become a popular cathode material thanks to its advantages of a sufficient operating voltage window and a highly reversible redox reaction. However, Vanadium pentoxide has several drawbacks, including poor electrical conductivity and slow ion diffusion. To resolve these problems, orthorhombic single crystal V₂O₅ sheets were synthesized by a facile solution combustion synthesis method to improve their performance by adding C₆H₁₂O₆. As cathode materials for the ZIBs, the V₂O₅/C particles with larger surfaces and higher oxygen defects concentration are obtained with C₆H₁₂O₆ addition, which increases the dynamic performance of ion diffusion and the activity of the vanadium-based cathode. The synthesized V₂O₅/C sample exhibited the specific capacitance of 220 mAh g^− 1 (V₂O₅ is 180 mAh g^− 1) in the aqueous electrolytes at 4 A g^− 1, which exhibited a high specific capacity of 85.5% after 500 cycles with nearly 100% coulomb efficiency, indicating improved specific capacitance and cyclic stability.

Combustion synthesis

Aqueous zinc ion batteries

Vanadium pentoxide

Carbon

Oxygen defect

Aqueous zinc-ion batteries (ZIBs) have received a lot of interest for their unique advantage in aqueous zinc-ion batteries with zinc as the negative electrode. It is mainly reflected in high theoretical capacity, low redox potential (-0.76 V relative to the standard hydrogen electrode), high stability, and abundant and cheap reserves[1]. ZIBs are becoming more and more attractive due to their great security, enormous ionic conductivity, low price, and high performance showing great superiority for several decades[2, 3]. To date, cathode materials are mostly obtained from manganese-based oxides (α-, γ-phase)[4, 5], and vanadium-based materials[6, 7] which are explored for reversible Zn²⁺ intercalation. Prussian blue analogues[8, 9], including copper hexacyanoferrate and zinc hexacyanoferrate, are other relative materials that possess analogous crystalline structures[10]. Among that, vanadium pentoxides (V₂O₅) have distinct characteristics that make them ideal candidates for cathode materials, including but not limited to a conventional layered structure, abundant materials source, and high energy density. Nevertheless, Since a result of its poor electronic conductivity, the performance of V₂O₅ under high current densities is compromised, as it will result in substantial polarization[11, 12]. V₂O₅ have the limitation of large volume expansion[13], and disintegration of active species leading to poor rate capability and capacity diminishing during cycles.[14]. High-capacity transition metal oxides are hybridized with or deposited over a broad surface area of carbon in order to reduce localized stress and enhance electrical conductivity.[15]. In response to these chemical variations, vanadium pentoxide V₂O₅/C composites have been developed. Zhang et al.[16] demonstrated that the edge-rich cathodes with vertically orientated graphene (VG) nanosheets serving as templates for V₂O₅ nanosheets showed a high capacity of 370 mAh g^− 1 (at a current density of 0.2 A g^− 1) for ZIBs through hydrothermal. Chen et al.[17] reported that the high conductivity of carbon nanotubes (CNTs) are used to improve the rate capability of V₂O₅ electrode. After 6000 cycles at 5 A g^− 1, the capacity retention ratio of the V₂O₅@CNTs electrode is 72%, which is 36% higher than that of pure V₂O₅ by hydrothermal. Wang et al.[18] presented the impregnation of a porous CNT film with an aqueous V₂O₅ sol under vacuum yields a highly flexible composite film of carbon nanotube film and V₂O₅ (CNTF@V₂O₅) with high strength and high conductivity. As a result, this CNTF@V₂O₅ film delivers a high capacity of 356.6 mAh g^− 1 at 0.4 A g^− 1. It can be seen that carbon composites can improve the conductivity and electrochemical performance of cathode materials for ZIBs.

Currently, common methods have been made to synthesize vanadium oxide, including hydrothermal techniques, chemical vapor deposition, sol-gel, powder metallurgy, technique of liquid exfoliation, soft template approaches, and supercritical solvothermal reactions and so on[19–24]. Nevertheless, these processes usually involve including intricate processes including long-term aging responses, ethanol immersion processes, long waits, several washings, and heating at various steps are required to reach the end result. A simple combination method with good extensibility and should be created for practical use at a cheap cost. Solution combustion synthesis (SCS)[25] is a suitable choice for the preparation of V₂O₅/C, which is an innovative method to produce vanadium pentoxide for aqueous zinc-ion batteries. SCS has the following advantages[26–28]: (1) low experimental environment requirements; (2) simplicity and low cost of instrumentation; (3) during the heating process, the mixture is promoted to flow so that the raw materials in the reaction process are uniform; (4) fast and efficient reaction process; (5) by adjusting the settings of combustion, product compositions may be easily modified. These advantages make it succeed by adding C₆H₁₂O₆ to the combustion feedstock, and it can quickly and easily obtain carbon-containing vanadium pentoxide powder.

In this paper, the SCS strategy is proposed to fabricate the V₂O₅/C as the cathode material for the ZIBs and the structure and electrochemical performance were analyzed systematically. The C with high-conductivity is contact with the V₂O₅ particles, which significantly enhances the conductivity of the V₂O₅/C cathode. The addition of C₆H₁₂O₆ increases the oxygen defects concentration, and the oxygen defects concentration could enhance the electrochemical characteristics of the V₂O₅/C electrode.

All of the reagents were of analytical quality and are utilized in their original form without additional purification. In the course of synthesis, ammonium metavanadate (NH₄VO₃) (0.03 M) acted as a vanadium source and ammonium nitrate (NH₄NO₃) (0.4 M) and urea (CO(NH₂)₂) (0.2 M) were the oxygen and oxidizing agents. C₆H₁₂O₆ was the carbon source (0.01 M). In a 500 ml glass, dissolving all reactants with 100 ml of deionized water to create the starting solution at room temperature. It dissolved into a white turbid liquid after being stirred evenly with a magnetic stirrer. Then the glass was placed in a muffle furnace. That once majority of the water had evaporated, the solution turned into a sticky paste and combusted instantly. The combustion process only took less than one minute and a foamy product was synthesized. For comparison, the reaction without adding glucose was also prepared in the same way.

Phases of the powders were investigated by X-ray diffraction (XRD, Rigaku D/max-RB12, Japan) at room temperature. Raman spectra were recorded on a Thermo Scientific DXR2xi Raman microscope with a laser excitation source of 514 nm. Fourier transform infrared spectroscopy (FTIR) spectra were collected on a BRUKER ALPHA spectrometer from 4000 to 400 cm^− 1. X-ray photoelectron spectroscopy (XPS, PHI-5300) was utilized to examine the chemical valence composition of the product's surface components. The morphology of the powders was characterized by scanning electron microscopy (SEM, Zeiss, ULTRA 55, German) and transmission electron microscopy (TEM, FEI, Tecnai G2 F20, USA).

Electrochemical measurements were performed in the CR2032-type coin cells. Active materials were combined with acetylene black and a binder to produce the electrode (functioning electrode), PVDF, at a weight ratio of 7:2:1. The PVDF was dissolved in N-methyl pyrrolidone. The mixture was mixed with an ultrasonic stirrer and a vibrating stirrer to form a slurry and evenly applied to the Ti foil. These prepared electrode sheets were dried at 80 ℃ in the drying oven for 8 h. The mass loading of active materials is 1 mg·cm². The CR2032-type coin cells were assembled in the air for electrochemical characterization. An aqueous solution of 3 M ZnSO₄ was used as an electrolyte. The counter electrode for electrochemical testing was a Zn metal disk. Using a Neware tester, galvanostatic charge and discharge tests were undertaken (CT-4008). Cyclic voltammetry (CV) curves were collected using an electrochemistry workstation (CHI₆18D) in a voltage window of 0.2 to-1.6 V and electrochemical impedance spectroscopy (EIS) measurements in the frequency range of 0.01 Hz to 100 kHz were performed on the electrochemical workstation.

To make clear how C₆H₁₂O₆ shaped the development of the V₂O₅/C combination, The development of the morphology of V₂O₅/C composite was shown using SEM characterization. The V₂O₅ (Fig. 1a) sample exhibits the glossy structure as regular blocks, with these sheets’ average size of around 200 nm. The V₂O₅/C (Fig. 1c) product shows a flake-like structure and the sample has a sheet structure with a few small pieces. The layer is smooth, and many of the fragments formed from sheet packing around 80 nm. After a little quantity of C₆H₁₂O₆ is added, the crystal development of V₂O₅ is altered[29], resulting in the surface structure of V₂O₅/C being rather rough. It is obvious that the particle size of V₂O₅/C is smaller than that of V₂O₅.

The microstructures of V₂O₅ and V₂O₅/C were then analyzed by TEM (Fig. 1b, f). It can be seen that V₂O₅ and V₂O₅/C show a stacked sheet structure. The d-spacing of the lattice fringes is 0.34 nm, the same as the (110) plane of V₂O₅/C (Fig. 1d). Besides, SAED depicts the single-crystal structure of the compound V₂O₅/C (Fig. 1e), as (-10-1, -101, 002) diffraction points of V₂O₅/C can be observed. EDS mappings reveal a homogeneous distribution of V, O, and C throughout the structure of V₂O₅/C (Fig. 1g–i), demonstrating the successful carbon mix of V₂O₅.

Figure 2a shows the XRD patterns of the V₂O₅ and V₂O₅/C samples. All diffraction peaks correspond well to those of the layered structure V₂O₅ with lattice constants a = 11.516 nm and c = 4.3727 nm, which accords with the literature values (PDF#41-1426), and no obvious peaks of additional contaminants are seen. The results show that the two samples are crystalline-phase V₂O₅. However, the diffraction peak of (110) and (310) planes of V₂O₅/C gradually weaken together with the C₆H₁₂O₆ content. This implies that the addition of C₆H₁₂O₆ surfactant would significantly hinder the favored development of (l10) planes, which indicated a decreasing degree of crystallinity.

Figure 2c depicts the Raman spectra of various V₂O₅ samples.The α-V₂O₅ is responsible for the characteristic peaks found at 144, 198, 286, 306, 407, 473, 524, 693 and 995 cm^− 1[30]. The peaks at 995 and 693 cm^− 1 are the stretching modes of the V = O₁ bonds and V-O₃ bonds, and stretching vibration of the V–O₄ bond corresponds to 524 cm^− 1 (Fig. 2b), while the peaks at 473 and 306 cm^− 1 can be attributed to the bending vibrations of V-O₂ and V-O₄ bonds. In contrast, the vibrations at 407 and 286 cm^− 1 are attributable to the bending of the V = O₁ bonds. [VO₅]–[VO₅] vibrations correspond to the two Raman bands at 194 and 141 cm^− 1. After adding C₆H₁₂O₆, the majority of the vibrations of V-O₂ (473 cm^− 1) and V-O₄ (524 cm^− 1) stay intact. The Raman peak at 693 cm^− 1 decreases by 32%, indicating that the oxygen vacancy site is primarily at the V-O₃ bridge sites[31, 32]. The vanadium oxide matrix containing C₆H₁₂O₆ as carbon sources exhibits two major Raman scatting peaks at around 1350 and 1580 cm^− 1. The imperfection and disorder of carbon is the cause of the 1350 cm^− 1 Raman scattering peak (D-band)[13]. In addition, the SP2 atomic motion of stretching in the carbon ring or long chain results in the 1580 cm^− 1 Raman scattering peak (G-band). This illustrates the degree of graphitization of carbon-based materials[33, 34], which indicates the existence of carbon.

Through the use of X-ray photoelectron spectroscopy (XPS), the samples' chemical composition was identified, as shown in Fig. 3a. It is important to estimate the sample obtained by XPS has the vanadium valance seen in Fig. 3b. The V 2p3/2 peaks of V₂O₅ were located at 516.3 eV (V⁴⁺) and 517.5 eV (V⁵⁺) (V⁴⁺/V⁵⁺ =0.05:1). The 2p3/2 peaks of V⁵⁺ become faint, as seen by the XPS spectrum of V₂O₅/C of V, while the peaks for V⁴⁺ increase (V⁴⁺/V⁵⁺=0.1:1). The increase in V⁴⁺ ratio may be due to the introduction of oxygen vacancies in V₂O₅/C, which is consistent with the Raman speculation. To investigate further, The O1s spectra of the V₂O₅/C and V₂O₅ samples are displayed in Fig. 3c, and two distinct peaks can be seen there. The lattice oxygen of V₂O₅/C (V₂O₅), also known as the OI peak, has a binding energy of 527.3 eV, and the oxygen vacancies in the metal oxide matrix are responsible for the peak at 528.4 eV. (named OII peak)[35, 36]. V₂O₅/C has 7.5% more oxygen vacancies than V₂O₅. The oxygen defects concentration could encourage the V₂O₅/C electrode to possess superior electrochemical characteristics[35].

The CV curves of V₂O₅/C and V₂O₅ at a scan rate of 0.1 mV s^− 1 and voltage range of 0.2 − 1.6 V are shown in Fig. 4a. The redox reactions of vanadium in the various valence states led to the appearance of multiple pairs of redox peaks on the quasi-rectangular curve of the V₂O₅/C and V₂O₅ electrode. Compared to V₂O₅, V₂O₅/C exhibited a greater current density, which might be attributable to its increased surface area. It was concluded that the former had a greater electrochemical reactivity and capacity than the latter.[37]. Figure 4b illustrates the first three cycles of CV plots for the V₂O₅/C electrode within a voltage window of 0.2 − 1.6 V at a scan speed of 0.1 mV s^− 1. In the forward scan, a slight shoulder (0.93 V) is detected, followed by two strong peaks (0.87 V and 0.59 V) that demonstrate the electrochemical intercalation of Zn²⁺ into the layered structure. In the reverse scan, three peaks at 0.76, 1.05, and 1.14 V correspond to the deintercalation of Zn²⁺ ions from the multilayer framework. In the forward scan, the peaks may have been caused by continual decreases from V⁵⁺ to lower oxidation states, whereas the reverse may have occurred in the reverse scan. It is seen that the sweep of the first cycle in the CV profile has a little different peak location than the other cycles. The displacement of peaks of the first cycle can be attributed to the slow activation of the new electrode[17]. In addition, following the first cycle, the subsequent CV curves exhibit strong repeatability and similarity, confirming the excellent electrochemical reversibility of the electrode. As seen in Fig. 4c, the CV curves exhibit comparable forms at various scan speeds, indicating that the as-obtained V₂O₅/C electrode material has an outstanding pseudo-capacitive response.

Table 1

EIS fitting parameters and ion diffusion coefficients for the pristine V₂O₅/C and V₂O₅ electrodes.
	Rs [Ω]	Rct [Ω]	D_Zn²⁺ [cm² s^− 1]
V₂O₅/C	0.72	11. 27	3.85×10^− 13
V₂O₅	10. 69	29. 04	1.19×10^− 13

To comprehend the dynamics of interfacial transport in the V₂O₅/C nanosheets, electrochemical impedance spectra (EIS) are performed. As shown in Fig. 5a, Nyquist plots of both pristine V₂O₅ and V₂O₅/C nanosheets consist of a depressed semicircle in the high-to-medium frequency range and an angled line in the low-frequency range. The Nyquist charts presented in the inset of Fig. 5a are analyzed using an analogous circuit. It is possible to compute the diffusion coefficient of Zn²⁺ using the equation

$$\text{D=}{\text{R}}^{\text{2}}{\text{T}}^{\text{2}}/\text{2}{\text{A}}^{\text{2}}{\text{n}}^{\text{4}}{\text{F}}^{\text{4}}{\text{C}}^{\text{2}}{\text{δ}}^{\text{2}}$$

where A represents the surface area, n is the valence of ions, C is the zinc ion concentration in the electrolyte, F represents the Faraday constant, R is the gas constant, T is the experimental temperature, and δ is the slope determined from the fitting lines between Zim and ω^−1/2. Table 1 shows the resistance of these electrodes. V₂O₅/C has a smaller Rs and Rct than the pristine V₂O₅ because the oxygen vacancies in the V₂O₅/C electrode increase the carrier concentration and enhance the electrical conductivity of V₂O₅/C[38]. The Zn-ion diffusion coefficients may be computed using the connection between low frequencies and the real component of impedance (Fig. 5b). The Zn²⁺ diffusion coefficient of V₂O₅/C (3.85×10^− 13 cm² s^− 1) is larger than that of the pristine V₂O₅ (1.19×10^− 13 cm² s^− 1). The quicker Zn²⁺ diffusion following hydrogenation, as seen by the enhanced conductivity and smooth Zn²⁺ tunnels brought forth by oxygen vacancies[39, 40].

Comparisons of rate capability and cycle stability are illustrated in Fig. 5c and 5d. Figure 5c displays the rate performances of the V₂O₅/C and V₂O₅, the V₂O₅/C demonstrated higher rate capability with average specific discharge capacities of 287, 270, 248, and 221 mAh g^− 1 at current densities of 1, 2, 4 and 8 A g^− 1. Figure 5d shows that the efficiency of V₂O₅/C electrode and the V₂O₅ electrode arrived by more than 100 percent during the first few dozens of cycles. This is due to the activation of drainage zinc ion batteries at the beginning. The activation procedure may be broken down into the two steps listed below. Along with the charge and discharge operation, the electrolyte will enter the interior space of V₂O₅, on the one hand[41]. On the other hand, the insertion/extraction of Zn²⁺ and the phase transition of V₂O₅ produce additional new active sites[41, 42]. It can also be found that the V₂O₅/C electrode also performs better cycling capability than the V₂O₅ electrode. The specific capacity of V₂O₅/C is maintained around 220 mAh g^− 1 at 4 A g^− 1. It gradually decreased to 188 mAh g^− 1 (85.5%) after 500 cycles with nearly 100% coulomb efficiency. However, the specific capacity of V₂O₅ is maintained around 180 mAh g^− 1 at 4 A g^− 1, and it exhibits the capacity of 139 mAh g^− 1 (77.2%) at 4 A g^− 1 after 500 cycles. Hence, the enhancement of V₂O₅/C composite rate capacity and cycle stability is credited to the large specified surface area and the well better electrical conductivity because of the carbon addition. The oxygen defects concentration could enhance the electrochemical characteristics of the V₂O₅/C electrode.

In summary, it has been synthesized effectively V₂O₅/C sheets by a facile Solution combustion synthesis method as the cathode material for aqueous ZIBs. With the EIS, XPS, and CV techniques, V₂O₅/C with mixed vanadium valences has more electrochemical activity, lower polarization, quicker ion diffusion capacity, and greater electrical conductivity than V₂O₅. On the one hand, the source of carbon potentially improve electrical and ionic conductivity. On the other hand, the concentration of oxygen flaws might enhance the V2O5/C electrode's electrochemical characteristics. It can maintain a higher specific capacity of 188 mAh g^− 1 (85.5%) at 4 A g^− 1 after 500 cycles with nearly 100% coulomb efficiency than V₂O₅ of 139 mAh g^− 1 (77.2%). This approach is applicable to electrodes of ZIBs and has the potential to be used to additional energy storage applications due to its simplicity and scalability.

Acknowledgments

This work is financially supported by the Natural Science Foundation of Fujian Province (2022J011269) and Industry-Academe-Research Project of Xiamen (2022XCY0402) and Open Fund of Fujian Provincial Key Laboratory of Functional Materials and Applications (Grant No. fm2022005).

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Direct synthesis of vanadium pentoxide powder with carbon recombination as aqueous zinc-ion battery cathode

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