[Retracted] MoWS<sub>2</sub> Nanosheet Composite with MXene as Lithium-Sulfur Battery Cathode Material

Feng, Wangjun; Zhao, Zhiqiang; Lei, Ziru; Zhang, Li

doi:https://doi.org/10.1155/2023/6211780

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Abstract Introduction Materials and Methods Results and Discussion Conclusion Data Availability Conflicts of Interest Acknowledgments References Copyright Related Articles

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Volume 2023 | Article ID 6211780 | https://doi.org/10.1155/2023/6211780

[Retracted] MoWS₂ Nanosheet Composite with MXene as Lithium-Sulfur Battery Cathode Material

Wangjun Feng,¹Zhiqiang Zhao,¹Ziru Lei,¹and Li Zhang¹

Academic Editor: Haichang Zhang

Received30 Sept 2022

Revised08 Oct 2022

Accepted24 Nov 2022

Published25 Jan 2023

Abstract

Due to their superior theoretical specific capacity and energy density, lithium-sulfur (L‒S) batteries are gaining popularity in order to achieve the growing terms for more power generation. However, drawbacks such as low electrical conductivity of the active ingredient sulfur, severe volume expansion and shuttle effect of polysulfides, rapidly decaying battery capacity, and short battery life have hampered their development. A MoWS₂@MXene@CNT composite material is used as the main cathode material for L-S batteries in this study. MoWS₂ can improve the electrochemical reaction rate by accelerating polysulfide conversion, whereas MXene can suppress electrode volume expansion. Furthermore, the addition of carbon nanotubes (CNT) with high electrical conductivity improves the rate of the electrochemical reaction. Therefore, the MoWS₂@MXene@CNT composites have good capacity and versatility as cathode materials and enhance the behavior of L-S batteries.

1. Introduction

Owing to energy shortages and environmental degradation, the demand for sustainable high-performance electronic devices, such as smartphones and electric vehicles, is increasing [1, 2]. However, commonly used energy storage devices, for instance, lithium-ion batteries, are no longer able to fulfill the growing energy needs of consumers [3–5]. Moreover, lithium-ion batteries for daily use have several disadvantages, such as environmental hazards, high manufacturing costs, and insufficient theoretical capacity [6, 7]. Thus, the exploration of a new generation of energy storage devices is ongoing. In recent years, the development of lithium-sulfur (L-S) batteries has rapidly progressed, positioning them as interchangeable energy materials owing to their environmentally friendliness and inexpensive raw materials [8–10]. However, L-S batteries have disadvantages, such as low electrical conductivity of the active material, shuttle effect of the intermediate product polysulfide, and partial conversion of Li₂S_n (4 ≤ n ≤ 8) into the last discharge products, thereby limiting their commercialization [11–13].

To overcome these issues, researchers have designed composite materials that can rapidly convert polysulfides and retard the shuttle effect [14, 15]. For example, carbon nanotubes [16], porous carbon [17], and carbon cloths [18] can be used as physical frameworks to accelerate the reaction kinetics and thus mitigate the shuttle effects. Transition metal oxides [19], sulfides [20], and carbides [21] can be used to accelerate the conversion of polysulfides. However, the force between polar materials and polar polysulfides is important in inhibiting the shuttle effect [22–24].

Herein, we synthesized MoWS₂@MXene@CNT composites. We selected the molybdenum-based metal sulfide MoWS₂ as the cathode material in this study [25, 26] because the strong interactions between the polar material MoWS₂ and polar polysulfide can significantly suppress the shuttle effect. Because of their excellent electrical conductivity, carbon nanotubes (CNT) were chosen as the carbon material, which aids in accelerating the conversion of polysulfide [27]. Furthermore, the layered structure of the transition metal carbide MXene [28, 29] can limit volume expansion [30, 31] when singlet sulfur is used as the electrode.

2. Materials and Methods

2.1. Synthesis of MoWS₂

First, Na₂MoO₄·2H₂O and Na₂WO₄·2H₂O in a molar mass ratio of 4 : 1 were dissolved in approximately 40 mL of deionized water. To this mixture, CH₄N₂S and C₂H₂O₄·2H₂O in a molar mass ratio of 5 : 1 were subsequently added. As the precursor solution transformed into a clear liquid, it was transferred to a Teflon reactor at 200°C for 24 hours. The contents were then repeatedly cleaned with distilled water before being vacuum dried.

2.2. Synthesis of MoWS₂@CNT

MoWS₂@CNT was created using a hydrothermal method as follows: first, 60 ml of deionized water was mixed with MoWS₂ and CNT in a mass ratio of 1 : 1. Following ultrasonication, the mixture was transferred to a Teflon reactor and the hydrothermal reaction was allowed to run for 12 hours at 200°C. Finally, the contents were cleaned with distilled water before being vacuum dried.

2.3. Synthesis of MXene and MoWS₂@MXene@CNT

First, 20 mL of 40% HF was added to a 100 mL Teflon reactor, followed by 10 minutes of slowly adding 1 g of Ti₃AlC₂. The mixture then continuously reacted at a rate of approximately 500 rpm at 40°C for 8 hours to produce MXene. Following etching, the contents were repeatedly cleaned with distilled water and ethanol to remove impurities until a pH of greater than 6 was achieved and then vacuum dried.

The MoWS₂@MXene@CNT composites were similarly synthesized. Specifically, the added CNT was converted into the MXene@CNT complex. The complete procedure is shown in Figure 1.

2.4. Synthesis of MoWS₂@CNT/S and MoWS₂@MXene@CNT/S

Grinding for 10 minutes combined the sulfur powder with the MoWS₂@CNT and MoWS₂@MXene@CNT powders in a mass ratio of 7 : 3. For 20 hours, the reaction occurred continuously in a Teflon-lined reactor containing argon gas at a temperature of 155°C. Finally, the compound materials MoWS₂@CNT/S and MoWS₂@MXene@CNT/S were obtained.

2.5. Materials Characterization

X-ray diffraction (XRD, Bruker D8 Advance, Cu-K radiation) was utilized to ascertain the crystallinity of the samples in the 5°–90° test range. Scanning electron microscopy was applied to examine the dimensions and shape of the samples (SEM, JSM-6700F). The internal structure and element distribution of the material were evaluated utilizing transmission electron microscopy (TEM, JEM-2100F). Multifunctional X-ray photoelectron spectroscopy was used to determine the composition and chemical state of the elements in the materials (XPS, SCALAB250Xi). The sulfur content in the materials was proven using thermogravimetric analysis (TGA) (Perkin Elmer TG47).

2.6. Electrochemical Test

The preprepared electrode sheet was cut into 0.6 cm diameter disks with an average surface sulfur loading of 1.5 mg/cm². The average thickness of the cathode was 0.1 nm. The components were then gathered, along with the Celgard 2400 septum, unoxidized lithium sheet cathode, Celgard 2025 button cell cathode housing, and lithium-sulfur cell electrolysis. The rate and long cycle assays were conducted on an electrochemical workstation using just a cell test system (CT2001A) with a test voltage range of 1.7–2.8 V. The tests included cyclic voltammetry (CV) and electrochemical impedance spectroscopy (Corrtest 350). Electrochemical impedance spectroscopy (EIS) was tested with a frequency band of 0.01–100 kHz and a voltage amplitude of 5 mV.

3. Results and Discussion

The preparation flowchart of MoWS₂@MXene@CNT composite is depicted in Figure 1. In Figure 2(a), the main characteristic peaks of MXene and MXene@CNT are located at 8.7°, 18.3°, 27.4°, 35.2°, and 60.6°, which correspond to the (002), (004), (006), (008), and (110) crystal planes of MXene [32]. Those of MXene@CNT composites are approximately at 26°, which corresponds to the carbon nanotube’s (002) crystal plane. Furthermore, Figure 2(a) shows that the characteristic peaks of MXene are sharp, indicating that MXene has excellent crystallinity. The XRD patterns of MoWS₂, MoWS₂@CNT, and MoWS₂@MXene@CNT composites are shown in Figure 2(b). A diffraction peak at 14.1° can be seen in the figure. The shift of the peak at the (002) crystal plane indicates the result of increased layer spacing when compared to the peaks of MoS₂ and WS₂in the literature (JCPDS card numbers: 75-1539 and 08-0237) [25].

(a)

(b)

(c)

Both the MoWS₂@CNT and MoWS₂@MXene@CNT composites show a minimal change because their overall crystallinity was inferior to that of the original MoWS₂ crystals; moreover, the characteristic peaks of MoWS₂ and the standard characteristic peaks of CNT dominate these two samples, which could better accelerate the reaction kinetics. MoWS₂ composites show obvious sharp (002) diffraction peaks, indicating that the hydrothermally prepared samples possess a high level of crystallinity. Meanwhile, for the composites, the evident diffraction peaks similarly indicate a higher crystallinity for materials prepared by the hydrothermal method, with standard cards at 14.38° and 14.32°, corresponding to the (002) crystal plane of MoS₂ and WS₂, respectively. By comparison, the diffraction peaks of the synthetic MoWS₂ (002) are smaller than the fixed peaks, indicating the presence of strain, stress, and a large layer spacing between layers in the structure [26]. In Figure 2(b), the characteristic peak of MXene is significantly lower, indicating that MoWS₂ is successfully modified on the Ti₃C₂T_x surface; furthermore, the peak of (002) shifts to the left, indicating increased layer spacing.

TGA was performed on the composites, and the TGA curves of the MoWS₂@CNT/S and MoWS₂ @MXene@CNT/S composites are presented in Figure 2(c). Meanwhile, the MoWS₂@CNT/S and MoWS₂ @MXene@CNT/S materials experience rapid mass loss in the 150–300°C range; this mass loss is primarily attributed to sulfur sublimation in the composite. The presence of sulfur is confirmed by the presence of a sublimed sulfur diffraction pattern in the material. The mass loss in MoWS₂@CNT/S and MoWS₂@MXene@CNT/S is 72.63 and 68.73 wt.% sulfur mass fractions, respectively, as shown in Figure 2(c).

After etching of the MAX phase precursor Ti₃AlC₂, the multilayer Ti₃C₂T_x obtained is shown in Figures 3(a)–3(c). The figures show a sparse accordion structure. In Figure 3(d), for the prepared MXene@CNT composites, long strips of CNT are densely compounded on MXene.

(a)

(b)

(c)

(d)

(e)

(f)

(g)

(h)

(i)

In the SEM images of MoWS₂ and MoWS₂@CNT shown in Figures 3(e), 3(g), and 3(h), the hydrothermally synthesized MoWS₂ has a three-dimensional nano-microflower structure and is intertwined in long strips of carbon nanotubes that can provide a good channel for ion transport [25].

For the MoWS₂@MXene@CNT composites (Figure 3(i)), the hinged CNT and the nano-microflower MoWS₂ are evidently interwoven and born together, and the CNT is densely grown on the surface of MXene. This forms an overall structure with a large and stable specific surface area, which indicates that MoWS₂@MXene@CNT was successfully prepared. These morphological and surface analyses confirm that MoWS₂@MXene@CNT composites can promote rapid insertion/deinsertion of ions between flowers.

The structure and morphology of the MoWS₂@MXene@CNT material were studied using TEM. Many long strips of carbon nanotubes are interwoven with black MoWS₂ particles to form a hinge structure (Figure 4(a)) that grow over the MXene to form the MoWS₂@MXene@CNT composite material (Figure 4(b)). The (002) lattice plane of CNT is distinctly visible in Figure 4(c).

(a)

(b)

(c)

Figures 5(a) and 5(b) similarly exhibit that the lamellar MXene is interspersed with hinge-like carbon nanotubes and black MoWS₂ nanoparticles. Figure 5(c) shows an evident lattice diffraction ring, indicating the good crystallinity of MoWS₂@MXene@CNT, which correlates directly to the spacing observed in the XRD plots, and HRTEM analysis confirms the XRD results. All of these results show that MoWS₂@MXene@CNT composites can be successfully prepared and have improved electrochemical activity due to their unique structure [25]. The elemental mapping images in Figure 5(d) obtained through the EDX spectroscopy confirm that Ti, C, Mo, S, and W have indeed been successfully coated onto MoWS₂@MXene@CNT.

The sample was analyzed by XPS, and the results are shown in Figure 6. The presence of Ti, C, S, Mo, and W in the composites is confirmed by the XPS data.

(a)

(b)

(c)

(d)

(e)

(f)

Figure 6 depicts the composite’s entire XPS profile. Figure 6(a) depicts the survey of the underside. The full spectrum shows the peaks of each element, proving that the MoWS₂@MXene@CNT composites were synthesized. Figures 6(b)–6(f) show the XPS spectra of Ti, C, Mo, S, and W.

In Figure 6(b), the three major diffraction peaks of Ti 2p are observed at 459.6, 465.3, and 469.6 eV, which correspond to the Ti-C (Ti 2p_3/2), Ti-X (Ti 2p_3/2), and TiO₂ (Ti 2p_3/2) bonds, respectively [33].

The C 1s spectrum is depicted in Figure 6(c), with three peaks at 284.8, 285.7, and 290.5 eV, corresponding to the C-C/C=C, C-O, and C=O bonds, respectively [34].

In Figure 6(d), two peaks near 162.5 and 163.7 eV, corresponding to S 2p_3/2 and S 2p_1/2, respectively, demonstrate the presence of sulfur in the MoWS₂@MXene@CNT composites [35].

The Mo 3d spectrum is depicted in Figure 6(e). The Mo 3d peak was deconvoluted into two additional peaks at 229.8 and 232.8 eV, corresponding to Mo 3d_5/2 and Mo 3d_3/2, respectively, as well as a S 2s peak at 226.7 eV. The Mo 3d peak points to the Mo⁴⁺ [25].

The high-resolution W 4f XPS profile of the MoWS₂@MXene@CNT samples is displayed in Figure 6(f). The existence of W⁴⁺ is strongly recommended by the two peaks of W 4f_7/2 and W 4f_5/2 at 37.1 and 39.0 eV, respectively [25, 36].

The composite was used as the cathode for CR2025 button cell assemblies to evaluate MoWS₂@MXene@CNT/S and its electrochemical performance as a cathode material for L-S batteries. The charge/discharge curves, rate performance, and CV diagrams of the MoWS₂@MXene@CNT/S and MoWS₂@CNT/S composite materials are presented in Figure 7. Figure 7(a) depicts the charge/discharge curve of the MoWS₂@MXene@CNT/S. Meanwhile, the discharge profile exhibits a L-S double discharge platform. At approximately 2.3 V, the first plateau is observed, which corresponds to a transition from the elemental sulfur state to the soluble high-valent polysulfides. And the other one is observed at about 2.1 V, corresponding to the transition from Li₂S_n (4 ≤ n ≤ 8) to Li₂S₂ and Li₂S. Figure 7(b) depicts the composites’ rapid loss of discharge capacity as the charging and discharging rates of MoWS₂@CNT/S increase. The large capacity loss could be thought to be due to the polysulfide, which ultimately resulted in the continuous loss of active material sulfur as well as the rapid decay of discharge capacity. The discharge capacity of the MoWS₂@MXene@CNT/S electrode material is 1319.4 mAh/g, which is clearly superior to that of the MoWS₂@CNT/S, which is 996.0 mAh/g. Figure 7(c) shows a rate performance graph of MoWS₂@CNT/S and MoWS₂@MXene@CNT/S with a discharge rate increasing from 0.1 C to 2 C. The rate performance of MoWS₂@MXene@CNT/S electrode is superior to that of MoWS₂@CNT/S electrode material. The CV curves were determined to better understand the electrochemical properties of MoWS₂@MXene@CNT/S. A split oxidation peak and two reduction peaks are obtained in Figure 7(d). The low and high potential peaks in the reduction peaks are approximately 2.1 and 2.3 V, respectively, corresponding to the insoluble Li₂S₂ and Li₂S and the conversion of the S₈ to high-order polysulfides (Li₂S_n, 4 ≤ n ≤ 8). Because of the occurrence of the reverse reaction from Li₂S to Li₂S_n to S₈ [36], the split oxidation peak is observed at about 2.4 V. Meanwhile, two reduction peaks of MoWS₂@MXene@CNT/S have such a greater area than MoWS₂@CNT/S, indicating that the addition of MXene can improve polysulfide redox kinetics [37, 38].

(a)

(b)

(c)

(d)

The cathode materials MoWS₂@MXene@CNT/S and MoWS₂@CNT/S have different capacities after 200 cycles at 0.2 C in Figure 8. The MoWS₂@MXene@CNT/S cathode material outperforms the MoWS₂@CNT/S cathode material in terms of discharge capacity and cycling performance. As a result of electrode material activation, the final capacity of the MoWS₂@MXene@CNT/S cathode material slightly increases, which can provide additional lithium interfacial storage at low potentials via a mechanism known as pseudocapacitance [39, 40].

To further evaluate the good electrochemical properties of the MoWS₂@MXene@CNT/S composites, the EIS of both electrode materials was investigated separately. In Figure 9, the EIS of both materials have a comparison after and before cycling. A semicircle and a diagonal line comprise the impedance diagram [41, 42]. The semicircle denotes the impedance of charge transfer between the electrode material and the electrolyte, and the diagonal line reflects the diffusion of lithium I in the electrode material [43]. MoWS₂@MXene@CNT has the smallest half-circle diameter and total electrochemical resistance before and after the multiplier cycle of the composites, indicating that it has the lowest charge transfer impedance. Table 1 displays the specific fitted values prior to the multiplicative cycle.

(a)

(b)

4. Conclusion

In this article, MoWS₂, MXene, MoWS₂@CNT, and MoWS₂@MXene@CNT complexes were prepared by hydrothermal and etching methods. Additionally, the electrode materials after sulfur loading were prepared. These materials were characterized using XRD, TGA, SEM, TEM, and XPS and evaluated for their electrochemical performance. In the MoWS₂@MXene@CNT composite, all three substances are simultaneously present in the electrode material. Furthermore, the polar substance MoWS₂ can accelerate the conversion of polysulfide, and the highly conductive CNT can accelerate the electron transfer rate. Meanwhile, MXene suppresses the volume expansion of the cell during discharge and enhances the electron conductivity. The final electrochemical tests showed that the MoWS₂@MXene@CNT/S electrode material exhibited a good rate and cycling stability compared to the MoWS₂@CNT/S electrode material, which provides a reference for transition metal sulfide and transition metal carbide composites as lithium-sulfur battery cathode materials.

Data Availability

The raw/processed data required to reproduce these findings cannot be shared at this time as the data also form part of an ongoing study.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

This work was supported by the National Natural Science Foundation of China (no. 21965019) and HongLiu First-class Disciplines Development Program of Lanzhou University of Technology.

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Copyright © 2023 Wangjun Feng et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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Advances in Materials Science and Engineering

Advanced Composite Materials and Their Applications

[Retracted] MoWS2 Nanosheet Composite with MXene as Lithium-Sulfur Battery Cathode Material

Abstract

1. Introduction

2. Materials and Methods

2.1. Synthesis of MoWS2

2.2. Synthesis of MoWS2@CNT

2.3. Synthesis of MXene and MoWS2@MXene@CNT

2.4. Synthesis of MoWS2@CNT/S and MoWS2@MXene@CNT/S

2.5. Materials Characterization

2.6. Electrochemical Test

3. Results and Discussion

4. Conclusion

Data Availability

Conflicts of Interest

Acknowledgments

References

Copyright

[Retracted] MoWS₂ Nanosheet Composite with MXene as Lithium-Sulfur Battery Cathode Material

2.1. Synthesis of MoWS₂

2.2. Synthesis of MoWS₂@CNT

2.3. Synthesis of MXene and MoWS₂@MXene@CNT

2.4. Synthesis of MoWS₂@CNT/S and MoWS₂@MXene@CNT/S