Sustainable and Scalable Approach for Enhancing the Electrochemical Performance of Molybdenum Disulfide (MoS<sub>2</sub>)

Kumar, Sunil; Kumar, Vinay; Devi, Raman; Sisodia, Avnish Kumar; Jatrana, Anushree; Singh, Raj Bahadur; Dahiya, Rita; Mishra, Ajay Kumar

doi:https://doi.org/10.1155/2022/1288623

Advances in Materials Science and Engineering

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

Research Article | Open Access

Volume 2022 | Article ID 1288623 | https://doi.org/10.1155/2022/1288623

Sustainable and Scalable Approach for Enhancing the Electrochemical Performance of Molybdenum Disulfide (MoS₂)

Sunil Kumar,¹Vinay Kumar,¹Raman Devi,¹Avnish Kumar Sisodia,²Anushree Jatrana,³Raj Bahadur Singh,⁴Rita Dahiya,¹and Ajay Kumar Mishra^5,6

Academic Editor: Antonio Riveiro

Received07 Oct 2022

Revised16 Dec 2022

Accepted17 Dec 2022

Published31 Dec 2022

Abstract

Molybdenum disulfide (MoS₂), the second most thoroughly investigated two-dimensional material after graphene, has attracted considerable interest in energy storage applications owing to its exceptional qualities, including its unique crystal structure, low electronegativity, and high specific capacity. In this study, we showed that a simple ball-milling procedure causes significant improvement in the capacitive properties of the bulk MoS₂ (BL-MoS₂). We characterized the material before and after the milling process using X-ray diffraction (XRD) and a BET surface area analyzer to find the material’s structural, crystalline features, and surface area, respectively. We prepared electrodes of BL-MoS₂ and ball-milled MoS₂ (BM-MoS₂) for electrochemical investigation. The charge storage characteristics were examined using cyclic voltammetry (CV), galvanostatic charge-discharge (GCD), and electrochemical impedance spectroscopy (EIS). The BM-MoS₂ and BL-MoS₂ have a specific capacitance of 114 F/g and 96 F/g, respectively.

1. Introduction

The world has recently turned its focus to the energy crisis, which has emerged as one of the biggest issues. This problem arises because of our overdependence on automatic and advanced technological devices. They ease our routine life, but they also consume electric power. The demand for energy increases very fast, but on the other hand, the energy harvesting and storage mechanism is not growing. To meet the global market for “energy,” the scientific community has to find new solutions and search for new methods and materials that possess prodigious performances in the energy harvesting, conversion, and storage sector [1].

Supercapacitors can fulfill the gap of hardship that we are facing and help us get rid of these challenges. The ability of supercapacitors to carry significantly greater energy-power efficiency, specific power density, faster charge-discharge rate, and a longer lifespan compared to rechargeable batteries make them a favorite for next-generation energy storage devices [2, 3]. Supercapacitors are having 1000 times more power density than that of batteries [4]. Despite extensive research and significant achievements in recent years, energy storage devices continuously face numerous challenges, including high energy density, fast charging, slow discharging, and long life, as well as their sustainable production using readily available and abundant materials.

To solve these restrictions, there is a significant demand for developing new concepts and materials with outstanding performance while being scalable, low-cost, and ecologically benign. Two-dimensional (2D) materials, especially layer-structuredtransition-metal dichalcogenides (TMDs), have gained much attention in the supercapacitor sector due to their unique physiochemical features such as large surface area, micro or mesoporous structure, and strong conductivity. Among them, molybdenum disulfide (MoS₂) has been identified as one of the most appealing materials and has recently been investigated in electrochemical energy storage applications. The structure of MoS₂ is similar to that of graphite, which has a layer-like structure made up of three atom layers with a Mo layer sandwiched between two S layers, all of which are held together by weak van der Waals forces [5]. The recent development in supercapacitor research has also focused on MoS₂ mainly because of its higher intrinsic ionic conductivity compared to oxides and high theoretical capacity than graphite [6]. For example, the study on MoS₂, used as an electrode material for supercapacitors due to its large surface area and sheet-like morphology, results in double-layer charge storage (EDLC) in the supercapacitor by Soon and Loh [7].

Along with the EDLC, the faradic capacitance also contributes to capacitance increment due to the diffusion of the ions into the MoS₂ layers and causes a significant role in enhancing charge storage capabilities. Therefore, a lot of work focused on synthesizing nanosized MoS₂ structures, and various methods are used for this purpose. All these methods make the material much more useful by altering its properties like surface area and conductivity and increasing the edge sites, which causes enhancement in the active sites. Every method has advantages and disadvantages, but scalability, environmental hazard, and accessible material production are the challenges. In order to address all these problems, the ball-milling process provides an excellent way to synthesize the desired material with large surface area and also resolves the issue of scalability [8]. In this study, we present a straightforward and scalable approach based on dry ball milling that improves the electrochemical characteristics of BL-MoS₂ without using any chemical agents or reactions. We observed that the BM-MoS₂ had high specific capacitance; hence, enhanced electrochemical features can be utilized for electrochemical supercapacitor applications. This work aims to study the effect of ball milling on the charge storage mechanism of BL-MoS₂.

2. Material and Methods

2.1. Chemicals

Molybdenum disulfide and potassium chloride were purchased from Sigma-Aldrich, and these chemicals were not further refined before being utilized.

2.2. Procedure of Ball-Milling of Bulk MoS₂

Using a “Fritsch Pulveristee 5 planetary” ball milling machine, the BL-MoS₂ was subjected to a 12-hour ball milling procedure. We employed 30 g of BL-MoS₂ powder and 300 g of stainless steel balls into a ball milling jar. The ball milling process was carried out at 300 rpm for 12 hours.

2.3. Characterization Techniques

The crystal structure of BL-MoS₂ and BM-MoS₂ was recorded by X-ray diffraction (XRD) on “Rigaku Mini Flex II X-ray Diffractometer” and surface area analysis was done using “Quantachrome Instruments v5.21” of Anton Paar. A Perkin-Elmer FTIR spectrometer was used to record the FTIR spectra in the range of 4000 cm⁻¹ to 400 cm⁻¹ to examine the different functional groups in the sample. The morphology of the samples was evaluated with the help of a field emission scanning electron microscope (FESEM) of JEOL iT-800, and an electrochemical workstation (Metrohm Autolab PGSTAT-204M) was used to accomplish the electrochemical investigation.

2.4. Preparation of an Electrode for Electrochemical Investigation

By mixing BM-MoS₂ and carbon black using a mortar and pestle, the working electrode was prepared to explore the electrochemical behavior of the processed material. This mixture was used to form a slurry. To make a slurry, we dissolve 3 mg of polyvinylidene fluoride (PVDF) in 2 ml in an organic solvent “N-methyl-2- pyrrolidine” using a magnetic stirrer. The stirring process continued until a transparent solution was formed, and then, the mixture of BM-MoS₂ (24 mg) and carbon black (3 mg) was added to this solution and stirred for 12 hours. Through this process, we obtained a thick slurry paste spread on the area of one centimeter square of the current collector (graphite sheet) with a mass loading of 1.39 mg of the active material and dried it in a vacuum oven for 12 hours at 80°. The ingredient’s mass ratio was 8 : 1:1 in the slurry. The same method was adopted to prepare the BL-MoS₂ working electrode. KCl (1 M) was used as an electrolyte to test the fabricated electrode at room temperature using a conventional three electrodes setup. The BL-MoS₂ and BM-MoS₂, Ag/AgCl electrodes, and spiral platinum wire were used as working, reference, and counter electrodes, respectively. At different scan rates of 10 mV/s to 200 mV/s, the CV recorded in the voltage window of −0.7 V to 0.7 V. GCD profiles were carried out at different current densities 1, 1.5, 2, 2.5, and 3 A/g. Further, the EIS analysis was carried out in the frequency range of 10 MHz to 100 kHz. Using equation (1), the specific capacitance was calculated from the GCD curve. The detailed discussion about how the specific capacitance was calculated is given in Table 1 of supplementary file.where C_p, I, t, m, and ΔV represent their usual meanings, i.e., the specific capacitance (F/g), discharge current (A), time duration of discharging (s), mass deposited on the electrode (g), and potential window (V), respectively.

3. Results and Discussion

3.1. XRD Analysis

Figure 1(a) shows the XRD spectra of both BL-MoS₂ and BM-MoS₂. The XRD spectra were observed from 10° to 80°. The diffraction peak observed at 14.2°, 32.6°, 39.5°, 44.2°, 49.8°, and 58.3°, relating to the (002), (100), (103), (006), (105), and (110) planes [9], respectively, is as shown in Figure 1(a). From this, we confirm that BL-MoS₂ and BM-MoS₂ both have crystalline natures. The BL-MoS₂ has a very sharp and highly intense peak at 14.38°, which belongs to the 2H structure of MoS₂. After ball milling (12 h), the processed material is BM- MoS₂ that has the same sharp peak but with reduced intensity, which shows the sign of layered MoS₂ [10] formation. It is important to note that the presence of the same peak after exfoliation can be connected to a certain level of layer restacking during the ball-milling process. The average crystallite size (D) of the BL-MoS₂ and BM-MoS₂ were calculated using the Scherer formula in equation (2). The average crystallite size of BL-MoS₂ and BM MoS₂ was 36 nm and 30 nm, respectively.where λ is the wavelength of Cu-K_α radiation, k (0.9) is the structure factor, β is the FWHM, and θ is the diffraction angle.

(a)

(b)

(c)

(d)

3.2. BET Analysis

The surface area was determined using the Brunauer–Emmet–Teller (BET) method for N₂adsorption-desorption isotherms. Figure 1(b) displays the N₂adsorption-desorption isotherms plots for BL-MoS₂ and BM-MoS₂. As already discussed, BL-MoS₂ exfoliated into numerous layers, size of the particles, and thickness decreases, which affects the surface area of the MoS₂ [11, 12]. The higher surface area has a more active site, which can also increase the interaction of electrode and electrolyte; as a result, we have higher electrochemical performance [8]. Both samples exhibit type IV isotherms, and the N₂adsorption-desorption isotherms illustrate that the volume of gas trapped was higher in the case of BM-MoS₂ than the BL-MoS₂. Therefore, because the MoS₂ layer is restacked by ball milling, BM-MoS₂ has a higher specific surface area (22.593 m²/g) than BL-MoS₂ (11.239 m²/g). Figure 1(c) represents both samples’ pore size distribution. BM-MoS₂ has a total pore volume of 0.544 cc/g determined by the density function theory (DFT) method for a radius smaller than 173.3 nm, and BL-MoS₂ has a total pore volume of 0.482 cc/g for a radius less than 183 nm calculated at a relative pressure of 0.9944.

3.3. FTIR Analysis

The FTIR spectra of BL-MoS₂ and BM-MoS₂ obtained in the IR region between 400 cm⁻¹ and 4000 cm⁻¹ are shown in Figure 1(d). The spectra of MoS₂ include an absorption peak at 596 cm⁻¹, which corresponds to the presence of the Mo-S bond, and an additional peak at 903 cm^−1, caused by the S-S bonds in MoS₂. The absorption bands at 1125 cm⁻¹ and 1634 cm⁻¹ are attributable to the stretching vibrations of the Mo-O bond and the hydroxyl group [13], respectively. The prominent peaks at about 3421 cm⁻¹ are caused by the stretching vibration of OH groups present due to moisture in the sample, while narrow peaks at 2917 cm⁻¹ are related to CH₂ [14].

3.4. FESEM Analysis

FESEM is used to characterize the morphologies and nanostructures shown in Figures 2(a)–2(d) at various scales. The crumpled BL-MoS2 indicates the creation of a few-layer MoS₂ nanosheet with a flower-like structure. The ball milling method results in the exfoliation of the BL-MoS₂ Figure 2(a) into nanosheets. The difference can also be seen in the FESEM pictures, as shown in Figures 2(b)–2(d). The BL-MoS_2, after the ball milling process, exhibits a flower-like nanosheet shape with an average thickness of 40 nm of nanosheets in the FESEM images. The energy dispersive X-ray (EDX) analysis shown in Figures 2(e) and 2(f) was performed to check the purity of both samples and to find out if any alterations were caused during the ball milling process. The EDX spectra of BL-MoS₂ are shown in Figure 2(e), and it confirms the purity of bulk material as it can be seen by the as-expected characterized peaks of Mo and S as major elements. We also get small content of carbon and oxygen. After the milling process, the purity of the sample (BM-MoS₂) remains intact, as shown in Figure 2(f), in which no additional signal was observed.

(a)

(b)

(c)

(d)

(e)

(f)

3.5. Electrochemical Analysis

The capacitive behavior of the material was initially tested using CV. Figure 3(a) depicts the bare graphite sheet CV curves, BL-MoS₂ and BM-MoS₂. BM-MoS₂ has a higher current response, resulting in a larger area of the voltammogram than pristine BL-MoS₂ and bare graphite sheet, indicating that it has a higher specific capacitance. The performance of CV for BL-MoS₂- and BM-MoS₂-coated graphite sheets at scan speeds ranging from 10 to 200 mV/s is depicted in Figures 3(b) and 3(c), respectively. Meanwhile, the integral area of all CV curves grows with increasing scan speeds in both cases without distortion in the CV curve. Moreover, this indicates the sample’s strong rate capabilities and capacitance nature. It is also evident that a minor departure from the perfect EDLC profiles in CV curves shows pseudocapacitance behavior [15], which might be caused by ion (K⁺) intercalation and deintercalation inside the layers of MoS₂ and electrolyte ion (K⁺) adsorption on the surface [9]. The ionic conductivity of electrolytes also plays an essential role in energy storage [16] and KCl matches this condition. Also, KCl has neutral nature and benefits such as reduced corrosion, lower costs, and environmental friendliness.

(a)

(b)

(c)

(d)

(e)

(f)

(g)

(h)

Because BM-MoS₂ has a higher surface area than BL-MoS₂, the specific capacitance rises [17]. The ball milling procedure to the bulk MoS₂ results in a large surface area, allowing ions to occupy more space and enriching the specific capacitance of the BL-MoS₂. The GCD investigation was performed to evaluate the prepared electrode’s capacity for charge storage. Both BL-MoS₂ and BM-MoS₂ have asymmetric GCD curves with a slightly irregular triangle shape, exposing the material’s pseudocapacitive nature and electric double-layer capacitance. Also, Dunn’s method was used for exploring the capacitive contribution and surface kinetics of the material (Figure 1(a) of supplementary file). We observed that the Faradaic process contributed as the main mechanism for charge storage in BL-MoS₂ electrode (Figure 1(b) of supplementary file). If the capacitance involved only ideal EDLC, the charging-discharging curve has a perfect triangular shape. The GCD curve of BL-MoS₂ and BM-MoS₂ at different current densities are shown in Figures 3(d) and 3(e). The BL-MoS₂ and BM-MoS₂ exhibit a specific capacitance of 96 F/g and 114 F/g, respectively, at a current density of 1 A/g. This study exposed that the BM-MoS₂ electrode would have greater capacitance than BL-MoS₂ because the increase in interaction area with the electrolyte ions due to large surface area [16] provides more ion diffusion channels than BL-MoS₂. The prepared electrode was subjected to EIS for further analysis. EIS includes valuable information about the material’s capacitive behavior, ion transportation kinetics, and various internal resistances of the electrode [18]. The EIS analysis was carried out in the frequency range of 10 MHz to 100 kHz, as shown in Figure 3(f), along with the circuit fit diagram. Both BL-MoS₂ and BM-MoS₂ have a small circular arc in the high-frequency region and a vertically aligned line with a high slope in the lower-frequency region. Using electrochemical circuit fit, we have found the material’s resistance of charge transfers (R_ct) from the radius of the semicircle in the high-frequency region [9]. The charge transfer resistance was 4.5 Ω and 5.3 Ω for BM-MoS₂ and BL-MoS_2, respectively. The lower R_ct indicates the enhanced diffusivity of electrolyte ions on the surface [19] of the processed material, which happens because of the large surface area and increased active sites of the BM-MoS₂. The BM-MoS₂ shows excellent cyclability and reversibility even after 5000 cycles as shown in Figure 3(g). The capacitance retention of the prepared electrode of BM-MoS₂ was also tested at a high current density of 10 A/g for 5000 cycles, shown in Figure 3(h), and it was found that after the 5000 cycles, the retention of capacitance was 91.7%, and this shows the high efficiency of the BM-MOS₂ electrode.

4. Conclusion

We have two MoS₂ samples, one being bulk MoS₂ (BL-MoS₂), while the other has undergone ball milling processing (BM-MoS₂). Both samples were characterized using XRD, which helps to determine the material’s crystallinity. From BET plots, the active surface area of BL-MoS₂ and BM-MoS₂ was determined to be 11.239 m²/g and 22.593 m²/g, with a total pore volume of 0.544 cc/g and 0.482 cc/g, respectively. BM-MoS₂ results in a slightly higher specific surface area. At a current density of 1 A/g, the constructed electrode using BM-MoS₂ has a specific capacitance of 114 F/g, while BL-MoS₂ has 96 F/g. MoS₂ treated by ball milling has a higher active surface area for electrolyte ion intercalation, which is beneficial for increasing specific capacitance with 91.7% capacitance retention after 5000 cycles. As a result, the suggested approach would open the way for developing high-efficiency supercapacitors using a cost-effective, environment-friendly, scalable, and sustainable approach containing MoS₂ as an active material imposed with a ball milling.

Data Availability

The data used to support the findings of this study are included within the article.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Supplementary Materials

This section contained a detailed analysis of the calculation of specific capacitance (table 1 of supplementary file) and Dunn’s method used to find the nature of the dominant type of capacitance for the BL-MoS₂ electrode and the reaction kinetics take place at the surface of the electrode. The type of capacitive contribution and kinetics of the BL-MoS₂ electrode is studied using Dunn’s equation. The CV curves are then recorded at different scan rates, as depicted in Fig. 1(a) of the supplementary file. Using power law, the experimental current I is plotted against the scan rate (ν) to obtain the slope of the log (I) versus log (ν) plot of the BL-MoS₂ electrode (Fig. 1 (b) of the supplementary file). (Supplementary Materials)

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Copyright © 2022 Sunil Kumar 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

Sustainable and Scalable Approach for Enhancing the Electrochemical Performance of Molybdenum Disulfide (MoS2)

Abstract

1. Introduction

2. Material and Methods

2.1. Chemicals

2.2. Procedure of Ball-Milling of Bulk MoS2

2.3. Characterization Techniques

2.4. Preparation of an Electrode for Electrochemical Investigation

3. Results and Discussion

3.1. XRD Analysis

3.2. BET Analysis

3.3. FTIR Analysis

3.4. FESEM Analysis

3.5. Electrochemical Analysis

4. Conclusion

Data Availability

Conflicts of Interest

Supplementary Materials

References

Copyright

Sustainable and Scalable Approach for Enhancing the Electrochemical Performance of Molybdenum Disulfide (MoS₂)

2.2. Procedure of Ball-Milling of Bulk MoS₂