Synthesis of 2-Dimensional Novel Ti3C2Tx/NaF nano-composites and Fabrication of Electrode for Electrochemical performance of Pseudo-capacitive Supercapacitor Device

doi:10.21203/rs.3.rs-3317415/v1

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Synthesis of 2-Dimensional Novel Ti₃C₂T_x/NaF nano-composites and Fabrication of Electrode for Electrochemical performance of Pseudo-capacitive Supercapacitor Device

https://doi.org/10.21203/rs.3.rs-3317415/v1

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published 18 Jan, 2024

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The increasing global demand for energy storage solutions has spurred interest in advanced materials for electrochemical energy storage devices. Transition-metal carbides and nitrides known as MXenes, characterized by remarkable conductivity and tunable properties, have gained attention for their potential in energy storage applications. The properties of two-dimensional (2-D) MXenes can be tuned by doping or composite formation for energy storage applications. We report a novel Ti₃C₂T_x/NaF composite via a straightforward hydrothermal process for supercapacitor electrode applications. Three different composites with varying NaF concentrations (1%, 3%, and 5%) were synthesized under uniform conditions. Structural characterization using X-ray diffraction (XRD) and scanning electron microscopy (SEM) confirmed the successful formation of the composites, whereas, distinct shifts in XRD peaks and new peaks revealed the presence of NaF. Electrochemical performance was evaluated by cyclic voltammetry (CV), galvanostatic charging-discharging (GCD), and electrochemical impedance spectroscopy (EIS). The composites exhibited pseudo-capacitive behavior with reversible redox reactions during charge and discharge cycles. Specific capacitance of 191 F/g at scan rates of 2 mV/s was measured in 1M KOH. Electrochemical impedance spectroscopy (EIS) revealed an escalating impedance factor as NaF content increases within Ti₃C₂T_x. This study underscores the versatile energy storage potential of Ti₃C₂T_x/NaF composites, offering insights into their tailored properties and behavior.

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The raising energy demands and depleting fossil fuel resources have attracted researchers for more creative and durable energy solutions ¹ . Energy storage devices (ESD) are of crucial importance for various energy storage technologies such as wind and solar. ESDs store energy in various forms, including electrochemical, kinetic, pressure, potential, electromagnetic, chemical, and thermal. Electrochemical energy storage is one of the leading energy storage mediums and it include various devices such as batteries, fuel cells, standard capacitors and, supercapacitors etc.² . Factors, such as energy density, power density, storage capacity, charge-discharge time/charging cycles, heat sensitivity, and maintenance/operating cost are important criterion used to select an ESD. Recently, supercapacitors have gained significant attention due to their higher power densities than batteries and higher energy densities than ordinary capacitors. SC can be categorized in two types: 1) electrical double-layer capacitors (EDLC), store charge electrostatically and no charge transfer occurs between the electrode and the electrolyte. Ions diffuse through the electrolyte to the electrodes because of the potential difference. 2) pseudocapacitors, the charge transport between the electrode and the electrolyte allows for electrochemical energy storage because of the redox reactions between the electrode and the electrolyte. In contrast to ELDCs, they have a larger specific capacitance and energy density because of reversible Faradic reactions at the electrode surface followed by charge transfer ³, however their self-discharging process is their main limitation ⁴.

Transition-metal carbides and nitrides (MXenes), are used as electrochemical energy storage materials because of their outstanding electrical conductivity, hydrophilic surface, excellent flexibility and tunable properties ⁵^,⁶. MXene are etched from their precursor M_n + 1AX_n phases ( where M is an early transition metal; A represent group A element and X is C and N) by selective etching of A phase which is mostly Al or Si. MAX powder mostly exhibit metallic or ceramic properties ⁷. After selective etching of MAX powder, high quality MXene is obtained from supernatant post centrifugation and washing ⁸. In the Ti₃C₂T_x, T_x denotes surface terminated species, such as O, OH, and F groups ⁹ . MXenes have this advantage over other two dimensional materials that it can easily tune its properties and form composites with other materials owing to these surface terminations ¹⁰^,¹¹. Mostly MXenes exhibit metallic behaviour but some MXenes gives semiconducting behaviour too ¹². Previously, various elements have been tested with Ti₃C₂T_x, either in the form of doping or composite. Wen et. al. group had reported nitrogen ¹³ and Sulphur ¹⁴ doped Ti₃C₂T_x and clay inspired MXenes, previously¹⁵. Introduction of a foreign atom into MXene layers, can replace M or X atom to form stable bonds ¹⁶^,¹⁷. It is worthy to note that MXenes can easily form composites with other materials such as polymers, oxides, and carbon nanotubes, which further provides an effective way to tune the properties of the material for various applications such as energy storage ¹⁸^,¹⁹. For example, Sulfur decorated Ti₃C₂T_x showed specific capacity of 135 mA/g at 2 A/g current density making it well suitable for sodium ion batteries ²⁰. CuS decorated MXene exhibited a specific capacity of 169.5 C/g at current density of 1 A/g ²¹. Under the current density of 0.1 A/g, specific capacity of 65 mAh/g was achieved for MnO₂-MXene composite ²². More importantly, three dimensional composite of MXene with porous carbon has proved to be an excellent host for sulfur in lithium sulfur batteries ²³. On the other hand, Sn⁴⁺decorated MXene exhibited promising properties as an anode with a high reversible specific capacitance of 635 mAh/g at 0.1 A/g current density ²⁴. Zheng, Z. et al prepared Au nanoparticles decorated MXene nanosheets with a specific capacitance of 278 F/g at 5 mV/s and 95% of cyclic stability after 10,000 cycles ²⁵. It was noted that polypyrrole particles acts as spacer preventing the restacking of MXene nanosheets, while contributing to higher capacitance of the hybrid material ²⁶. The phosphorus doped Ti₃C₂T_x with P-O and P-C bonds support rapid ion transfer into electrode thus provide a capacitance of 476.9 F/g ²⁷. Flexible nitrogen-doped carbon nanotube (N-CNT)/Ti₃C₂T_x (MXene)/polyacrylonitrile (PAN) nanocomposite films showed a high specific capacitance of 446.18 F/g at 5 mV/s ²⁸. Three-dimensional (3D) hybrid porous aerogel composed of sulfur and nitrogen doped reduced graphene oxide and MXene (S,N-rGO@MXene) resulted in a specific capacitances of 85.4 F/g and 88.9 F/g, respectively ²⁹. Carbon-coated Fe₃O₄ nanoparticles were deposited on MXene nanosheets and the nanocomposite exhibited a specific capacity of 231.5 mAh/g even after 200 cycles ³⁰. MnO₂-MXene-CNT fibers demonstrated a capacitance of 371.1 F/cm³ in three-electrode system ³¹.

In this work, we investigate the influence of Ti₃C₂T_x/NaF composite on specific capacitance using the essential electrolyte KOH. First, Si was etched from Ti₃SiC₂ MAX powder ³², which was further delaminated to create spacing between the layers of Ti₃C₂T_xnanosheets. Ti₃C₂Tx/NaF composite with concentrations ranging from 1% to 5% were prepared using the hydrothermal method. The material was used to fabricate the electrode using Ni foam as substrate, and XRD, SEM and EDX were used for analysis of the nanocomposite material. Electrochemical testing was used to observe specific capacitance, coloumbic efficiency and cyclic stability. GCD curves are to determine the specific capacitance, energy, and power density. Electrochemical Impedance Spectroscopy (EIS) was utilized to measure the electrical conductivity of the electrode material.

2.1 Materials

Hydrofluoric acid (HF 48%), Hydrogen peroxide (H₂O₂ 35%), Tetramethylammonium hydroxide (TMAOH), Nickel foam was purchased from Sigma Aldrich and Co.

2.2 Synthesis of Ti3C2 MXene

As shown in Fig. 1(a) Ti₃C₂T_x MXene was obtained by selective etching selective etching of Si from Ti₃SiC₂ using a straightforward oxidant-assisted method similar to one reported earlier³³. The process begins by mixing 45 mL of diluted hydrofluoric acid (HF) with 5 mL of hydrogen peroxide (H₂O₂). (Caution: Hydrofluoric acid is an extremely corrosive substance, and it is of paramount importance to be fully cognizant of the associated risks and adhere to stringent safety protocols when working with HF and chemicals that generate HF). Hydrogen peroxide is added to accelerate the etching as titanium and carbide in the MAX phase have a strong bond so Si is difficult to etch with HF alone. The prepared solution was carefully placed in an ice bath under continuous stirring for 20 mins and 3 g of MAX powder was gradually introduced into the solution over time span of 20 mins. The solution was kept on continuous stirring for 2 hours at low temperature. Following this, the container was moved to a preheated silicone oil bath (at 50°C) and was constantly stirred for 45 hours at 500 rpm using a Teflon magnetic stirrer. This process facilitates separation Si from Ti₃SiC₂ and 2D structure is obtained. Subsequently, the obtained Ti₃C₂ was washed in DI water via centrifugation at 5000 rpm for multiple cycles to neutralize the pH and remove H₂O₂ and HF. Then the solution was vacuum-filtered using 0.2 ${\mu }$m filter paper, and the resulting powder was dried overnight in a vacuum oven set at 60°C. The MXene powder was subsequently subjected to delamination using tetramethylammonium hydroxide (TMAOH). The process involves soaking of MXene powder in TMAOH, followed by dilution with water, and magnetic stirring at 500 rpm for 24 hours. Afterwards, the pH was neutralized by washing using a centrifuge machine at 5000 rpm while continuously monitoring the pH. Additionally, during this process any remaining contaminants are cleaned as well. Then the solution was subjected to vacuum filtration using 0.2 ${\mu }$m filter paper and subsequently dried overnight in a vacuum oven at 40°C.

2.3 Synthesis of NaF-MXene composite

The synthesis of the NaF-MXene composite via a facile hydrothermal method was executed with meticulous attention. The procedure involves MXene dispersion in deionized water at a ratio of 20 mg/30 mL through 20 minutes of sonication, followed by a similar treatment of NaF dispersion (0.2 mg/20 mL) to ensure uniform distribution. These individual dispersions were subsequently amalgamated in a Teflon beaker and further sonicated for 30 minutes to achieve homogeneity. The resultant solution was then hydrothermally treated within a Teflon-lined autoclave at 90°C for 16 hours. Then the composite solution was vacuum filtrated and subsequently dried in a vacuum oven to eliminate residual solvents and water. The synthesis protocol was replicated to yield three distinct types of composites with NaF concentrations of 1%, 3%, and 5%, hereafter, referred as composite 1, 2 and 3, respectively.

2.4 Electrode Fabrication

The electrode fabrication process involves a sequence of precise steps as shown in Fig. 2. Initially, the nickel foam (1 cm²) was meticulously cleaned, starting with a rinsing in DI water, followed by a 10-minute through immersion in ethanol. Then the nickel foam was dried, at 60 ⁰C to 90 ⁰C until it was fully dried. For electrode fabrication slurry was formulated using precise proportions: 80% active material (Ti₃C₂T_x/NaF), 10% polyvinylidene difluoride (PVDF) binder, and 10% carbon black, all suspended in N-methyl pyrrolidone (NMP) solvent. After 10 minutes of sonication, the slurry was drop-casted on the cleaned Ni Foam substrate. Then it underwent an overnight drying process in a vacuum oven and was subsequently mechanically compressed using a hydraulic press machine under 500 PSI pressure for five seconds.

2.5 Characterization

Structural analysis of the Ti₃C₂T_x and Ti₃C₂Tx/NaF was performed using an X-ray diffractometer (DRON 8, BRUKER UNITED STATES) equipped with Cu Kα radiation as the X-ray source. Scanning Electron Microscopy (SEM), 6490A, JEOL Japan and energy dispersive X-ray spectroscopy (EDX) were used to study morphology and elemental distribution of the prepared samples. Gamry potentiostat was used to determine electrochemical properties. Three electrodes set up was used for CV, GCD and EIS measurements with composite material coated Ni foam as working electrode, Platinum wire as counter electrode and Ag/AgCl as reference electrode. The fabricated electrode was used as the working electrode. The chosen electrolyte was a 1M KOH solution and the specific capacitance was measured as:-

$C=\frac{1}{2\times s\times Vo\times \frac{dv}{dt}}{\int }_{{v}_{i}}^{{v}_{f}}I\left(V\right)dv$

(1)

Where I is the load current, V_o is the initial potential in the cyclic voltammograms, m is the mass of active material in the working electrode, v is the scan rate, and V is the potential window. The discharge time is obtained from the GCD curve, whereas energy and power density can be calculated from the discharge time using the following Eqs. (2) and (3).

$$\text{E} = \frac{1}{2}\times \text{C}{\times \left({\Delta }\text{V}\right)}^{2}\times \frac{1}{3,600}$$

P = $\frac{\text{E}}{\text{t}}$ $\times$ 3,600(3)

3.1 X-ray Diffraction Analysis (XRD)

The XRD patterns of commercial Ti₃SiC₂ MAX powder and the derived MXene were measured. Figure 3(a) shows XRD pattern of commercial Ti₃SiC₂ MAX powder, which has noticeable peaks at specific angles, such as 2θ = 9.10°, 20.05°, 31.30°, 34.50°, 37.70°, 39.50°, 41.30°, 42.50°, 58.40°, and 60.250°. These peaks correspond to distinct crystallographic planes inherent in the Ti₃SiC₂ structure. Figure 3(b) shows the shifted peaks for MXene at 2θ = 9.950°, 18.350°, 30.20°, 40.80°, and 60.85°. In the MXene several peaks were eliminated, whereas some peaks exhibited shifts compared to the initial pattern. The shift indicates increased interlayer spacing, while broadening of the (002) peak is due to Si layer substitution with functional groups (T_x), signifying exfoliation and delamination ³⁴. Moreover, the presence of a minor peak along the (104) plane in the MXene pattern suggest minute amount of silicon (Si) within the resulting Ti₃C₂Tx MXene material.

Figure 3(c) presents the XRD patterns of pristine Ti₃C₂T_x sample. The XRD pattern of Ti₃C₂T_x/NaF composite (composite 1) displays sharp peaks at 2θ = 8.12°, 25.28°, 33.68°, 39.09°, and 59.82° (see Fig. 3(d)) with few shifted to the left. The existence of additional peak at 2θ = 57.88° with the plane (220) suggests the impregnation of NaF into the layers and onto the surface of Ti₃C₂. Figure 3(e) displays sharp peaks centered at 2θ = 9.96°, 25.54°, 35.12°, 39.46°, 60.68° in the XRD pattern of the composite 2. The intensity of the peaks increases with the increasing doping concentration; a new NaF peak can be seen at 2θ = 58.32°. The XRD pattern composite 3 is shown in Fig. 3(f). The patterns have distinct peaks at 2θ = 8.95°, 25.20°, 35.150°, 40.80°, and 60.85°, which are slightly shifted from left to right. The shift might reflect of incorporation of NaF within the composite structure. Overall, XRD results with left shifted peaks and peaks for NaF at certain angles confirm the formation of the composite.

3.2 Morphological and structural Analysis of NaF-MXene composite

Figure 4(a-d) show SEM images of the Ti₃C₂T_x captured at 20 KV, which reveals accordion-like morphology suggesting formation of the delaminated Ti₃C₂Tx phase after selective etching of Si. Figure 5(a) shows EDX spectrum of Ti₃C₂T_x MXene, which reveals a considerable amount of Ti and carbon. Various termination group elements such as N, O, and F are present in the MXene.

Traces of Si are also present as impurities. The SEM and EDX images of Ti₃C₂T_x/NaF composite are shown in Figure. 4. Figure 4(e-h) shows SEM images of Ti₃C₂Tx/NaF composite 1. We can also see several NaF spots on the Ti₃C₂ surface, which complement XRD results. Figure 5 (b) show EDX spectra of the same sample which reveals significant amount of Ti and carbide, with a modest amount of Na and F, suggesting formation of NaF/Ti₃C₂T_x composite. Figure 4(i)-(l) and Fig. 4(m)-(p) show SEM images for composite 2 and composite 3, respectively.

All images indicate incorporation of NaF onto the surface of the MXene layers and the results are in agreement with the XRD findings. Figure 5(c) and Fig. 5(d) show EDX spectra of the composite 2 and composite 3, respectively. Both figures suggest incorporation of NaF in MXene, wherein that increased Na and F concentration in Fig. 5(d) suggest higher impregnation of NaF for composite formation.

3.3 Electrochemical performance of NaF-MXene composite

The electrochemical performance of the fabricated electrode was analyzed using cyclic voltammetry (CV) and Electrochemical Impedance Spectroscopy (EIS). Cyclic voltammetry (CV) analysis was conducted to assess the charge transfer rate at the electrolyte-electrode interface. Figure 6(a)-(c), are representative cyclic voltammetry (CV) curves of electrode fabricated from composite 1, composite 2 and composite 3 at different scan rates ranging from 2 mV/s to 200 mV/s. The nonrectangular shaped cyclic voltammograms exhibit the faradic behavior and occurrence of redox reaction during charging and discharging cycle thus suggesting the pseudo-capacitor behavior of the device. Furthermore, the Faradaic current peak across the scanned potential range signifies reversible charge and discharge at the electrode-electrolyte interface. A noticeable rise in the potential difference between oxidation and reduction peaks can be clearly seen. The potential difference between oxidation and reduction peaks increased with higher scan rates. This suggest increase in irreversible and quasi-reversible reactions at faster scan rate ^35,36. This shift is primarily attributed to the electrode's internal resistance and the polarization induced by the elevated scan rate ³⁷. Figure 6(d)-(f), respectively, indicate relationship between scan rate and capacitance for electrode fabricated from composite 1, composite 2 and composite 3, respectively. It is worthy to note that the specific capacitance becomes low at higher scan rates due to phenomenon, like limited ion diffusion, ohmic drop and non-ideal behavior of the electrochemical system. Contrarily, at lower scan rate, higher specific capacitance is due to enhanced ion diffusion, reduced ohmic drop and extended ionic adsorption on the electrode surface. We observed drop in capacitance from 191 F/g to 20 F/g for scan rate of 2 mV/s to 200 mV/s for device fabricated from composite 1. It was noted that capacitance reduces with the increasing concentration of NaF. For example, highest capacitance for composite 1 was 191 F/g, which was dropped to 137 F/g in case of composite 2. Smaller amount of NaF improve capacitance, however increased amount of NaF resulted in lower capacitance. The charge storage phenomenon for the developed electrodes were studied using Galvanostatic Charging Discharging (GCD). Figure 6(g)-(l), show GCD curves for electrode fabricated from composite 1, 2 and 3.

The plots show the charging and discharging at different gravimetric current densities within voltage range of 0.1–0.6 V. They exhibited symmetrical and triangular shaped charge discharge profiles suggest characteristic pseudocapacitive behavior of the electrode material. For stable operational current density range, we tested device at different values such as 6 A/g to 4, 3, 2, 1, 0.5, 0.1 A/g. The charging and discharging process was completed within 1 sec at a current density of 6 A/g. On the other hand, charging and discharging time significantly increased at 0.5 A/g; however, the device entered into a saturation region. This can be avoided by limiting voltage window from 0.6 V to 0.5 V. As illustrated in Fig. (h), (j), and (l), saturation region disappeared as soon as the voltage window was reduced. Energy density and power density were calculated using equations (2, 3). For example, highest energy density and power density of 6.63 Wh/g and 54.24 W/g were calculated for composite 1.

Electrochemical Impedance Spectroscopy (EIS) is an important tool which offers valuable insights into ion transfer and resistive as well as capacitive properties of the electrode. Figure 7, shows the EIS Nyquist plots for composite 1, 2 and 3, which were measured in a frequency range from 100 kHz to 10 MHz. Real and imaginary impedance are denoted by Z′ and Z″ ohm, respectively, whereas left and right portions of the curves refer to higher and lower frequencies, respectively. The intersection of plots on the real axis at higher frequencies indicates the internal resistance of the device, which include electrolyte resistance, electroactive material’s intrinsic resistance, and contact resistance ³⁸. Similarly, semicircle's diameter at high frequencies indicates faradic charge transfer resistance (R_ct) of the redox reactions, whereas, any inclined line at low frequencies corresponds to Warburg impedance ³⁹. Furthermore, the region of the graph with a 45^o slope at higher frequency region is attributed to higher diffusion rate. Figure 7 (a)-(b), clearly show a slope of 45^o at higher frequency region which corresponds to higher diffusion process in the composite with lower concentration of NaF leading to the higher capacitance. The result is in good agreement with CV results. The fitted model was applied to the actual model using Randle's model. For this purpose, an equivalent circuit using an ESR, a resistor, a capacitor, and a Warburg resistor was created as illustrated in the inset of Fig. 7. The increasing size of semicircle at the higher frequency region with decreasing content of NaF indicate lower charge transfer resistance at lower NaF.

We synthesized and characterized a novel Ti₃C₂T_x/NaF composite through hydrothermal process for potential energy storage applications. Three distinct composite samples were synthesized, each with varying concentrations of NaF (1%, 3%, and 5%). The electrochemical properties and behavior of these composites as supercapacitor electrodes were explored. The structural analysis of the composites was carried out using X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD patterns of the composites exhibited shifted peaks and new peaks associated with the presence of NaF, confirming the successful formation of the Ti₃C₂Tx/NaF composite. SEM images showcased the accordion-like morphology of Ti₃C₂Tx, indicating successful delamination, while NaF spots were observed on the surface, validating the incorporation of NaF in the Ti₃C₂Tx. Electrochemical performance was evaluated through cyclic voltammetry (CV), galvanostatic charging-discharging (GCD), and electrochemical impedance spectroscopy (EIS). The CV curves displayed characteristic pseudo-capacitive behavior, with reversible redox reactions during charge and discharge cycles. GCD analysis further supported the pseudo-capacitive nature of the composites, displaying symmetrical and triangular charge-discharge profiles. The energy density and power density of the composites were calculated, with composite 1 exhibiting the highest values of 6.63 Wh/g and 54.24 W/g, respectively. Furthermore, composite 1 showed considerably a specific capacitance of up to 191 F/g at a scan rate of 2 mV/s in KOH electrolyte. The presence of NaF influenced the charge transfer resistance and diffusion rate, with lower NaF concentrations resulting in improved charge transfer characteristics. The tailored properties of these composites, influenced by NaF concentration, offer promising avenues for advanced energy storage solutions.

Funding Acknowledgment:

The authors acknowledge the financial support from the Higher Education Commission of Pakistan under grant No: 5339/Federal/NRPU/R&D/HEC/2015 and project titled "Controlled Synthesis of Two-Dimensional Nanosheets and Multilayer For Electronic Devices"

Data availability

The datasets used and/or analyzed during the current study are available from the corresponding author on reasonable request.

Competing interest

Authors declare no Competing Financial or Non-Financial Interests

Author contributions

M. R. performed the experiments during synthesis of samples and performed different measurements. Initially he worked on data analysis and write 1^st version of manuscript. D. H. wrote the main manuscript, helped in figures (Prepared Fig-1 & 2), helps in data interpretation and reviewed the manuscript. S. U. A. conceptualized the idea, analyzed the data in detail, reviewed the manuscript and played a leading role as supervisor. S. R. co-supervised the project, provided the Lab facilities and helped in the process optimization. S. Z. helped during synthesis of samples and performing different measurements. S. S contributed in drafting manuscript and uplifted it’s English for final version. All authors reviewed the final version of the manuscript.

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No competing interests reported.

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Synthesis of 2-Dimensional Novel Ti₃C₂T_x/NaF nano-composites and Fabrication of Electrode for Electrochemical performance of Pseudo-capacitive Supercapacitor Device

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Journal Publication

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Abstract

Figures

1. Introduction

2. Materials and Methods

2.1 Materials

2.2 Synthesis of Ti3C2 MXene

2.3 Synthesis of NaF-MXene composite

2.4 Electrode Fabrication

2.5 Characterization

3. Results and discussion

3.1 X-ray Diffraction Analysis (XRD)

3.2 Morphological and structural Analysis of NaF-MXene composite

3.3 Electrochemical performance of NaF-MXene composite

4. Conclusion

Declarations

References

Additional Declarations

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Journal Publication

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