Adsorptive and Catalytic Ti3C2S2 MXene for High‐Performance Lithium–Sulfur Batteries

doi:10.21203/rs.3.rs-4938660/v1

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Adsorptive and Catalytic Ti₃C₂S₂ MXene for High‐Performance Lithium–Sulfur Batteries

https://doi.org/10.21203/rs.3.rs-4938660/v1

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MXenes have emerged as promising candidates for hosting sulfur in lithium-sulfur (Li-S) batteries due to their exceptional electrical conductivity. Despite recognition of the significant influence of functional groups on the MXene surface on sulfur conversion reactions, a clear experimental understanding remains elusive. This study unveils that Ti₃C₂ MXene functionalized with –S groups demonstrates superior capabilities in anchoring and catalyzing lithium polysulfides (LiPSs) compared to counterparts functionalized with –Cl and –F groups. The Ti₃C₂S₂ MXene is synthesized via the molten salt method, followed by functional group replacement. Ti₃C₂S₂ MXene exhibits robust chemisorption strength, effectively mitigating LiPS dissolution and shuttling. Additionally, it demonstrates remarkable electrocatalytic prowess for Li₂S deposition/decomposition, thereby enhancing reaction kinetics. As a result, Ti₃C₂S₂ MXene-modified separators allow Li-S cells to achieve a high capacity of 1305 mAh/g at 0.1 C, alongside excellent cyclic retention of ≈81% after 1000 cycles. Even with an S loading of 6.5 mg/cm², it attains a notable areal capacity exceeding 5.5 mAh/cm². This work underscores the potential of surface modification strategies in boosting the anchoring and electrocatalytic performance of Ti₃C₂S₂ MXene in Li-S batteries.

Materials Engineering

Ti3C2S2

MXene

lithium-sulfur batteries

modified separator

Lithium-sulfur (Li-S) batteries are at the forefront of next-generation energy storage systems, offering significantly higher theoretical energy densities compared to conventional lithium-ion batteries.^1,2 The promise of Li-S batteries is rooted in sulfur's high theoretical capacity (1672 mAh/g) and its natural abundance and environmental benignity.^3,4 However, several persistent challenges hinder their practical deployment, including the dissolution and shuttling of lithium polysulfides (LiPSs), poor conductivity of sulfur and its discharge products, and volume changes during cycling.^5,6 Addressing these issues is crucial for realizing the full potential of Li-S batteries.

Recent advancements in Li-S batteries have been driven by various strategies to mitigate the aforementioned challenges. One of the most explored approaches is the use of conductive carbon-based materials, such as graphene and carbon nanotubes, to improve the electrical conductivity of sulfur cathodes.^7,8 However, while these materials help in enhancing conductivity, they often fall short in effectively anchoring LiPSs, leading to significant capacity fade and poor cycle life.^9–13 Another strategy involves the incorporation of polar materials such as metal oxides, sulfides, and nitrides to chemically adsorb LiPSs and suppress their dissolution and shuttling.^14,15 For example, TiO₂ and MoS₂ have shown promise in binding LiPSs due to their polar surfaces,^16,17,18 but their relatively low electrical conductivity can limit the overall battery performance.

MXenes, particularly Ti₃C₂ MXene, have gained attention due to their unique combination of high electrical conductivity and tunable surface chemistry.^19,20 The versatility of MXenes stems from their ability to be functionalized with various surface groups, such as –OH, –O, –F, and –Cl, which can be tailored to enhance specific properties.²¹ Studies have demonstrated that functional groups on MXenes play a crucial role in their interaction with LiPSs and the overall electrochemical performance of the batteries.^22,23 For example, MXene with –Cl functional groups has been demonstrated to be superior than that with –F ones.²⁴ Furthermore, everal theoretical studies showed highlighted that Ti₃C₂ MXene with –S functional groups showed better LiPS adsorption capabilities compared to other functionalized counterpart.^22,25,26 Despite these advances, a clear experimental understanding of how different functional groups affect sulfur conversion reactions remains limited.

This study focuses on Ti₃C₂ MXene, a widely studied member of the MXene family, functionalized with various surface groups to elucidate their impact on sulfur chemistry. Specifically, we investigate Ti₃C₂ MXene functionalized with –S and –Cl groups to determine their effectiveness in anchoring and catalyzing LiPSs. Our findings reveal that Ti₃C₂ MXene functionalized with –S groups (Ti₃C₂S₂) exhibits superior performance in mitigating LiPS dissolution and enhancing electrocatalytic activity for Li₂S deposition/decomposition. The Ti₃C₂S₂ MXene is synthesized via the molten salt method, followed by functional group replacement, resulting in a material with robust chemisorption strength and remarkable electrocatalytic capabilities. When applied in Li-S cells, Ti₃C₂S₂ MXene-modified separators enable a high capacity of 1305 mAh/g at 0.1 C and excellent cyclic retention of approximately 81% after 1000 cycles. Even at a high sulfur loading of 6.5 mg/cm², the cells achieve a notable areal capacity exceeding 5.5 mAh/cm². This work underscores the potential of surface modification strategies in enhancing the anchoring and electrocatalytic performance of MXenes in Li-S batteries.

As schematically illustrated in Fig. 1a, Ti₃C₂S₂ MXene was synthesized using a molten salt etching and functional group replacement method from the Ti₃AlC₂ MAX phase with ZnCl₂ and Li₂S. Initially, Ti₃AlC₂ MAX was mixed with ZnCl₂ and annealed at 500°C to produce Ti₃C₂Cl₂ MXene. Subsequently, Ti₃C₂S₂ MXene was obtained by substituting –Cl groups with –S groups using Li₂S at 800°C. The identities and crystal structures of the samples were first verified using X-ray diffraction (XRD) analysis. The results indicate a shift in the (002) peak intensity of Ti₃AlCl₂ (JCPDS: #52–0875) to lower angles in both Ti₃C₂Cl₂ and Ti₃C₂S₂ MXene (Figure S1), suggesting significant crystal structure modification and successful exfoliation of the MAX phase. The (002) peaks of Ti₃C₂Cl₂ and Ti₃C₂S₂ MXene are located at 8.96° and 7.93°, corresponding to layer spacings of 9.82 Å and 11.14 Å, respectively. Scanning electron microscopy (SEM) was performed to examine the morphology of Ti₃C₂S₂ MXene, as shown in Fig. 1b-d. The SEM images confirm that the MXene exfoliates into a 2D layered accordion-like structure. Elemental mapping analysis (EDS) further confirms a homogeneous distribution of Ti, C, Cl, and O elements (Fig. 1e). These results conclusively demonstrate the successful synthesis of Ti₃C₂S₂ MXene.

Ti₃C₂S₂ was coated on the polypropylene (PP) separator to prepare modified separators (Fig. 2a). It can be seen that the Ti₃C₂S₂ MXene layer is evenly attached to the PP separator and it presents a uniform and smooth surface (Fig. 2b). The thickness of Ti₃C₂S₂ was only 10 µm (Fig. 2b). In addition, the Ti₃C₂S₂/PP composite separator remained undestroyed and attached after about 180° bends, indicating the excellent adhesion and flexibility (Figure S2).

We investigated the interaction of Ti₃C₂S₂ MXene with LiPSs using visual adsorption and catalysis tests. The adsorption capability of Ti₃C₂S₂ MXene was analyzed by immersing each sample in a 5 mM Li₂S₆ solution. After 5 hours of adsorption, the Li₂S₆ electrolyte mixed with Ti₃C₂Cl₂ MXene retained a yellow color (Fig. 3a), indicating limited adsorptivity. In contrast, the Li₂S₆ electrolyte treated with Ti₃C₂S₂ MXene became nearly colorless, demonstrating the strong adsorption ability of Ti₃C₂S₂ MXene toward LiPSs. This robust chemisorption is expected to effectively suppress the polysulfide shuttle effect.^28–30 Furthermore, the Ti₃C₂S₂-coated separator enhanced the symmetric cell's performance, as evidenced by a larger current response, lower reaction polarization, and higher reduction potentials compared to the Ti₃C₂Cl₂-coated separator (Fig. 3b). These findings indicate that Ti₃C₂S₂ MXene promotes faster sulfur conversion reaction kinetics.^31,32

To investigate the impact of Ti₃C₂S₂ MXene on electrochemical performance, Li–S cells with Ti₃C₂Cl₂- and Ti₃C₂S₂-modified separators were assembled and tested. The rate capabilities of these cells are presented in Fig. 4a. Cells with Ti₃C₂S₂-modified separators exhibited significantly higher reversible capacities compared to those with unmodified PP separators. As current densities increased, the advantages of the Ti₃C₂S₂-modified separators became even more pronounced. At a low rate of 0.1 C, the cells with Ti₃C₂S₂-modified separators achieved a high discharge capacity of 1305 mAh/g. Even at higher current densities, these cells maintained impressive discharge capacities of 1185, 1075, 943, 802, and 656 mAh/g at 0.2, 0.5, 1, 2, and 5 C, respectively. Notably, when the current densities were reverted to 0.1 C, the cells retained high reversible capacities of 1208 mAh/g, which correspond to 97% of the original discharge capacities, respectively. This stability and reversibility highlight the effectiveness of Ti₃C₂S₂-modified separators. In contrast, the capacities of cells with Ti₃C₂Cl₂-modified separators showed a sharp decline from 1203 mAh/g to 252 as the rates increased from 0.1 C to 5 C, respectively. Upon reducing the current densities back to 0.1 C, these cells displayed lower reversible capacities of 1011 mAh/g, corresponding to only 84.1% of the original discharge capacities. Figure 4b illustrates the long-term cycling performance of cells using Ti₃C₂S₂-modified separators. These cells demonstrated excellent performance, delivering discharge capacities of 695 mAh/g (81%) at 1 C after 1000 cycles. Importantly, the cells maintained a high Coulombic efficiency of nearly 100% over most cycles. Conversely, cells with Ti₃C₂Cl₂-modified separators exhibited a significantly larger capacity decay at the same rate. These results clearly demonstrate that Ti₃C₂S₂ outperforms Ti₃C₂Cl₂ in enhancing both the rate capability and cycling stability of Li–S batteries.

Figure 5 illustrates the cycling performance of cells using Ti₃C₂S₂-modified separators with varying sulfur loadings, aimed at assessing the impact of Ti₃C₂S₂ MXene on the electrochemical performance at higher sulfur loadings. For a sulfur loading of 5.0 mg/cm², the cells with Ti₃C₂S₂-modified separators exhibit an initial discharge capacity of 4.69 mAh/cm². Even after 100 cycles, these cells maintain an excellent discharge capacity of 3.35 mAh/cm², corresponding to a high capacity retention of 71%. The charge/discharge curves for the 1st and 100th cycles, shown in Figure S3, reveal no significant change in the plateau potential, further demonstrating the high reversibility of the Ti₃C₂S₂-modified separators. When the sulfur loading is increased to 6.5 mg/cm², the cells with Ti₃C₂S₂-modified separators continue to exhibit strong cycling performance, with high capacity retentions of 4.21 mAh/cm² after 100 cycles. These results clearly demonstrate that Ti₃C₂S₂ effectively enhances the electrochemical performance of cells, even at higher sulfur loadings.

In conclusion, our research demonstrates the significant potential of Ti₃C₂ MXene functionalized with sulfur in addressing the critical challenges faced by Li-S batteries. By leveraging the robust chemisorption and electrocatalytic properties imparted by the sulfur functional groups, Ti₃C₂S₂ MXene effectively mitigates LiPS dissolution and enhances the sulfur conversion reactions. The superior performance of Ti₃C₂S₂ MXene-modified separators, evidenced by high specific capacities, excellent cyclic retention, and remarkable areal capacities, underscores the effectiveness of this functionalization strategy. The success of Ti₃C₂S₂ MXene in achieving a high capacity of 1305 mAh/g at 0.1 C and maintaining approximately 81% cyclic retention after 1000 cycles, even at high sulfur loadings, positions it as a promising material for next-generation energy storage systems. This study paves the way for further exploration of functionalized MXenes, not only broadening the understanding of their role in Li-S battery chemistry but also opening new avenues for the development of advanced materials in energy storage technologies.

Experimental

Synthesis of Ti₃C₂Cl₂ and Ti₃C₂S₂

Ti₃C₂Cl₂ was prepared via the molten salt method. Firstly, 0.5 g Ti₃AlC₂ powder and 3 g ZnCl₂ powder were mixed in a mortar and moved into a graphite crucible. Then, the graphite crucible was kept at 500°C for 6 h under an Ar atmosphere. The heating rate was set at 5°C/min. After natural cooling, the samples were continuously stirred in hydrochloric acid solution (1 M) for 2 h at room temperature. After that, the powder was filtrated and washed with high-purity water, and dried for 24 h under vacuum at 35°C to obtain the Ti₃C₂Cl₂. Ti₃C₂Cl₂ was prepared by substituting –Cl groups with –S groups using Li₂S at 800°C.

Material characterization

The X-ray diffraction (XRD, D8 Advance, Bruker) was performed to evaluate the phase composition with Cu − Kα radiation (λ = 0.154 nm) from 5 to 65°. The morphologies and elements distribution were verified using the scanning electron microscopy (SEM, JSM-IT300, JEOL) with energy dispersive spectrometry (EDS, X-Max N20, Oxford Instruments).

Electrochemical measurements

To prepare the cathodes, the mixture of 80%wt CNTs/S, 10%wt acetylene black (AB) and 10%wt polyvinylidene fluoride (PVDF) were blended for 2 h in N-methyl-2-pyrrolidone (NMP) to prepare the slurry. Then, the slurry was coated on an Al foil and then dried at 70°C for 10 h. The sulfur loading of the cathode was around 1.0, 5.0, and 6.5 mg cm^− 2.

The electrochemical performances were evaluated by assembling CR2032 coin cells with Li foil anodes and Ti₃C₂Cl₂- and Ti₃C₂S₂-modified separators. The electrolyte consists of 1.0 M lithium bis(trifluoromethane)sulfonimide (LiTFSI) and 0.1 M LiNO3 dissolved in 1,3-dioxolane (DOL) and 1,2-dimethoxyethane (DME) solvents (1:1 in volume).

The electrochemical workstation (CHI760) was employed to collect the cyclic voltammetry (CV) curves (from 1.7 to 2.8 V at 0.1 mV s^− 1) and the electrochemical impedance spectroscopy (EIS) Nyquist plots (with a frequency range of 10^–2 to 105 Hz and an amplitude of 5 × 10^–3 V). LAND CT2001A system was used for galvanostatic charge-discharge (GCD) measurements between 1.7 and 2.8 V.

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The authors declare no competing interests.

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Adsorptive and Catalytic Ti₃C₂S₂ MXene for High‐Performance Lithium–Sulfur Batteries

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