Impact of Mesoporous Carbon Structure on Sulfur Utilization and Electrochemical Performance in Lithium-Sulfur Batteries

Impact of Mesoporous Carbon Structure on Sulfur Utilization and Electrochemical Performance in Lithium-Sulfur Batteries | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Impact of Mesoporous Carbon Structure on Sulfur Utilization and Electrochemical Performance in Lithium-Sulfur Batteries Waleed Jan, Adnan Daud Khan, Faiza Jan Iftikhar This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7083420/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 26 Dec, 2025 Read the published version in Journal of Applied Electrochemistry → Version 1 posted 9 You are reading this latest preprint version Abstract Lithium-sulfur batteries (LiSBs) have emerged as a promising alternative for next-generation high-energy-density storage systems due to their exceptional theoretical specific capacity (1675 mAh/g) and high energy density (2600 Wh/kg). However, achieving practical performance remains challenging due to issues such as poor sulfur utilization, polysulfide shuttling, and limited cycle stability. The structural and compositional properties of mesoporous carbon materials in the cathode, particularly CMK-3, CMK-5, and CMK-8, play a crucial role in overcoming these limitations. These materials influence electrical conductivity, sulfur retention, and electrochemical stability, making their selection and optimization vital for improving LiSB efficiency. This study systematically investigates the interplay between sulfur loading, energy density, discharge capacity, and carbon structure at the cell level using experimental characterization. Results indicate that CMK-8 offers the most favorable performance, combining high sulfur loading capacity with strong polysulfide retention and enhanced cycling stability due to its large pore volume and interconnected structure. CMK-3 displays moderate electrochemical stability, particularly at lower sulfur loadings, but suffers from performance decline under high loading conditions. In contrast, CMK-5 exhibits the weakest electrochemical performance, with significant capacity fading and poor coulombic efficiency, indicating that its pore architecture is less suitable for effective sulfur confinement and long-term cycling. The findings reveal that moderate sulfur loading, rather than excessive sulfur incorporation, yields the best balance between high discharge capacities, capacity retention, and long-term cycling performance. By optimizing carbon pore structures, sulfur distribution, and cathode architecture, this research offers valuable insights into the design of high-performance LiSBs. The results contribute to the development of next-generation LiSBs with enhanced energy densities, paving the way for their practical deployment in energy storage applications, electric vehicles, and portable electronics. sulfur carbon cathode sulfur loading energy density Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 1. INTRODUCTION There has been considerable interest in developing rechargeable batteries other than lithium-ion (Li-ion) over the last couple of decades in search of higher energy density [ 1 ]. In comparison to the widely used Li-ion batteries (LIBs), the lithium-sulfur battery (LiSB) has shown great promise due to its higher theoretical specific energy and capacity [ 2 ]. Due to the abundant availability of sulfur, utilizing it as an active material in LiSBs will result in reduced costs [ 3 ]. Despite many efforts and notable breakthroughs, LiSBs still face challenges, namely inadequate system-level energy densities, performance challenges, and high operation costs, preventing their commercialization. Polysulfide shuttle mechanism, sulfur insulating properties, and inefficient cathode designs all contribute to these problems [ 4 ]. Researchers are optimizing sulfur loading, electrolyte-to-sulfur ratio, and addressing the polysulfide shuttling effect to enhance LiSB performance. Materials like MnO 2 and V 2 O 5 have shown strong polysulfide adsorption, improving efficiency. Innovations such as single-atom catalysts and encapsulating polysulfide electrolytes aim to mitigate the shuttle effect and extend battery lifespan. Efforts also focus on predicting performance, developing commercial parameters, and introducing novel materials to advance LiSB technology [ 5 ]. For LiSBs to achieve high performance, efficient cathode design is an essential approach [ 6 ]. Researchers have recently undertaken comprehensive modeling and definition of critical parameters, specifically the electrolyte/sulfur (E/S) and carbon/sulfur (C/S) ratios, for optimizing LiSBs [ 7 – 10 ]. A vital factor in the cathode design is the sulfur loading, which determines LiSB performance greatly; high sulfur loading will enhance the energy density of LiSBs [ 11 ]. To attain a high discharge capacity and expanded cycle life, LiSBs should have high E/S ratios and low Sulfur loading (average literature studies show Sulfur loading of up to 2 mg/cm 2 and E/S ratios of 36 mL/g) [ 12 , 13 ]. However, LiSBs have low energy densities because of the excessive electrolyte concentration and inadequate active material loading in the cathode, making them practically unusable in the global market [ 14 , 15 ]. Based on the discovered results, Eroglu and colleagues proposed that LiSBs should have a sulfur loading exceeding 7 mg/cm 2 for a consistently high energy density across the battery [ 16 ]. Moreover, Chung and colleagues put forward the claim that LiSBs targeted for high energy density must have a sulfur loading exceeding 6 mg/cm² [ 17 ]. Despite a few recent experiments, high sulfur loading investigations are limited, owing mostly to the challenge of creating thick and mechanically robust cathodes. In a study conducted by Cheon et al., cathode thickness was found to impact the LiSB performance. A thick Li 2 S layer causes a high diffusional resistance, which results in a decrease in sulfur utilization as the cathode thickness increases [ 18 ]. The choice of carbon material in the cathode plays a pivotal role in determining electronic conductivity, sulfur retention, and polysulfide suppression. Mesoporous carbon structures with high surface area and tailored pore sizes have been widely explored to mitigate the adverse effects of polysulfide shuttling and sulfur’s insulating nature. CMK-3, CMK-5, and CMK-8, a family of ordered mesoporous carbons, offer large pore volumes, interconnected structures, and tunable surface areas, making them promising sulfur hosts. Among these, CMK-8 demonstrates superior polysulfide retention due to its larger pore size and interconnected pore network, which supports higher sulfur utilization and enhanced cycle stability. The incorporation of mesoporous carbons into the cathode matrix enhances electrochemical stability and energy efficiency. Recent studies have examined the impact of different surface areas and pore structures in activated carbon materials [ 19 ]. For instance, Xiang et al. stated in their investigation that a specific pore volume and carbon particle size are critical for achieving large sulfur loading and sulfur utilization [ 20 ]. According to Barchasz et al., the amount of polysulfide deposited on the cathode at discharge was regulated by the size of the carbon grain. Furthermore, large electrode surface areas prevent full electrode passivation, improving battery discharge performance [ 21 ]. In the literature, various surface areas and pore diameters of activated carbon have been examined [ 22 ]. A large surface area and tiny pores are required to attain high sulfur use and discharge capacity [ 23 ]. Yu et al. introduced Nitrogen-functionalized porous carbon/CNT hybrid nanowires as a bifunctional interlayer for high-performance LiSBs, enhancing polysulfide trapping, adsorption, and conversion. The coating enables the deposition of lithium polysulfide, which inhibits the shuttle effect, while the CNT backbone ensures a conductive network for electron/ion transport. The nitrogen-doped surface captures lithium polysulfides, promoting conversion and lithium sulfide growth, improving battery performance. After 700 cycles at 0.5 C, the CNTNC-10 interlayer maintains a high initial capacity of 1395.4 mAh/g with a low decay rate of 0.025, demonstrating excellent stability. It also shows outstanding rate performance, delivering 765.9 mAh/g at 2000 mA/g, highlighting its potential for enhancing LiSBs [ 24 ]. LiSBs could benefit from an improved cathode design by addressing mass and charge transport problems [ 25 , 26 ]. Enhancing electrochemical performance can be achieved through the utilization of hollow carbon microspheres doped with nitrogen and embedded with cobalt within a cathode composed of carbon and sulfur, which provides a substantial area for sulfur loading [ 27 ]. A distinct study proposes an inventive cathode design to mitigate the shuttle effect of polysulfides. This design entails encapsulating a hollow carbon skeleton with an interconnected spacing [ 28 ]. High porosity carbon nanofiber cathodes not only provide high sulfur utilization but also allow electrolyte permeability [ 29 ]. Liu et al. demonstrated that high efficiency and cyclic stability in LiSBs were achieved using Co 3 O 4 nanocages encased in microcapsules with metal-organic frameworks (MOFs) [ 30 ]. There has been a lot of research on how different types of carbon affect LiSB’s electrochemical characteristics, but little is known about how different carbon features affect battery performance at the cell or system level. The impacts of the type of carbon and the amount of sulfur on the electrochemical properties of the LiSB at the cell and system levels were investigated in this work using experimental methodologies. This study systematically investigates the effects of CMK-3, CMK-5, and CMK-8 as cathode materials in LiSBs, focusing on their structural properties, sulfur retention capabilities, and electrochemical performance. By analyzing the relationship between surface area, pore volume, particle size, and sulfur loading, we provide a comprehensive understanding of how mesoporous carbon influences capacity retention, cycle stability, and rate performance. These insights contribute to the development of optimized cathode architectures that enhance LiSB efficiency, paving the way for higher energy densities and longer cycle life in next-generation battery systems. 2. RESULTS AND ANALYSIS Figure 1 shows the voltage curves for LiS cells with different sulfur loading and mesoporous carbon cathodes. The discharge profiles in Fig. 1 illustrate the electrochemical response of LiSBs employing CMK-3, CMK-5, and CMK-8 as host materials, each evaluated at varying sulfur loadings. A clear trend emerges across all samples: lower sulfur loadings (in the range of 1.3–1.8 mg/cm²) consistently yield higher initial discharge capacities, whereas increasing the sulfur content results in diminished capacity. This decline is attributed to limitations in Li-ion accessibility and ineffective electrochemical conversion processes at elevated sulfur levels [ 31 ]. Excessive sulfur accumulation within the porous matrix likely impedes full electrochemical participation due to pore clogging, leading to polysulfide buildup at the carbon interface, where further reduction forms insoluble species such as Li₂S₂ and Li₂S that block active sites [ 32 ]. Among the three hosts, CMK-3 demonstrates relatively stable discharge behavior even at higher loadings (up to 3.1 mg/cm²), maintaining a well-defined two-plateau profile characteristic of sulfur redox reactions. This implies that its highly ordered mesoporous architecture promotes uniform sulfur distribution, effective polysulfide confinement, and sufficient ion transport pathways, thereby mitigating the impact of cathode thickening. In contrast, CMK-5 exhibits less defined plateaus and steeper voltage decay, especially as loading increases, indicating increased polarization and mass transport limitations. The less favorable performance suggests suboptimal pore connectivity and reduced electrolyte accessibility, which hinders both redox kinetics and sulfur utilization under higher load conditions. CMK-8, while capable of delivering extended discharge capacity at lower loading, shows partial suppression of the low-voltage plateau with increased sulfur content. This indicates hindered conversion of intermediate polysulfides to Li₂S, which is crucial for maximizing energy output. The observed decline is likely exacerbated by insufficient electrolyte infiltration in thicker electrodes, a well-documented challenge in high-loading LiSBs the due to the low wettability of sulfur and carbon materials with organic electrolytes [ 33 ]. As the cathode thickens, inadequate wetting and poor ionic conductivity exacerbate polarization, leading to capacity fade and an increased voltage drop. Furthermore, diminished electronic conductivity across thicker electrodes may also contribute to the loss of plateau clarity and overall electrochemical inefficiency. Figure 2 presents the electrochemical performance of the CMK-3, CMK-5, and CMK-8 cathodes under moderate sulfur loadings, focusing on capacity retention and coulombic efficiency. Among them, CMK-8 demonstrates the most stable behavior, characterized by a relatively flat capacity curve and narrow error bars. This suggests efficient sulfur confinement and consistent ion transport, likely facilitated by its favorable pore architecture. CMK-3 shows intermediate performance, with a gradual capacity decline over cycles that may be attributed to limited pore accessibility or weaker interaction with sulfur species, despite having a similar sulfur loading to CMK-8. In contrast, CMK-5 performs the worst, exhibiting a sharp capacity drop and unstable coulombic efficiency. Its poor performance is likely due to inadequate sulfur utilization and significant polysulfide loss, aggravated by suboptimal pore connectivity and insufficient electronic pathways. Notably, the prominent fluctuations observed in the retention curves of CMK-5, and to a lesser extent, CMK-3, indicate unstable redox kinetics and uneven sulfur reactivation during cycling. These variations may result from transient pore blockages by Li₂S/Li₂S₂, inconsistent electrolyte penetration, or inhomogeneous sulfur distribution. For CMK-5 in particular, the combination of higher sulfur content and poorly interconnected mesopores likely contributes to localized concentration gradients and increased polarization, leading to erratic capacity behavior. Interestingly, CMK-8 exhibits a slight increase in capacity during the initial 60 cycles, which can be attributed to an electrochemical activation phase. This involves improved wetting of the porous matrix, redistribution of active sulfur species, and more effective polysulfide confinement. However, beyond this activation period, a gradual decline is observed, likely due to electrode degradation, pore clogging by insulating discharge products, and reduced electronic connectivity within the thickened cathode. These factors collectively diminish sulfur utilization and increase internal resistance, contributing to long-term capacity fading. The galvanostatic discharge profiles of CMK-3, CMK-5, and CMK-8 cathodes, as shown in Fig. 3 , illustrate clear distinctions in their electrochemical response and capacity retention over extended cycling. In the initial stages, all three materials exhibit the characteristic two-step discharge process of LiSBs, reflecting the sequential reduction of elemental sulfur (S₈) to soluble long-chain polysulfides (~ 2.3–2.1 V), followed by conversion to insoluble short-chain species and Li₂S (~ 2.1–1.7 V). However, the stability and clarity of these features evolve differently depending on the carbon matrix. CMK-3 displays prominent discharge plateaus in the first cycle, suggesting effective sulfur activation and relatively uniform reaction kinetics. Yet, by the 100th cycle, the high-voltage plateau is largely diminished and overall capacity declines from approximately 800 mAh/g to below 500 mAh/g. This fading behavior, coupled with increasing voltage hysteresis, signals a gradual loss of active material and growing internal resistance, likely due to incomplete polysulfide retention and electrode degradation. CMK-5, despite its initially high capacity (~ 850 mAh/g), shows rapid deterioration. The plateaus are poorly defined from the outset, and the profiles become increasingly sloped and indistinct with cycling. By the 100th cycle, the discharge curve is nearly featureless, and capacity drops significantly. Such behavior points to ineffective sulfur confinement and hindered redox activity, likely resulting from an unsuitable pore structure or inhomogeneous sulfur distribution, exacerbated by the higher loading. In comparison, CMK-8 maintains better structural and electrochemical stability. Its discharge curves remain more consistent through the 10th cycle, and even by the 100th, the lower-voltage plateau remains discernible. Although capacity decreases from ~ 750 mAh/g to ~ 500 mAh/g, the slower rate of decay and retention of plateau features suggest improved redox reversibility and stronger resistance to degradation. The moderate increase in hysteresis further supports the conclusion that CMK-8 provides a more efficient framework for polysulfide management. Overall, these results emphasize that the mesostructure of the carbon host plays a more critical role than sulfur loading in determining long-term battery performance. CMK-5, with the highest sulfur content, fails to deliver sustained capacity due to poor structural compatibility, whereas CMK-8 achieves better cycling outcomes despite similar loading to CMK-3. The progressive loss of discharge features and increase in polarization across all samples highlight the ongoing challenge of stabilizing polysulfide species in LiSBs. Figure 4 compares the electrochemical performance of LiSBs with varying sulfur loadings using three mesoporous carbon hosts: CMK-3, CMK-5, and CMK-8. The first plot illustrates peak discharge capacities, which initially increase with sulfur loading, reaching a maximum near 2.0 mg/cm², followed by a sharp decline at higher loadings. This behavior reflects the trade-off between increased active material and the onset of transport limitations, including reduced electronic pathways, hindered electrolyte penetration, and enhanced polarization. Among the materials, CMK-8 achieves the highest initial capacity (~ 900 mAh/g), attributed to its large pore volume and interconnected 3D framework that promotes efficient redox reactions. However, this advantage rapidly diminishes at higher loadings due to non-uniform sulfur deposition and mechanical rigidity, which compromise structural integrity and ion transport. CMK-3, with its linear mesoporous structure, displays more moderate but stable performance across the tested range. While its peak capacity is lower, it demonstrates greater tolerance to increased sulfur content, likely due to better mechanical robustness and more uniform sulfur distribution. CMK-5, in contrast, exhibits limited performance overall but uniquely peaks at ~ 2.3 mg/cm² in the 50th -cycle data (Plot 2), suggesting it may momentarily facilitate high utilization at specific loadings. Nevertheless, its steep capacity fade beyond this point points to poor long-term stability and inefficient charge transport. The third plot reveals a consistent decline in average discharge voltage with increasing sulfur loading for all cathodes. This reduction is indicative of higher overpotentials, decreased reaction kinetics, and elevated internal resistance under thicker electrode configurations. CMK-8 again shows the most favorable voltage profile, consistent with its lower polarization and faster charge transfer, while CMK-5 suffers from the greatest voltage suppression, confirming its poor conductivity and limited electrochemical reversibility. Collectively, these results highlight the delicate balance required between structural accessibility, mechanical resilience, and sulfur distribution. Optimizing pore architecture is critical for maximizing capacity while preserving cycling stability in mesoporous carbon-based sulfur cathodes. Figure 5 presents system-level modeling results for LiSBs incorporating CMK-3, CMK-5, and CMK-8 carbon hosts, showing projected trends in specific energy (Wh/kg, Plot 1) and energy density (Wh/L, Plot 2) as a function of sulfur loading. These projections incorporate electrode-level electrochemical data and account for inactive material contributions, making them highly relevant for practical cell design. In Plot 1, specific energy improves with increasing sulfur content up to approximately 2.0 mg/cm² across all carbon types. This initial rise reflects enhanced active material utilization and a favorable balance between energy output and structural support. Beyond this point, however, the trends begin to diverge sharply. CMK-8 exhibits a continued upward trajectory in specific energy, reaching values above 90 Wh/kg at higher loadings. This suggests not only excellent electrochemical performance at the material level but also a structural framework capable of accommodating thick electrodes without substantial loss of efficiency. Its 3D pore connectivity likely ensures sustained electronic and ionic transport even as sulfur content increases. CMK-3 demonstrates more conservative gains, with specific energy plateauing near 75 Wh/kg. Although this material lacks the steep drop-off observed in CMK-5, its relatively flatter curve at higher loadings implies diminishing returns as thickness increases—likely due to diffusion limitations and moderate conductivity that constrain further performance improvement. This makes CMK-3 more stable but less scalable for high-energy applications. CMK-5 presents a markedly different profile, characterized by a sharp peak near 1.6 mg/cm² followed by a steep decline. This behavior highlights a critical performance bottleneck in mass transport or charge transfer beyond optimal sulfur content. The collapse in specific energy at higher loadings suggests that CMK-5’s pore architecture cannot sustain efficient electrochemical reactions once the electrode becomes too thick or poorly infiltrated with electrolyte. In this context, system-level modeling reveals that even a material capable of high areal capacity under ideal lab-scale conditions may fail to deliver in realistic configurations if it lacks sufficient structural and transport resilience. Plot 2 reinforces these observations in terms of volumetric performance. CMK-8 achieves the highest energy density (~ 120 Wh/L), peaking around 2.0 mg/cm² before experiencing a modest decline and then recovering at higher sulfur levels. This non-monotonic behavior likely reflects the interplay between improved packing density and increasing internal resistance. The ability to rebound in performance at higher loadings further underscores CMK-8’s mechanical integrity and efficient pore utilization. CMK-3, while lagging behind in absolute performance, maintains a relatively flat curve beyond 2 mg/cm², indicative of predictable and stable volumetric output, albeit with limited room for optimization. In contrast, CMK-5 again suffers a dramatic collapse after its peak, emphasizing its unsuitability for thick-electrode formats where electrolyte access and sulfur retention are critical. Taken together, these projections reveal the decisive impact of host structure on energy delivery at the system level. While CMK-5 may appear competitive at moderate sulfur loadings, its rapid degradation under practical constraints negates that advantage. CMK-3 offers dependable, if unspectacular, performance, suitable for applications prioritizing stability. CMK-8 stands out as the most promising candidate, combining scalability with high energy yields, both gravimetric and volumetric, due to its synergistic structural and conductive properties. These findings underscore the necessity of integrating system-level modeling early in the materials development pipeline to identify architectures that retain electrochemical advantages under real-world constraints. For LiSBs targeting commercial viability, such predictive assessments are essential in bridging the gap between lab-scale results and practical energy storage solutions. 3. EXPERIMENTAL METHODOLOGY Various mesoporous carbon materials were mixed with sulfur (purchased from Sigma Aldrich) and a binder (polyvinylidene fluoride, PVDF, obtained from MTI) using a mortar and pestle for 15 minutes. The carbon sources utilized in this study were CMK-3, CMK-5, and CMK-8, selected for their high surface area, tunable pore structures, and enhanced sulfur retention capabilities. The main properties of the mesoporous carbon materials that were examined are comprehensively outlined in Table 1 . Table 1 Essential Characteristics of the Investigated Carbon Materials Name Total pore Volume (cm³/g) Pore Diameter (nm) Micropore Volume (cm³/g) Micropore surface area (m 2 /g) BET Surface area (m 2 /g) Particle’s Size (nm) Electrical Conductivity (S/cm) Tap density (g/cm 3 ) CMK-3 1.2–1.5 3–5 0.05–0.15 100–300 1000–1500 30–50 20–60 0.3–0.5 CMK-5 1.3–1.7 4–6 0.05–0.20 150–350 1100–1500 50–80 15–50 0.3–0.5 CMK-8 1.0–1.4 5–7 0.10–0.25 200–400 800–1200 100–150 10–40 0.25–0.45 A 20/70/10 weight percentage was adjusted for carbon/sulfur/binder. The solid mixture was dissolved using N-methyl-2-pyrrolidone (NMP, obtained from MTI) solvent until a homogeneous slurry was achieved. Afterwards, a magnetic stirrer was used to mix the slurry overnight at room temperature before mixing it again at 60°C for two hours. In the end, the slurry went through a three-hour ultrasonic treatment. As soon as the slurry had been homogenized, it was cast using the doctor blade technique (15 mm thick, procured from MTI) onto an aluminum current collector. During casting, the slurry's thickness was adjusted to control the cathode's Sulfur loading between 0.6 and 3.1 mg/cm 2 (calculated as 300, 550, 700, or 800 µm). After drying overnight at 60°C in the oven, the electrodes were annealed for four hours at 60°C. As discussed in the previous section, LiSBs perform better when sulfur is encapsulated in nanocarbon structures. Since we wanted to look into sulfur loading and carbon characteristics in a way that was easy to understand, we conducted this study using the most popular traditional cathode manufacturing method. This study employed the fabrication of two-electrode CR2032 coin cells within an Ar-filled glove box (Siemens, O 2 and H 2 O concentrations < 0.5 ppm). The Celgard polymeric separator (with an area of 3.02 cm 2 and a thickness of 25 mm, obtained from MTI) was utilized as the separator, and the anode consisted of a lithium metal foil (with an area of 2.01 cm 2 and a thickness of 160 mm, obtained from MTI). To prepare the liquid electrolyte for the cells, a 0.1M solution of lithium nitrate (LiNO 3 ) (purchased from Sigma Aldrich) was combined with a 1M solution of lithium BIS(trifluoromethanesulfonyl)imide (LiTFSI) (obtained from Sigma Aldrich). The electrolyte was dissolved in a blend of 1,3-dioxolane (DOL, procured from Sigma Aldrich) and 1,2-dimethoxyethane (DME, procured from Sigma Aldrich) at a volume ratio of 1:1. Following this, the electrolyte amount in each cell sample was modified to attain the desired E/S ratio of 12 µLm/g, a critical parameter for optimizing capacity retention rates. The Neware galvanostatic battery cycler was utilized to assess cell performance at room temperature by applying a current rate of 0.5 C, considering LiSB's theoretical capacity of 1675 mAh/g. 4. CONCLUSION This study systematically evaluated the electrochemical consequences of employing different mesoporous carbon architectures, specifically CMK-3, CMK-5, and CMK-8, as cathode hosts in LiSBs, while also varying the active material loading. The findings conclusively demonstrate that the specific structural attributes of the carbon host profoundly dictate battery behavior, influencing sulfur utilization, polysulfide management, and long-term stability. CMK-8 emerged as the superior performer among the tested materials, exhibiting enhanced capacity retention and greater stability over prolonged cycling, particularly when accommodating higher sulfur levels (up to its studied limits). This advantage is attributed to its larger pore dimensions (5–7 nm) and well-interconnected three-dimensional network, which appear crucial for physically confining soluble polysulfide intermediates, mitigating their detrimental shuttle effect, and facilitating sustained ion and electron transport even within the thicker electrode structures necessitated by higher loadings. In contrast, CMK-5, despite possessing a comparable theoretical surface area and pore volume to CMK-3, displayed rapid performance degradation and poor coulombic efficiency, especially as sulfur content increased. This suggests its specific pore architecture (4–6 nm, potentially less interconnected or with different tortuosity) is less adept at effectively trapping soluble intermediates or maintaining conductive pathways under operational stress, leading to significant polarization, active material loss, and overall electrochemical inefficiency. CMK-3, with its ordered linear mesopores (3–5 nm), presented intermediate results, offering reasonable initial stability but ultimately showing limitations in maintaining high performance at elevated sulfur loadings compared to CMK-8, likely due to constraints in ion diffusion pathways or less effective volume accommodation for sulfur species. Crucially, the study reinforced that merely increasing sulfur loading is not a universally beneficial strategy. An optimal loading threshold, generally observed around 2.0 mg/cm² in these systems, provided the best balance between capacity and stability. Beyond this point, all systems suffered from diminished specific capacity, increased voltage hysteresis, and faster fading. This decline stems from aggravated mass transport limitations, incomplete active material utilization due to pore clogging or poor electrolyte penetration deep within the thicker cathode, and amplified polarization effects. System-level energy density projections further substantiated these experimental observations, highlighting CMK-8's potential for achieving higher practical gravimetric (Wh/kg) and volumetric (Wh/L) energy densities due to its ability to better sustain performance at higher, more application-relevant loadings. Therefore, this research underscores that advancing LiSBs necessitates a sophisticated approach to cathode design, focusing critically on tailoring the carbon host's architecture, balancing pore volume, size distribution, connectivity, and mechanical stability, to effectively manage the complex sulfur redox chemistry and achieve durable, high-energy storage. Declarations Conflicts of Interest: The authors declare no conflict of interest. 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Energy Fuels 34(3):3931–3940 Su L, Zhang J, Chen Y, Yang W, Wang J, Ma Z, Shao G, Wang G (2021) Cobalt-embedded hierarchically-porous hollow carbon microspheres as multifunctional confined reactors for high-loading Li-S batteries. Nano Energy 85:105981 Zhang S, Xu Z, Jiang Z, Xiao Z, Tang A, Yang H (2022) The unique interconnected structure of hollow carbon skeleton doped by F and N facilitating rapid Li ions diffusion in lithium-sulfur batteries. Carbon 195:207–218 Saroha R, Cho JS (2022) Nanofibers comprising interconnected chain-like hollow N‐doped C nanocages as 3D free‐standing cathodes for Li–S batteries with super‐high sulfur content and lean electrolyte/sulfur ratio. Small Methods 6(5):2200049 Liu J, Zhu Y, Cai J, Zhong Y, Han T, Chen Z, Li J (2022) Encapsulating Metal-Organic-Framework Derived Nanocages into a Microcapsule for Shuttle Effect-Suppressive Lithium-Sulfur Batteries. Nanomaterials 12(2):236 Chen H-J, Yang S, Zhang M-Y, Sun Q (2024) Embedding covalent sulfur composite inside mesoporous carbon doped with Ni-N sites for high-performance lithium-sulfur batteries. J Energy Storage 91:112027 Lu D, Li Q, Liu J, Zheng J, Wang Y, Ferrara S, Xiao J, Zhang J-G, Liu J (2018) Enabling high-energy-density cathode for lithium–sulfur batteries. ACS Appl Mater Interfaces 10(27):23094–23102 Sun F, Qu Z, Wang H, Liu X, Pei T, Han R, Gao J, Zhao G, Lu Y (2021) Vapor deposition of aluminium oxide into N-rich mesoporous carbon framework as a reversible sulfur host for lithium-sulfur battery cathode. Nano Res 14:131–138 Additional Declarations No competing interests reported. Cite Share Download PDF Status: Published Journal Publication published 26 Dec, 2025 Read the published version in Journal of Applied Electrochemistry → Version 1 posted Editorial decision: Revision requested 19 Sep, 2025 Reviews received at journal 13 Sep, 2025 Reviews received at journal 01 Sep, 2025 Reviewers agreed at journal 29 Aug, 2025 Reviewers agreed at journal 29 Aug, 2025 Reviewers invited by journal 29 Aug, 2025 Editor assigned by journal 12 Jul, 2025 Submission checks completed at journal 10 Jul, 2025 First submitted to journal 09 Jul, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-7083420","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":509453898,"identity":"c0fe69b2-4eca-44ff-a43f-8ae2a773ba72","order_by":0,"name":"Waleed Jan","email":"data:image/png;base64,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","orcid":"","institution":"University of Engineering \u0026 Technology","correspondingAuthor":true,"prefix":"","firstName":"Waleed","middleName":"","lastName":"Jan","suffix":""},{"id":509453899,"identity":"52b24ca9-94c0-4a42-8708-eb4d3d8c9f18","order_by":1,"name":"Adnan Daud Khan","email":"","orcid":"","institution":"University of Engineering \u0026 Technology","correspondingAuthor":false,"prefix":"","firstName":"Adnan","middleName":"Daud","lastName":"Khan","suffix":""},{"id":509453900,"identity":"1ec856a8-1608-46c9-8cf5-be2f15e25b44","order_by":2,"name":"Faiza Jan Iftikhar","email":"","orcid":"","institution":"National University of Technology (NUTECH)","correspondingAuthor":false,"prefix":"","firstName":"Faiza","middleName":"Jan","lastName":"Iftikhar","suffix":""}],"badges":[],"createdAt":"2025-07-09 11:38:16","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-7083420/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-7083420/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s10800-025-02423-w","type":"published","date":"2025-12-26T15:57:14+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":90711787,"identity":"dde879e0-7c85-4cf6-bcb6-223c68037391","added_by":"auto","created_at":"2025-09-06 07:09:55","extension":"jpeg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":491644,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eFirst discharge voltage profiles at 0.5 C for LiSBs with various carbon cathodes and sulfur loading\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"floatimage1.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-7083420/v1/d2a73362ee5ac6b406b87f75.jpeg"},{"id":90711905,"identity":"0aa37a61-5546-4bf4-9fbb-5e1198f61925","added_by":"auto","created_at":"2025-09-06 07:17:55","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":328308,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eCapacity retention and coulombic efficiency of CMK-3, CMK-5, and CMK-8 carbon cathodes with varying sulfur loadings: CMK-3 (0.6 mg/cm²), CMK-5 (0.7 mg/cm²), and CMK-8 (0.6 mg/cm²)\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-7083420/v1/eab8fa7051233d4720af8962.png"},{"id":90711789,"identity":"21c2dc29-2dd8-4124-b8cc-a8fc813a1f8c","added_by":"auto","created_at":"2025-09-06 07:09:55","extension":"jpeg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":431026,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eComparison of discharge profiles for various carbon cathodes featuring different levels of sulfur loading at the 1\u003c/strong\u003e\u003csup\u003e\u003cstrong\u003est\u003c/strong\u003e\u003c/sup\u003e\u003cstrong\u003e, 10\u003c/strong\u003e\u003csup\u003e\u003cstrong\u003eth\u003c/strong\u003e\u003c/sup\u003e\u003cstrong\u003e, and 100\u003c/strong\u003e\u003csup\u003e\u003cstrong\u003eth\u003c/strong\u003e\u003c/sup\u003e\u003cstrong\u003e cycles\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"floatimage3.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-7083420/v1/d0b0397208d3ce6d7637c824.jpeg"},{"id":90711256,"identity":"3a211eda-a550-4e1f-a7b6-614a2ba8bb21","added_by":"auto","created_at":"2025-09-06 07:01:55","extension":"jpeg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":419845,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eImpact of carbon type and sulfur loading on 1) peak capacity, 2) 50th-cycle capacity, and 3) voltage at 50% DOD\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"floatimage4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-7083420/v1/9863de86d0f9e586eae90c05.jpeg"},{"id":90711906,"identity":"65edccc3-9fc9-4f0a-8fa0-3c4515dc4d0a","added_by":"auto","created_at":"2025-09-06 07:17:55","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":201360,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003eSystem-level model projections (for 1) Wh/kg and 2) Wh/L) of the LiSB at different sulfur loading using various carbon electrodes\u003c/strong\u003e\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-7083420/v1/5947e691a48e949944e68b07.png"},{"id":99172314,"identity":"5cd2dd1d-0c00-4a49-bc0b-578c8a1c08b4","added_by":"auto","created_at":"2025-12-29 16:07:42","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2593486,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7083420/v1/a60915c9-3e9e-4ead-ba90-70d464d19d5d.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Impact of Mesoporous Carbon Structure on Sulfur Utilization and Electrochemical Performance in Lithium-Sulfur Batteries","fulltext":[{"header":"1. INTRODUCTION","content":"\u003cp\u003eThere has been considerable interest in developing rechargeable batteries other than lithium-ion (Li-ion) over the last couple of decades in search of higher energy density [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]. In comparison to the widely used Li-ion batteries (LIBs), the lithium-sulfur battery (LiSB) has shown great promise due to its higher theoretical specific energy and capacity [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. Due to the abundant availability of sulfur, utilizing it as an active material in LiSBs will result in reduced costs [\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. Despite many efforts and notable breakthroughs, LiSBs still face challenges, namely inadequate system-level energy densities, performance challenges, and high operation costs, preventing their commercialization. Polysulfide shuttle mechanism, sulfur insulating properties, and inefficient cathode designs all contribute to these problems [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eResearchers are optimizing sulfur loading, electrolyte-to-sulfur ratio, and addressing the polysulfide shuttling effect to enhance LiSB performance. Materials like MnO\u003csub\u003e2\u003c/sub\u003e and V\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e have shown strong polysulfide adsorption, improving efficiency. Innovations such as single-atom catalysts and encapsulating polysulfide electrolytes aim to mitigate the shuttle effect and extend battery lifespan. Efforts also focus on predicting performance, developing commercial parameters, and introducing novel materials to advance LiSB technology [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eFor LiSBs to achieve high performance, efficient cathode design is an essential approach [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]. Researchers have recently undertaken comprehensive modeling and definition of critical parameters, specifically the electrolyte/sulfur (E/S) and carbon/sulfur (C/S) ratios, for optimizing LiSBs [\u003cspan additionalcitationids=\"CR8 CR9\" citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. A vital factor in the cathode design is the sulfur loading, which determines LiSB performance greatly; high sulfur loading will enhance the energy density of LiSBs [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. To attain a high discharge capacity and expanded cycle life, LiSBs should have high E/S ratios and low Sulfur loading (average literature studies show Sulfur loading of up to 2 mg/cm\u003csup\u003e2\u003c/sup\u003e and E/S ratios of 36 mL/g) [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. However, LiSBs have low energy densities because of the excessive electrolyte concentration and inadequate active material loading in the cathode, making them practically unusable in the global market [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. Based on the discovered results, Eroglu and colleagues proposed that LiSBs should have a sulfur loading exceeding 7 mg/cm\u003csup\u003e2\u003c/sup\u003e for a consistently high energy density across the battery [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. Moreover, Chung and colleagues put forward the claim that LiSBs targeted for high energy density must have a sulfur loading exceeding 6 mg/cm\u0026sup2; [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]. Despite a few recent experiments, high sulfur loading investigations are limited, owing mostly to the challenge of creating thick and mechanically robust cathodes. In a study conducted by Cheon et al., cathode thickness was found to impact the LiSB performance. A thick Li\u003csub\u003e2\u003c/sub\u003eS layer causes a high diffusional resistance, which results in a decrease in sulfur utilization as the cathode thickness increases [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eThe choice of carbon material in the cathode plays a pivotal role in determining electronic conductivity, sulfur retention, and polysulfide suppression. Mesoporous carbon structures with high surface area and tailored pore sizes have been widely explored to mitigate the adverse effects of polysulfide shuttling and sulfur\u0026rsquo;s insulating nature. CMK-3, CMK-5, and CMK-8, a family of ordered mesoporous carbons, offer large pore volumes, interconnected structures, and tunable surface areas, making them promising sulfur hosts. Among these, CMK-8 demonstrates superior polysulfide retention due to its larger pore size and interconnected pore network, which supports higher sulfur utilization and enhanced cycle stability. The incorporation of mesoporous carbons into the cathode matrix enhances electrochemical stability and energy efficiency. Recent studies have examined the impact of different surface areas and pore structures in activated carbon materials [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. For instance, Xiang et al. stated in their investigation that a specific pore volume and carbon particle size are critical for achieving large sulfur loading and sulfur utilization [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. According to Barchasz et al., the amount of polysulfide deposited on the cathode at discharge was regulated by the size of the carbon grain. Furthermore, large electrode surface areas prevent full electrode passivation, improving battery discharge performance [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. In the literature, various surface areas and pore diameters of activated carbon have been examined [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. A large surface area and tiny pores are required to attain high sulfur use and discharge capacity [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eYu et al. introduced Nitrogen-functionalized porous carbon/CNT hybrid nanowires as a bifunctional interlayer for high-performance LiSBs, enhancing polysulfide trapping, adsorption, and conversion. The coating enables the deposition of lithium polysulfide, which inhibits the shuttle effect, while the CNT backbone ensures a conductive network for electron/ion transport. The nitrogen-doped surface captures lithium polysulfides, promoting conversion and lithium sulfide growth, improving battery performance. After 700 cycles at 0.5 C, the CNTNC-10 interlayer maintains a high initial capacity of 1395.4 mAh/g with a low decay rate of 0.025, demonstrating excellent stability. It also shows outstanding rate performance, delivering 765.9 mAh/g at 2000 mA/g, highlighting its potential for enhancing LiSBs [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eLiSBs could benefit from an improved cathode design by addressing mass and charge transport problems [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e, \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. Enhancing electrochemical performance can be achieved through the utilization of hollow carbon microspheres doped with nitrogen and embedded with cobalt within a cathode composed of carbon and sulfur, which provides a substantial area for sulfur loading [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. A distinct study proposes an inventive cathode design to mitigate the shuttle effect of polysulfides. This design entails encapsulating a hollow carbon skeleton with an interconnected spacing [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. High porosity carbon nanofiber cathodes not only provide high sulfur utilization but also allow electrolyte permeability [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. Liu et al. demonstrated that high efficiency and cyclic stability in LiSBs were achieved using Co\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e nanocages encased in microcapsules with metal-organic frameworks (MOFs) [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eThere has been a lot of research on how different types of carbon affect LiSB\u0026rsquo;s electrochemical characteristics, but little is known about how different carbon features affect battery performance at the cell or system level. The impacts of the type of carbon and the amount of sulfur on the electrochemical properties of the LiSB at the cell and system levels were investigated in this work using experimental methodologies. This study systematically investigates the effects of CMK-3, CMK-5, and CMK-8 as cathode materials in LiSBs, focusing on their structural properties, sulfur retention capabilities, and electrochemical performance. By analyzing the relationship between surface area, pore volume, particle size, and sulfur loading, we provide a comprehensive understanding of how mesoporous carbon influences capacity retention, cycle stability, and rate performance. These insights contribute to the development of optimized cathode architectures that enhance LiSB efficiency, paving the way for higher energy densities and longer cycle life in next-generation battery systems.\u003c/p\u003e"},{"header":"2. RESULTS AND ANALYSIS","content":"\u003cp\u003eFigure \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e shows the voltage curves for LiS cells with different sulfur loading and mesoporous carbon cathodes.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe discharge profiles in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e illustrate the electrochemical response of LiSBs employing CMK-3, CMK-5, and CMK-8 as host materials, each evaluated at varying sulfur loadings. A clear trend emerges across all samples: lower sulfur loadings (in the range of 1.3\u0026ndash;1.8 mg/cm\u0026sup2;) consistently yield higher initial discharge capacities, whereas increasing the sulfur content results in diminished capacity. This decline is attributed to limitations in Li-ion accessibility and ineffective electrochemical conversion processes at elevated sulfur levels [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]. Excessive sulfur accumulation within the porous matrix likely impedes full electrochemical participation due to pore clogging, leading to polysulfide buildup at the carbon interface, where further reduction forms insoluble species such as Li₂S₂ and Li₂S that block active sites [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e]. Among the three hosts, CMK-3 demonstrates relatively stable discharge behavior even at higher loadings (up to 3.1 mg/cm\u0026sup2;), maintaining a well-defined two-plateau profile characteristic of sulfur redox reactions. This implies that its highly ordered mesoporous architecture promotes uniform sulfur distribution, effective polysulfide confinement, and sufficient ion transport pathways, thereby mitigating the impact of cathode thickening. In contrast, CMK-5 exhibits less defined plateaus and steeper voltage decay, especially as loading increases, indicating increased polarization and mass transport limitations. The less favorable performance suggests suboptimal pore connectivity and reduced electrolyte accessibility, which hinders both redox kinetics and sulfur utilization under higher load conditions. CMK-8, while capable of delivering extended discharge capacity at lower loading, shows partial suppression of the low-voltage plateau with increased sulfur content. This indicates hindered conversion of intermediate polysulfides to Li₂S, which is crucial for maximizing energy output. The observed decline is likely exacerbated by insufficient electrolyte infiltration in thicker electrodes, a well-documented challenge in high-loading LiSBs the due to the low wettability of sulfur and carbon materials with organic electrolytes [\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e]. As the cathode thickens, inadequate wetting and poor ionic conductivity exacerbate polarization, leading to capacity fade and an increased voltage drop. Furthermore, diminished electronic conductivity across thicker electrodes may also contribute to the loss of plateau clarity and overall electrochemical inefficiency.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e presents the electrochemical performance of the CMK-3, CMK-5, and CMK-8 cathodes under moderate sulfur loadings, focusing on capacity retention and coulombic efficiency. Among them, CMK-8 demonstrates the most stable behavior, characterized by a relatively flat capacity curve and narrow error bars. This suggests efficient sulfur confinement and consistent ion transport, likely facilitated by its favorable pore architecture. CMK-3 shows intermediate performance, with a gradual capacity decline over cycles that may be attributed to limited pore accessibility or weaker interaction with sulfur species, despite having a similar sulfur loading to CMK-8. In contrast, CMK-5 performs the worst, exhibiting a sharp capacity drop and unstable coulombic efficiency. Its poor performance is likely due to inadequate sulfur utilization and significant polysulfide loss, aggravated by suboptimal pore connectivity and insufficient electronic pathways. Notably, the prominent fluctuations observed in the retention curves of CMK-5, and to a lesser extent, CMK-3, indicate unstable redox kinetics and uneven sulfur reactivation during cycling. These variations may result from transient pore blockages by Li₂S/Li₂S₂, inconsistent electrolyte penetration, or inhomogeneous sulfur distribution. For CMK-5 in particular, the combination of higher sulfur content and poorly interconnected mesopores likely contributes to localized concentration gradients and increased polarization, leading to erratic capacity behavior.\u003c/p\u003e\u003cp\u003eInterestingly, CMK-8 exhibits a slight increase in capacity during the initial 60 cycles, which can be attributed to an electrochemical activation phase. This involves improved wetting of the porous matrix, redistribution of active sulfur species, and more effective polysulfide confinement. However, beyond this activation period, a gradual decline is observed, likely due to electrode degradation, pore clogging by insulating discharge products, and reduced electronic connectivity within the thickened cathode. These factors collectively diminish sulfur utilization and increase internal resistance, contributing to long-term capacity fading.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe galvanostatic discharge profiles of CMK-3, CMK-5, and CMK-8 cathodes, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e, illustrate clear distinctions in their electrochemical response and capacity retention over extended cycling. In the initial stages, all three materials exhibit the characteristic two-step discharge process of LiSBs, reflecting the sequential reduction of elemental sulfur (S₈) to soluble long-chain polysulfides (~\u0026thinsp;2.3\u0026ndash;2.1 V), followed by conversion to insoluble short-chain species and Li₂S (~\u0026thinsp;2.1\u0026ndash;1.7 V). However, the stability and clarity of these features evolve differently depending on the carbon matrix. CMK-3 displays prominent discharge plateaus in the first cycle, suggesting effective sulfur activation and relatively uniform reaction kinetics. Yet, by the 100th cycle, the high-voltage plateau is largely diminished and overall capacity declines from approximately 800 mAh/g to below 500 mAh/g. This fading behavior, coupled with increasing voltage hysteresis, signals a gradual loss of active material and growing internal resistance, likely due to incomplete polysulfide retention and electrode degradation. CMK-5, despite its initially high capacity (~\u0026thinsp;850 mAh/g), shows rapid deterioration. The plateaus are poorly defined from the outset, and the profiles become increasingly sloped and indistinct with cycling. By the 100th cycle, the discharge curve is nearly featureless, and capacity drops significantly. Such behavior points to ineffective sulfur confinement and hindered redox activity, likely resulting from an unsuitable pore structure or inhomogeneous sulfur distribution, exacerbated by the higher loading. In comparison, CMK-8 maintains better structural and electrochemical stability. Its discharge curves remain more consistent through the 10th cycle, and even by the 100th, the lower-voltage plateau remains discernible. Although capacity decreases from ~\u0026thinsp;750 mAh/g to ~\u0026thinsp;500 mAh/g, the slower rate of decay and retention of plateau features suggest improved redox reversibility and stronger resistance to degradation. The moderate increase in hysteresis further supports the conclusion that CMK-8 provides a more efficient framework for polysulfide management.\u003c/p\u003e\u003cp\u003eOverall, these results emphasize that the mesostructure of the carbon host plays a more critical role than sulfur loading in determining long-term battery performance. CMK-5, with the highest sulfur content, fails to deliver sustained capacity due to poor structural compatibility, whereas CMK-8 achieves better cycling outcomes despite similar loading to CMK-3. The progressive loss of discharge features and increase in polarization across all samples highlight the ongoing challenge of stabilizing polysulfide species in LiSBs.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e compares the electrochemical performance of LiSBs with varying sulfur loadings using three mesoporous carbon hosts: CMK-3, CMK-5, and CMK-8. The first plot illustrates peak discharge capacities, which initially increase with sulfur loading, reaching a maximum near 2.0 mg/cm\u0026sup2;, followed by a sharp decline at higher loadings. This behavior reflects the trade-off between increased active material and the onset of transport limitations, including reduced electronic pathways, hindered electrolyte penetration, and enhanced polarization. Among the materials, CMK-8 achieves the highest initial capacity (~\u0026thinsp;900 mAh/g), attributed to its large pore volume and interconnected 3D framework that promotes efficient redox reactions. However, this advantage rapidly diminishes at higher loadings due to non-uniform sulfur deposition and mechanical rigidity, which compromise structural integrity and ion transport. CMK-3, with its linear mesoporous structure, displays more moderate but stable performance across the tested range. While its peak capacity is lower, it demonstrates greater tolerance to increased sulfur content, likely due to better mechanical robustness and more uniform sulfur distribution. CMK-5, in contrast, exhibits limited performance overall but uniquely peaks at ~\u0026thinsp;2.3 mg/cm\u0026sup2; in the 50th -cycle data (Plot 2), suggesting it may momentarily facilitate high utilization at specific loadings. Nevertheless, its steep capacity fade beyond this point points to poor long-term stability and inefficient charge transport. The third plot reveals a consistent decline in average discharge voltage with increasing sulfur loading for all cathodes. This reduction is indicative of higher overpotentials, decreased reaction kinetics, and elevated internal resistance under thicker electrode configurations. CMK-8 again shows the most favorable voltage profile, consistent with its lower polarization and faster charge transfer, while CMK-5 suffers from the greatest voltage suppression, confirming its poor conductivity and limited electrochemical reversibility. Collectively, these results highlight the delicate balance required between structural accessibility, mechanical resilience, and sulfur distribution. Optimizing pore architecture is critical for maximizing capacity while preserving cycling stability in mesoporous carbon-based sulfur cathodes.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e presents system-level modeling results for LiSBs incorporating CMK-3, CMK-5, and CMK-8 carbon hosts, showing projected trends in specific energy (Wh/kg, Plot 1) and energy density (Wh/L, Plot 2) as a function of sulfur loading. These projections incorporate electrode-level electrochemical data and account for inactive material contributions, making them highly relevant for practical cell design. In Plot 1, specific energy improves with increasing sulfur content up to approximately 2.0 mg/cm\u0026sup2; across all carbon types. This initial rise reflects enhanced active material utilization and a favorable balance between energy output and structural support. Beyond this point, however, the trends begin to diverge sharply. CMK-8 exhibits a continued upward trajectory in specific energy, reaching values above 90 Wh/kg at higher loadings. This suggests not only excellent electrochemical performance at the material level but also a structural framework capable of accommodating thick electrodes without substantial loss of efficiency. Its 3D pore connectivity likely ensures sustained electronic and ionic transport even as sulfur content increases. CMK-3 demonstrates more conservative gains, with specific energy plateauing near 75 Wh/kg. Although this material lacks the steep drop-off observed in CMK-5, its relatively flatter curve at higher loadings implies diminishing returns as thickness increases\u0026mdash;likely due to diffusion limitations and moderate conductivity that constrain further performance improvement. This makes CMK-3 more stable but less scalable for high-energy applications. CMK-5 presents a markedly different profile, characterized by a sharp peak near 1.6 mg/cm\u0026sup2; followed by a steep decline. This behavior highlights a critical performance bottleneck in mass transport or charge transfer beyond optimal sulfur content. The collapse in specific energy at higher loadings suggests that CMK-5\u0026rsquo;s pore architecture cannot sustain efficient electrochemical reactions once the electrode becomes too thick or poorly infiltrated with electrolyte. In this context, system-level modeling reveals that even a material capable of high areal capacity under ideal lab-scale conditions may fail to deliver in realistic configurations if it lacks sufficient structural and transport resilience. Plot 2 reinforces these observations in terms of volumetric performance. CMK-8 achieves the highest energy density (~\u0026thinsp;120 Wh/L), peaking around 2.0 mg/cm\u0026sup2; before experiencing a modest decline and then recovering at higher sulfur levels. This non-monotonic behavior likely reflects the interplay between improved packing density and increasing internal resistance. The ability to rebound in performance at higher loadings further underscores CMK-8\u0026rsquo;s mechanical integrity and efficient pore utilization. CMK-3, while lagging behind in absolute performance, maintains a relatively flat curve beyond 2 mg/cm\u0026sup2;, indicative of predictable and stable volumetric output, albeit with limited room for optimization. In contrast, CMK-5 again suffers a dramatic collapse after its peak, emphasizing its unsuitability for thick-electrode formats where electrolyte access and sulfur retention are critical. Taken together, these projections reveal the decisive impact of host structure on energy delivery at the system level. While CMK-5 may appear competitive at moderate sulfur loadings, its rapid degradation under practical constraints negates that advantage. CMK-3 offers dependable, if unspectacular, performance, suitable for applications prioritizing stability. CMK-8 stands out as the most promising candidate, combining scalability with high energy yields, both gravimetric and volumetric, due to its synergistic structural and conductive properties. These findings underscore the necessity of integrating system-level modeling early in the materials development pipeline to identify architectures that retain electrochemical advantages under real-world constraints. For LiSBs targeting commercial viability, such predictive assessments are essential in bridging the gap between lab-scale results and practical energy storage solutions.\u003c/p\u003e"},{"header":"3. EXPERIMENTAL METHODOLOGY","content":"\u003cp\u003eVarious mesoporous carbon materials were mixed with sulfur (purchased from Sigma Aldrich) and a binder (polyvinylidene fluoride, PVDF, obtained from MTI) using a mortar and pestle for 15 minutes. The carbon sources utilized in this study were CMK-3, CMK-5, and CMK-8, selected for their high surface area, tunable pore structures, and enhanced sulfur retention capabilities. The main properties of the mesoporous carbon materials that were examined are comprehensively outlined in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e.\u003c/p\u003e\u003cp\u003e\u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e\u003ccaption language=\"En\"\u003e\u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e\u003cdiv class=\"CaptionContent\"\u003e\u003cp\u003eEssential Characteristics of the Investigated Carbon Materials\u003c/p\u003e\u003c/div\u003e\u003c/caption\u003e\u003ccolgroup cols=\"9\"\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e\u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e\u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c8\" colnum=\"8\"\u003e\u003c/div\u003e\u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c9\" colnum=\"9\"\u003e\u003c/div\u003e\u003cthead\u003e\u003ctr\u003e\u003cth align=\"left\" colname=\"c1\"\u003e\u003cp\u003eName\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c2\"\u003e\u003cp\u003eTotal pore Volume (cm\u0026sup3;/g)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c3\"\u003e\u003cp\u003ePore Diameter (nm)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c4\"\u003e\u003cp\u003eMicropore Volume (cm\u0026sup3;/g)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c5\"\u003e\u003cp\u003eMicropore surface area (m\u003csup\u003e2\u003c/sup\u003e/g)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c6\"\u003e\u003cp\u003eBET Surface area (m\u003csup\u003e2\u003c/sup\u003e/g)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c7\"\u003e\u003cp\u003eParticle\u0026rsquo;s Size (nm)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c8\"\u003e\u003cp\u003eElectrical Conductivity (S/cm)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c9\"\u003e\u003cp\u003eTap density (g/cm\u003csup\u003e3\u003c/sup\u003e)\u003c/p\u003e\u003c/th\u003e\u003c/tr\u003e\u003c/thead\u003e\u003ctbody\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003eCMK-3\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e\u003cp\u003e1.2\u0026ndash;1.5\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003e3\u0026ndash;5\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e\u003cp\u003e0.05\u0026ndash;0.15\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e100\u0026ndash;300\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e1000\u0026ndash;1500\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e30\u0026ndash;50\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c8\"\u003e\u003cp\u003e20\u0026ndash;60\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e\u003cp\u003e0.3\u0026ndash;0.5\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003eCMK-5\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e\u003cp\u003e1.3\u0026ndash;1.7\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003e4\u0026ndash;6\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e\u003cp\u003e0.05\u0026ndash;0.20\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e150\u0026ndash;350\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e1100\u0026ndash;1500\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e50\u0026ndash;80\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c8\"\u003e\u003cp\u003e15\u0026ndash;50\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e\u003cp\u003e0.3\u0026ndash;0.5\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003eCMK-8\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e\u003cp\u003e1.0\u0026ndash;1.4\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c3\"\u003e\u003cp\u003e5\u0026ndash;7\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e\u003cp\u003e0.10\u0026ndash;0.25\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e200\u0026ndash;400\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e800\u0026ndash;1200\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003e100\u0026ndash;150\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c8\"\u003e\u003cp\u003e10\u0026ndash;40\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\".\" colname=\"c9\"\u003e\u003cp\u003e0.25\u0026ndash;0.45\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003c/tbody\u003e\u003c/colgroup\u003e\u003c/table\u003e\u003c/div\u003e\u003c/p\u003e\u003cp\u003eA 20/70/10 weight percentage was adjusted for carbon/sulfur/binder. The solid mixture was dissolved using N-methyl-2-pyrrolidone (NMP, obtained from MTI) solvent until a homogeneous slurry was achieved. Afterwards, a magnetic stirrer was used to mix the slurry overnight at room temperature before mixing it again at 60\u0026deg;C for two hours. In the end, the slurry went through a three-hour ultrasonic treatment. As soon as the slurry had been homogenized, it was cast using the doctor blade technique (15 mm thick, procured from MTI) onto an aluminum current collector. During casting, the slurry's thickness was adjusted to control the cathode's Sulfur loading between 0.6 and 3.1 mg/cm\u003csup\u003e2\u003c/sup\u003e (calculated as 300, 550, 700, or 800 \u0026micro;m). After drying overnight at 60\u0026deg;C in the oven, the electrodes were annealed for four hours at 60\u0026deg;C. As discussed in the previous section, LiSBs perform better when sulfur is encapsulated in nanocarbon structures. Since we wanted to look into sulfur loading and carbon characteristics in a way that was easy to understand, we conducted this study using the most popular traditional cathode manufacturing method. This study employed the fabrication of two-electrode CR2032 coin cells within an Ar-filled glove box (Siemens, O\u003csub\u003e2\u003c/sub\u003e and H\u003csub\u003e2\u003c/sub\u003eO concentrations\u0026thinsp;\u0026lt;\u0026thinsp;0.5 ppm). The Celgard polymeric separator (with an area of 3.02 cm\u003csup\u003e2\u003c/sup\u003e and a thickness of 25 mm, obtained from MTI) was utilized as the separator, and the anode consisted of a lithium metal foil (with an area of 2.01 cm\u003csup\u003e2\u003c/sup\u003e and a thickness of 160 mm, obtained from MTI). To prepare the liquid electrolyte for the cells, a 0.1M solution of lithium nitrate (LiNO\u003csub\u003e3\u003c/sub\u003e) (purchased from Sigma Aldrich) was combined with a 1M solution of lithium BIS(trifluoromethanesulfonyl)imide (LiTFSI) (obtained from Sigma Aldrich). The electrolyte was dissolved in a blend of 1,3-dioxolane (DOL, procured from Sigma Aldrich) and 1,2-dimethoxyethane (DME, procured from Sigma Aldrich) at a volume ratio of 1:1. Following this, the electrolyte amount in each cell sample was modified to attain the desired E/S ratio of 12 \u0026micro;Lm/g, a critical parameter for optimizing capacity retention rates. The Neware galvanostatic battery cycler was utilized to assess cell performance at room temperature by applying a current rate of 0.5 C, considering LiSB's theoretical capacity of 1675 mAh/g.\u003c/p\u003e"},{"header":"4. CONCLUSION","content":"\u003cp\u003eThis study systematically evaluated the electrochemical consequences of employing different mesoporous carbon architectures, specifically CMK-3, CMK-5, and CMK-8, as cathode hosts in LiSBs, while also varying the active material loading. The findings conclusively demonstrate that the specific structural attributes of the carbon host profoundly dictate battery behavior, influencing sulfur utilization, polysulfide management, and long-term stability. CMK-8 emerged as the superior performer among the tested materials, exhibiting enhanced capacity retention and greater stability over prolonged cycling, particularly when accommodating higher sulfur levels (up to its studied limits). This advantage is attributed to its larger pore dimensions (5\u0026ndash;7 nm) and well-interconnected three-dimensional network, which appear crucial for physically confining soluble polysulfide intermediates, mitigating their detrimental shuttle effect, and facilitating sustained ion and electron transport even within the thicker electrode structures necessitated by higher loadings. In contrast, CMK-5, despite possessing a comparable theoretical surface area and pore volume to CMK-3, displayed rapid performance degradation and poor coulombic efficiency, especially as sulfur content increased. This suggests its specific pore architecture (4\u0026ndash;6 nm, potentially less interconnected or with different tortuosity) is less adept at effectively trapping soluble intermediates or maintaining conductive pathways under operational stress, leading to significant polarization, active material loss, and overall electrochemical inefficiency. CMK-3, with its ordered linear mesopores (3\u0026ndash;5 nm), presented intermediate results, offering reasonable initial stability but ultimately showing limitations in maintaining high performance at elevated sulfur loadings compared to CMK-8, likely due to constraints in ion diffusion pathways or less effective volume accommodation for sulfur species.\u003c/p\u003e\u003cp\u003eCrucially, the study reinforced that merely increasing sulfur loading is not a universally beneficial strategy. An optimal loading threshold, generally observed around 2.0 mg/cm\u0026sup2; in these systems, provided the best balance between capacity and stability. Beyond this point, all systems suffered from diminished specific capacity, increased voltage hysteresis, and faster fading. This decline stems from aggravated mass transport limitations, incomplete active material utilization due to pore clogging or poor electrolyte penetration deep within the thicker cathode, and amplified polarization effects. System-level energy density projections further substantiated these experimental observations, highlighting CMK-8's potential for achieving higher practical gravimetric (Wh/kg) and volumetric (Wh/L) energy densities due to its ability to better sustain performance at higher, more application-relevant loadings. Therefore, this research underscores that advancing LiSBs necessitates a sophisticated approach to cathode design, focusing critically on tailoring the carbon host's architecture, balancing pore volume, size distribution, connectivity, and mechanical stability, to effectively manage the complex sulfur redox chemistry and achieve durable, high-energy storage.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003ch2\u003eConflicts of Interest:\u003c/h2\u003e\u003cp\u003eThe authors declare no conflict of interest.\u003c/p\u003e\u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eW.J.: Writing \u0026ndash;original draft, Investigation, Methodology; A.D.K.: Supervision, conceptualization, resources, project administration; F.J.I.: Validation, formal analysis, visualization, writing \u0026ndash; review \u0026amp; editing\u003c/p\u003e\u003ch2\u003eAcknowledgments\u003c/h2\u003e\u003cp\u003eWe acknowledge the support of U.S-Pakistan Center for Advanced Studies in Energy, University of Engineering \u0026amp; Technology, Peshawar.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eChen Y, Wang T, Tian H, Su D, Zhang Q, Wang G (2021) Advances in lithium\u0026ndash;sulfur batteries: from academic research to commercial viability. 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J Electrochem Soc 166(8):A1490\u003c/span\u003e\u003c/li\u003e\u003cli\u003e\u003cspan\u003eMichaelis C, Erisen N, Eroglu D, Koenig GM Jr (2019) Electrochemical performance and modeling of lithium-sulfur batteries with varying carbon to sulfur ratios. Int J Energy Res 43(2):874\u0026ndash;883\u003c/span\u003e\u003c/li\u003e\u003cli\u003e\u003cspan\u003eChen R, Zhou Y, Li X (2024) Nanocarbon-enabled mitigation of sulfur expansion in lithium\u0026ndash;sulfur batteries. Energy Storage Mater 68:103353\u003c/span\u003e\u003c/li\u003e\u003cli\u003e\u003cspan\u003eRao F, Xiao Q, Wei Y, Wang J, Yu R, Wang D (2024) Balanced Polysulfide Containment and Lithium Ion Transport in Lithium-Sulfur Batteries via Nitrogen-doped Carbon Hollow Multi-shelled Structures on Modified Separators. 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Nano Res 14:131\u0026ndash;138\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"journal-of-applied-electrochemistry","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jach","sideBox":"Learn more about [Journal of Applied Electrochemistry](http://link.springer.com/journal/10800)","snPcode":"10800","submissionUrl":"https://submission.nature.com/new-submission/10800/3","title":"Journal of Applied Electrochemistry","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"sulfur, carbon, cathode, sulfur loading, energy density","lastPublishedDoi":"10.21203/rs.3.rs-7083420/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7083420/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eLithium-sulfur batteries (LiSBs) have emerged as a promising alternative for next-generation high-energy-density storage systems due to their exceptional theoretical specific capacity (1675 mAh/g) and high energy density (2600 Wh/kg). However, achieving practical performance remains challenging due to issues such as poor sulfur utilization, polysulfide shuttling, and limited cycle stability. The structural and compositional properties of mesoporous carbon materials in the cathode, particularly CMK-3, CMK-5, and CMK-8, play a crucial role in overcoming these limitations. These materials influence electrical conductivity, sulfur retention, and electrochemical stability, making their selection and optimization vital for improving LiSB efficiency. This study systematically investigates the interplay between sulfur loading, energy density, discharge capacity, and carbon structure at the cell level using experimental characterization. Results indicate that CMK-8 offers the most favorable performance, combining high sulfur loading capacity with strong polysulfide retention and enhanced cycling stability due to its large pore volume and interconnected structure. CMK-3 displays moderate electrochemical stability, particularly at lower sulfur loadings, but suffers from performance decline under high loading conditions. In contrast, CMK-5 exhibits the weakest electrochemical performance, with significant capacity fading and poor coulombic efficiency, indicating that its pore architecture is less suitable for effective sulfur confinement and long-term cycling. The findings reveal that moderate sulfur loading, rather than excessive sulfur incorporation, yields the best balance between high discharge capacities, capacity retention, and long-term cycling performance. By optimizing carbon pore structures, sulfur distribution, and cathode architecture, this research offers valuable insights into the design of high-performance LiSBs. The results contribute to the development of next-generation LiSBs with enhanced energy densities, paving the way for their practical deployment in energy storage applications, electric vehicles, and portable electronics.\u003c/p\u003e","manuscriptTitle":"Impact of Mesoporous Carbon Structure on Sulfur Utilization and Electrochemical Performance in Lithium-Sulfur Batteries","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-09-06 07:01:50","doi":"10.21203/rs.3.rs-7083420/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-09-19T09:42:34+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-09-13T14:44:39+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-09-01T11:25:07+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"210405436370472660373496761841492282484","date":"2025-08-29T08:33:18+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"151129650441360662986517016249835651777","date":"2025-08-29T06:06:05+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-08-29T05:59:35+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-07-12T15:45:11+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-07-10T08:53:06+00:00","index":"","fulltext":""},{"type":"submitted","content":"Journal of Applied Electrochemistry","date":"2025-07-09T11:26:25+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"journal-of-applied-electrochemistry","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jach","sideBox":"Learn more about [Journal of Applied Electrochemistry](http://link.springer.com/journal/10800)","snPcode":"10800","submissionUrl":"https://submission.nature.com/new-submission/10800/3","title":"Journal of Applied Electrochemistry","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"0f206df5-80cb-4ee7-b292-45cca319160a","owner":[],"postedDate":"September 6th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2025-12-29T16:01:27+00:00","versionOfRecord":{"articleIdentity":"rs-7083420","link":"https://doi.org/10.1007/s10800-025-02423-w","journal":{"identity":"journal-of-applied-electrochemistry","isVorOnly":false,"title":"Journal of Applied Electrochemistry"},"publishedOn":"2025-12-26 15:57:14","publishedOnDateReadable":"December 26th, 2025"},"versionCreatedAt":"2025-09-06 07:01:50","video":"","vorDoi":"10.1007/s10800-025-02423-w","vorDoiUrl":"https://doi.org/10.1007/s10800-025-02423-w","workflowStages":[]},"version":"v1","identity":"rs-7083420","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7083420","identity":"rs-7083420","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}