Pt‐Rh/TiO2/activated carbon as highly active and stable HI decomposition catalyst for hydrogen production in sulfur‐iodine (SI) process

Pt‐TiO₂ loaded on activated carbon was studied as an active and stable catalyst to HI decomposition for H₂ formation in the sulfur‐iodine process. Although the activity of TiO₂‐loaded catalyst was slightly lower HI conversion than that of CeO₂ loaded one, the higher stability against HI decomposition reaction was achieved and almost equilibrium conversion was sustained over ~65 h examined. Moreover, effects of Rh or Ir addition on HI conversion were studied and it was found that Pt‐Rh bimetallic system was highly active and stable to HI decomposition. Scanning transmission electron micrograph observation suggested that the increased HI decomposition activity was assigned to the increased dispersion of Pt particles. High dispersion state of Pt was sustained after HI decomposition at 773 K by addition of Rh. Since the formation of PtI₄ was suggested by X‐ray photoelectron spectroscopy measurement during HI decomposition, increased stability by addition of Rh seems to be assigned to the high chemical stability of Rh against iodine. Almost the equilibrium HI conversion on Pt‐Rh‐TiO₂/M563 was sustained over 300 hours at 673 K.     

Pt/zirconia catalyst for hydrogen generation from HI decomposition reaction of S–I cycle

Hydrogen energy is considered as one of the ideal solutions for the fulfilment of the ever increasing energy demand. It is mainly due to the following two reasons: firstly, it can be produced from a very abundant source, that is, water; and secondly, it does not leave any harmful effect on the environment. Thermochemical cycles are amongst the most promising ways to generate hydrogen from water in an environment‐friendly manner. Sulfur–iodine cycle is one of the most efficient thermochemical cycles. In this paper, we discuss synthesis of Pt/zirconia catalysts for HI decomposition reaction, which is one of the important steps of S–I thermochemical cycle. The catalysts were characterized by X‐ray diffraction, scanning electron microscopy (SEM), field emission gun‐SEM, transmission electron microscopy, N₂ adsorption and H₂ chemisorption. The catalytic activity and stability of these catalysts, for liquid phase decomposition of hydriodic acid was evaluated. Conversion is found to be dependent on the noble metal loading, with 18.7% conversion for 2% Pt/ZrO₂ catalyst as compared with 2.7% of without catalyst, although the specific activity is highest for 0.5% Pt/ZrO₂ catalyst. The catalyst was found to be stable under liquid phase HI decomposition reaction conditions. Copyright © 2014 John Wiley & Sons, Ltd.     

Pt/graphite catalyst for hydrogen generation by HI decomposition reaction in S–I thermochemical cycle

Hydrogen is an attractive energy carrier for future because of various reasons. Therefore its large scale production is the need of the hour. One of the ways to achieve this is sulfur iodine thermochemical cycle and HI decomposition reaction is one of the three reactions constituting the cycle. Pt/graphite catalysts with different loading of platinum were prepared by impregnating colloidal graphite with hexachloroplatinic acid solution followed by reduction under N₂ flow. The catalysts prepared have been characterized by X‐ray diffraction, Raman, scanning electron microscopy, X‐ray photoelectron spectroscopy and Brunauer–Emmett–Teller surface area. These catalysts have been employed for liquid phase HI decomposition under different conditions. To evaluate the stability of this catalyst against noble metal leaching under the reaction conditions, the eluent was analyzed by using ICP‐OES. Platinum loaded catalysts (0.5%, 1% and 2%) show 8.4%, 17.5% and 23.4% conversion respectively. From the present study we conclude that Pt/graphite is a suitable and stable catalyst for liquid phase HI decomposition reaction. Copyright © 2015 John Wiley & Sons, Ltd.     

Sulfuric acid decomposition on the Pt/n-SiC catalyst for SI cycle to produce hydrogen

The sulfuric acid decomposition should be performed in the wide temperature ranges from 550 °C to 950 °C to absorb the sensible heat of He in SI process. Therefore, the catalysts for the reaction should be stable even in the very corrosive reaction condition of 650 °C. Here, the Pt/n-SiC catalyst was prepared for the purpose and compared with the Pt/SiC catalyst. The both catalysts showed the high stability in the temperature ranges from 650 to 850 °C. The n-SiC with the surface area of 187.1 m²/g was prepared using nano-sized SiO₂, which resulted in amorphous SiC phase. The SiC support with the surface area of 19.2 m²/g for the comparison showed the well crystalline structure. In spite of the large surface area differences between the n-SiC and SiC support, the Pt particle sizes of the Pt/n-SiC (average Pt size: 26.4 nm) catalyst were not so much different from those of the Pt/SiC (average Pt size: 26.1 nm) catalyst after the calcination at 1000 °C for 3 h. However, the catalytic activity of the Pt/n-SiC was much higher than that of the Pt/SiC. XRD analysis indicated that the Pt particles on the Pt/n-SiC was more stable than those of the Pt/SiC in the sulfuric acid decomposition and XPS analysis showed that the Pt valence state on the Pt/n-SiC was higher than that on the Pt/SiC. The surface analysis showed that the surface of the n-SiC particles was covered by SiO₂ and Si₄C_4−xO₄. These experimental results indicate that the Pt metal particles on n-SiC were stabilized on the oxidized Si surface. Therefore, it is suggested that the Pt particles stabilized on the oxidized Si surface can be a reason for the higher activity of the Pt/n-SiC catalyst as compared with the Pt/SiC catalyst.     

Supporting high-loading Ni on SBA-15 as highly active and durable catalyst for ammonia decomposition reaction

Although supported Ni is generally considered the most active non-noble metal catalyst for decomposing NH₃ to produce CO_x-free H₂, its activity is not sufficient. Herein, supporting high-loading Ni on SBA-15 is explored to alleviate the low intrinsic activity issue of Ni. SBA-15 supports with tunable textual properties are synthesized to support Ni catalyst for NH₃ decomposition. Characterization shows that Ni catalyst with a loading close to 40 wt% supported on SBA-15 with the largest specific surface area (Ni/SBA-15-80) exhibits a NH₃ decomposition performance much better than those reported on other Ni-based NH₃ decomposition catalysts, resulting from its favorable textural properties and high Ni loading. In addition, Ni/SBA-15-80 shows excellent catalytic stability, with no activity degradation over an 80-h NH₃ decomposition test. This work reveals the importance of textural properties of support and Ni loading to NH₃ decomposition performance and can provide a new idea for synthesizing high-performance NH₃ decomposition catalysts.     

Photocatalytic hydrogen production from glycerol–water mixture over Pt‐N‐TiO2 nanotube photocatalyst

The effects of several modifications on TiO₂ P25 in producing hydrogen from glycerol–water mixture have been investigated. Prior to further modification, TiO₂ underwent hydrothermal treatment at 130°C for several hours to obtain nanotube shape. TiO₂ nanotubes (TiNT) was then doped with platinum (Pt) and nitrogen (N) by employing photo‐deposition and impregnation method, respectively. SEM and XRD results showed that Pt‐N‐TiNT was successfully obtained as pure anatase crystal structure. The effects of glycerol content to photocatalytic activity of hydrogen production have also been studied, result in 50%v of glycerol as the optimum concentration correspond to the stoichiometric volume ratio of glycerol reforming. The results of photo‐production test showed that TiNT (nanotube) could enhance hydrogen generation by two times compared with unmodified P25 (nanoparticle). Meanwhile, simultaneous modification of TiNT by Pt and N dopants (Pt‐N‐TiNT) lead to activity improvement up to 13 times compared with P25. The output of this study may contribute toward finding an alternative pathway to produce H₂ from renewable resources. Copyright © 2012 John Wiley & Sons, Ltd.     

Detailed kinetic modeling of homogeneous HI decomposition for hydrogen production—Part II: Effect of I2 on HI decomposition

The kinetic modeling of homogeneous decomposition of hydrogen iodide (HI) and HI/H₂O vapors with the addition of diatomic iodine (I₂) using the mechanism proposed in the companion work (part I) in the sulfur–iodine cycle was investigated in this paper. Thermodynamic results calculated by FactSage and the kinetic experiment verified the applicability of the mechanism. The effect of temperature, residence time, pressure, HI/H₂O/I₂ molar ratio, HI/I₂ molar ratio, and sensitivity analysis on the HI conversion was observed in the modeling process. The addition of small amount of diatomic iodine greatly decreases the HI conversion, and the overall pressure could promote the HI decomposition rate in the kinetic process. Sensitivity analysis shows that hydrogen yield was most sensitive to reactions (4) HI + H = H₂ + I, (1) HI + HI = H₂ + I₂, (5) HI + I = I₂ + H, and (8) HI + OH = H₂O + I. The existence of diatomic iodine increases the reverse reaction of (1) and (5).     

Comparisons of Pt catalysts supported on active carbon,carbon molecular sieve,carbon nanotubes and graphite for HI decomposition at different temperature

A series of Pt catalysts supported on activated carbon (AC), carbon molecular sieve (CMS), carbon nanotubes (CNT) and graphite (GR) were prepared by the impregnation method. Their catalytic performances in HI decomposition were evaluated in a fixed bed reactor at temperatures ranging from 400 to 550 °C under atmospheric pressure. The different Pt catalysts before and after HI decomposition at different temperature were characterized by BET, XRD and TEM, respectively. The results of the activity evaluation indicated that the activity order of different Pt catalysts changed significantly with the variation of reaction temperature. At 400 °C, different supported Pt catalysts activities decreased in order of Pt/CMS > Pt/AC > Pt/CNT > Pt/GR. At 450 °C, the activities of different Pt catalysts followed the order of Pt/AC ≈ Pt/CNT > Pt/CMS > Pt/GR. At 500 and 550 °C, the Pt/CNT showed the optimum activity and stability during HI decomposition, which could be attributed to the high dispersion of Pt particles and the special microstructure of CNT. The XRD and TEM results illustrated that the Pt particle size or Pt dispersion in different supported Pt catalysts showed different sensitivity to the reaction temperature.     

Detailed kinetic modeling of homogeneous HI decomposition for hydrogen production,part I: Effect of H2O on HI decomposition

A new, detailed kinetic model was developed for the homogeneous decomposition of HI–H₂O solutions in vapor phase in the sulfur–iodine cycle. The kinetics of the process was represented by a reaction mechanism involving 32 reactions and 11 species. Comparisons between the kinetic calculations and experimental data showed that this model correctly predicted the hydrogen yield at the 500 °C–1000 °C temperature range under 1 atm. The effects of temperature, reaction time, and HI/H₂O ratio on HI decomposition and hydrogen sensitivity analysis were investigated in the modeling process. The model predicted that the effect of the addition of H₂O changed from inhibiting the decomposition ratio to promoting it with increasing temperature. The sensitivity analysis showed that elementary reactions (1) HI + HI = H₂+I₂, (4) HI + H = H₂ + I, (5) HI + I = H + I₂, and (8) HI + OH = H₂O + I played important roles in hydrogen production. The reaction path of HI decomposition with H₂O was constructed based on detailed kinetic modeling and sensitivity analysis results.     

Hydrogen‐rich gas production from catalytic gasification of pine sawdust over Fe‐Ce/olivine catalyst

In order to improve hydrogen production and reduce tar generation during the biomass gasification, a catalyst loaded Fe‐Ce using calcined olivine as the support (Fe‐Ce/olivine catalysts) was prepared through deposition‐precipitation method. The characteristics of catalysts were determined by XRF, BET, XRD, and FTIR. Syngas yield, hydrogen yield, and tar yield were used to evaluate the catalyst activity. Meanwhile, the stability of catalysts was also studied. The results showed that the specific surface area and pore volume of olivine after calcined at high temperature were improved which was beneficial for the load of metals. α‐Fe₂O₃ and CeO₂ were the main active component of Fe‐Ce/olivine catalyst. The Fe‐Ce/olivine catalyst displayed a good performance on the catalytic gasification of pine sawdust with a syngas yield of 0.93 Nm³/kg, H₂ yield of 21.37 mol/kg, and carbon conversion rate of 55.14% at a catalytic temperature and gasification temperature of 800°C. Meanwhile, the Fe‐Ce/olivine catalyst could maintain a good stability after 150 minutes used.     

Cu/La2O3/Al2O3催化剂上甲醇水蒸气重整制氢反应

研究以并流共沉淀法制备Cu/La2 O3 /Al2 O3 系列催化剂催化甲醇水蒸气重整制氢反应过程 ,考察了La2 O3含量、反应温度、水醇比、液体空速 (WHSV)等因素对催化剂活性的影响。结果表明 :催化剂表现出较好的低温活性、高氢气选择性和稳定性。La2 O3 质量分数为 15 % ,在 2 5 0℃反应时 ,催化剂活性表现最佳 ,甲醇摩尔转化率为94 .5 % ,氢气选择性为 10 0 % ,CO摩尔分数为 1.0 5× 10 -7。     

Cu/ZnO/Al2O3催化剂涂层工艺参数的优化

针对甲醇水蒸汽重整制氢反应，研制了一种新型的适用于微槽道反应器的Cu/ZnO/Al2O3催化剂涂层。通过对其关键制备参数的优化，筛选出COAT-14-6（CuO 14wt．％，ZnO6wt．％）为性能最佳的催化剂涂层。研究发现Cu，ZnO／Al2O3涂层催化剂的活性与活性铜的表面积和催化剂的还原性密切相关。100h的连续性实验结果表明，涂覆了COAT-14-6的微槽道反应器可以与10W的燃料电池配套。     

A high‐performance CeO2@Pt‐Beta yolk‐shell catalyst used in low‐temperature ethanol steam reforming for high‐purity hydrogen production

A novel Pt‐based Beta encapsulated CeO₂ yolk‐shell catalyst was successfully synthesized via a RF layer in the synthetic process. The CeO₂@Pt‐Beta catalyst showed high catalytic activity and stability toward the LT‐ESR with respect to the reference Pt‐Beta, CeO₂‐Pt‐Beta, which benefited from the special yolk‐shell structure and the synergistic effect between the CeO₂ movable core and Pt metal. The confinement effect of the yolk‐shell architecture contributed to the high dispersion of Pt nanoparticles as well as to the accumulation of reactant molecules in the enclosed void space, which ensured the reactants reacted with CeO₂ and Pt to achieve a complete reaction.     

Pt/ZrO2 catalyst for a single-stage water-gas shift reaction: Ti addition effect

Ti modified Pt/ZrO₂ catalysts were prepared to improve the catalytic activity of Pt/ZrO₂ catalyst for a single-stage WGS reaction and the Ti addition effect on ZrO₂ was discussed based on its characterization and WGS reaction test. Ti impregnation into ZrO₂ increased the surface area of the support and the Pt dispersion. The reducibility of the catalyst was enhanced in the controlled Ti impregnation (∼20 wt.%) over Pt/ZrO₂ by the Pt-catalysed reduction of supports, particularly, at the interface between ZrO₂ and TiO₂. The significant CO₂ gas band in the DRIFTS results of Pt/Ti[20]/ZrO₂ indicated that the Ti addition made the formate decomposition rate faster than the Pt/ZrO₂ catalyst, linked with the enhanced Pt dispersion and reducibility of the catalyst. Consequently, Ti impregnation over the ZrO₂ support led to a remarkably enhanced CO conversion and the reaction rate of Pt/Ti[20]/ZrO₂ increased by a factor of about 3 from the bare Pt/ZrO₂ catalyst.     

Synthesis,characterization and corrosion performance evaluation of DDR membrane for H2 separation from HI decomposition reaction

An all silica DDR (deca dodecasil rhombohedral) zeolite membrane with dense, interlocked structure has been developed for separation of H₂ from HI/I₂ mixture of HI decomposition reaction. In this work, the DDR zeolite membrane was synthesized on the seeded clay-alumina substrate within 5 days. The seeds were synthesized by sonication mediated hydrothermal process within short crystallization time which enhanced the nucleation for the membrane growth. The synthesized membranes along with seed crystals were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR), Field emission scanning electron microscope (FESEM) and energy dispersive X-ray spectroscopy (EDAX). The selectivity of hydrogen with respect to CO₂ and Ar was evaluated by single gas permeation studies at room temperature. The tests for corrosion resistance were carried out upto 120 h with both support and DDR membrane at 130 °C which confirmed the stability of membrane under the harsh HI/I₂ environment.     

Synthesis and characterization of H3PW12O40/Ce0.1Ti0.9O2 for dimethyl carbonate formation via Methanol carbonation

Ce_0.1Ti_0.9O₂ and H₃PW₁₂O₄₀/Ce_0.1Ti_0.9O₂ catalysts were synthesized with a sol–gel method to form dimethyl carbonate (DMC) at reaction temperatures T = 110, 170, and 220 °C and volumetric flow-rate ratios CO₂/N₂ = 1/4, 1/7, and 1/9. The zeolite-like properties of H₃PW₁₂O₄₀/Ce_0.1Ti_0.9O₂ with an organized Keggin heteropolyacid structure were demonstrated from X-ray diffraction patterns and Fourier transform infrared spectra. ³¹P nuclear magnetic resonance spectra indicated that the Keggin heteropolyacid structure was formed through the addition of heteropoly acid (H₃PW₁₂O₄₀). The bond lengths between titanium (Ti(IV)) and its adjacent atoms in the first shell (TiO) of Ce_0.1Ti_0.9O₂ and H₃PW₁₂O₄₀/Ce_0.1Ti_0.9O₂ were 1.90 and 1.86 Å, respectively, confirmed with EXAFS spectra. At 170 °C and CO₂/N₂ = 1/7, the optimal methanol conversion (5.5%), DMC selectivity (91.4%), and DMC yield (5.0%) of H₃PW₁₂O₄₀/Ce_0.1Ti_0.9O₂ were greater than those of Ce_0.1Ti_0.9O₂. Linear regressions of the pseudo-first-order model indicated that the largest rate constant (4.16 × 10⁻³ min⁻¹), turnover number (TON = 29.07), and turnover frequency (TOF = 4.85 × 10⁻² min⁻¹) of DMC formation were obtained with H₃PW₁₂O₄₀/Ce_0.1Ti_0.9O₂ at 170 °C and CO₂/N₂ = 1/7. A reaction mechanism induced by oxygen vacancies over the surfaces of Ce_0.1Ti_0.9O₂ and H₃PW₁₂O₄₀/Ce_0.1Ti_0.9O₂ is proposed to describe the formation of DMC.     

Syngas production via CO2 reforming of methane over plasma assisted synthesized Ni‐Co/Al2O3‐ZrO2 nanocatalysts with different Ni‐loadings

Ni‐Co/Al₂O₃‐ZrO₂ nanocatalysts with 5, 10 and 15 wt.% nominal Ni content have been prepared by impregnation followed by a non‐thermal plasma treatment, characterized and tested for dry reforming of methane. For nanocatalysts characterization the following techniques have been used: XRD, FESEM, TEM, EDX dot‐mapping, BET, FTIR and XPS. The dry reforming of methane was carried out at different temperatures (550‐850 °C) using a feed mixture of CH₄:CO₂ (1:1). Among the nanocatalysts studied, the catalyst with the medium Ni content (10 wt.%) was the most active in dry reforming of methane. This higher activity exhibited by Ni‐Co/Al₂O₃‐ZrO₂ catalyst with medium Ni content (10 wt.% ) can be attributed to small and well dispersed particles of Ni within the catalyst. Apart from the narrow surface particle size distribution in the case of Ni(10 wt.%)‐Co/Al₂O₃‐ZrO₂, the presence of small active components with average size of 7.5 nm is proposed to be the reason for the superior performance of the catalyst. Ni(10 wt.%)‐Co/Al₂O₃‐ZrO₂ nanocatalyst had maximum surface area and the lower surface area was observed in the case of Ni(5 wt.%)‐Co/Al₂O₃‐ZrO₂ and Ni(15 wt.%)‐Co/Al₂O₃‐ZrO₂ due to the formation of the larger agglomeration and higher mean particle size of nickel particles, respectively. Although, GHSV enhancment had inverse effect on product yield but yield reduction for Ni‐Co/Al₂O₃‐ZrO₂ catalyst with 10 wt.% Ni was less drastic at high GHSVs. According to XRD and XPS, existence of NiAl₂O₄ confirms strong interaction between Ni and support but higher loadings of Ni resulted in less NiAl₂O₄; loser interaction between support and active phase. Small particles of active components and well‐defined dispersion of them in Ni(10 wt.%)‐Co/Al₂O₃‐ZrO₂ nanocatalyst resulted in stability of the catalyst for either feed conversion or H₂/CO molar ratio. Copyright © 2013 John Wiley & Sons, Ltd.     

Nanocomposite Ni/ZrO2: Highly active and stable catalyst for H2 production via cyclic stepwise methane reforming reactions

This work investigates the catalytic performance of nanocomposite Ni/ZrO₂-AN catalyst consisting of comparably sized Ni (10–15 nm) and ZrO₂ (15–25 nm) particles for hydrogen production from the cyclic stepwise methane reforming reaction with either steam (H₂O) or CO₂ at 500–650 °C, in comparison with a conventional Ni/ZrO₂-CP catalyst featuring Ni particles supported by large and widely sized ZrO₂ particles (20–400 nm). Though both catalysts exhibited similar activity and stability during the reactions at 500 and 550 °C, they showed remarkably different catalytic stabilities at higher temperatures. The Ni/ZrO₂-CP catalyst featured a significant deactivation even during the methane decomposition step in the first cycle of the reactions at ≥600 °C, but the Ni/ZrO₂-AN catalyst showed a very stable activity during at least 17 consecutive cycles in the cyclic reaction with steam. Changes in the catalyst beds at varying stages of the reactions were characterized with TEM, XRD and TPO–DTG and were correlated with the amount and nature of the carbon deposits. The Ni particles in Ni/ZrO₂-AN became stabilized at the sizes of around 20 nm but those in Ni/ZrO₂-CP kept on growing in the methane decomposition steps of the cyclic reaction. The small and narrowly sized Ni particles in the nanocomposite Ni/ZrO₂-AN catalyst led to a selective formation of filamentous carbons whereas the larger Ni particles in the Ni/ZrO₂-CP catalyst a preferred formation of graphitic encapsulating carbons. The filamentous carbons were favorably volatilized in the steam treatment step but the CO₂ treatment selectively volatilized the encapsulating carbons. These results identify that the nature but not the amount of carbon deposits is the key to the stability of Ni/ZrO₂ catalyst and that the nanocomposite Ni/ZrO₂-AN would be a promising catalyst for hydrogen production via cyclic stepwise methane reforming reactions.     

Conversion of hydrogen/carbon dioxide into formic acid and methanol over Cu/CuCr2O4 catalyst

Cu/CuCr₂O₄ catalysts were prepared by impregnation method at various calcination temperatures (300, 400, and 500 °C) and then reduced in H₂ stream. The aggregated particles and decreasing surface area/pore volumes of the deactivated catalysts during HCOOH and CH₃OH formations were also observed. Particularly, the EXAFS data showed that first shells of Cu atoms transforms from Cu–O to Cu–Cu after catalytic reactions, their bond distances and coordination numbers are quite different, respectively. It revealed that metallic Cu atoms are one of the important active species over catalyst surface at different reaction temperatures having many unoccupied binding sites for HCOOH and CH₃OH formations. Additionally, the optimal calcination temperature for Cu/CuCr₂O₄ catalysts was demonstrated at 400 °C that attributed to its strongest acidity and basicity. The catalytic reactions in the duration of HCOOH and CH₃OH preparation were proposed that were composed of HCOOH formation, CH₃OH formation, and CH₃OH decomposition happening at CuCr₂O₄, Cu, and CuO active sites, respectively. The highest CO₂ conversion (14.6%), HCOOH selectivity/yield (87.8/12.8%), and TON/TOF values (4.19/0.84) were obtained at 140 °C and 30 bar in 5 h, respectively. Optimal rate constant (2.57 × 10^?2 min^?1) and activation energy (16.24 kJ mol^?1) of HCOOH formation were evaluated by pseudo first-order model and Arrhenius equation, respectively.     

β‐molybdenum carbide/carbon nanofibers as a shuttle inhibitor for lithium‐sulfur battery with high sulfur loading

We report the synthesis of β‐molybdenum carbide/carbon nanofibers (β‐Mo₂C/CNFs) by electrospinning and annealing process, when exploited as an interlayer in Li‐S batteries, demonstrating significantly improved electrochemical behaviors. The synthesized β‐Mo₂C/CNFs with 3D network structure and high surface area are not only conducive to ion transport and electrolyte penetration but also effectively intercept the shuttle of lithium polysulfide by polar surface interaction. Moreover, the reaction kinetics of the batteries enhanced is due to the presence of β‐Mo₂C, promoting the solid‐state polysulfide conversion reaction in the charge‐discharge process. Compared with the batteries with CNF interlayer and without interlayer, the batteries using a β‐Mo₂C/CNFs interlayer with a sulfur loading of 4.2 mg cm^‐2 delivered excellent electrochemical performance because of a facile redox reaction during cycling. The discharge capacity at the first cycle at 0.7 mA cm^?2 was 1360 mAh g^?1, maintaining a specific capacity of 974 mAh g^?1 after 160 cycles. Furthermore, it showed a high‐rate capacity of 700 mAh g^?1 at 14 mA cm^?2. This work demonstrates the β‐Mo₂C/CNFs as a promising interlayer to exploit Li‐S battery commercialization.