Fe 2 O 3 nano particles embedded Fe 2 O 3 /BP2000 composite for Li-S battery

Fe 2 O 3 nano particles embedded Fe 2 O 3 /BP2000 composite for Li-S battery | 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 Fe 2 O 3 nano particles embedded Fe 2 O 3 /BP2000 composite for Li-S battery Yi Lu, Tao Liu This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3972507/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 12 You are reading this latest preprint version Abstract Shuttle effect of lithium polysulfides in lithium sulfur batteries greatly influenced their commercialization. Therefore, it is urgent to develop a cheep and effective way to alleviate the shuttle effect. Fe is an active transition element which has good catalytic ability, in this work, a simple wet impregnation method was used to make Fe ions infiltrate into the pores of BP2000 (a kind of commercial conductive carbon), then it was calcined in N 2 atmosphere to get a Fe 2 O 3 /BP2000 composite and used as a separator modification layer. The Fe 2 O 3 nano particles are decorated in the pores of BP2000 which greatly enhanced the absorption ability on lithium polysulfides, additionally it also has excellent catalytic effect on lithium polysulfides, thus the Fe 2 O 3 /BP2000 layer can be served as a secondary collector to re-engage the polysulfides in the cathode reaction. In this way, the lithium sulfur batteries use the Fe 2 O 3 /BP2000 modified separator show impressive electrochemical performances. Fe2O3/BP2000 modified separator shuttle effect lithium polysulfides lithium sulfur battery Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Introduction The rapid development of electronic devices and electrical vehicles stimulates the demands for high performance secondary batteries. In recent years, Li-S battery has attracted much notice based on the high theoretical capacity of 1675 mAh g − 1 for sulfur cathode. What is more, the advantages of natural abundance, cheep price, low pollution make Li − S battery become one of the most promising secondary batteries[ 1 – 3 ]. Despite these advantages, the practical use of Li-S battery still faces several challenges. First of all, the insulating nature of sulfur induces low active material utilization. Secondly, the volume difference between sulfur and end product Li 2 S can cause the positive electrode to crack. Thirdly, the migration of soluble lithium polysulfides between cathode and anode which is called “shuttle effect” can lead to several obstacles such as low Coulombic efficiency, poor durability, Lithium dendrite deposition in the anode, etc.[ 4 – 6 ]. Thus, a variety of approaches to address the above obstacles are investigated. For example, various carbon based materials and other materials have been reported to act as the sulfur host to enhance the conductivity of sulfur, confine the soluble lithium polysulfides and alleviate the volume change. Electrolytes are also optimized by changing the solvents, salts, and additives to decrease the solubility of lithium polysulfides or slow down the migration speed of lithium polysulfides. Furthermore, various strategies have been conducted to prevent the lithium dendrite deposition on the Li anode so as to improve its interfacial and structural stability[ 7 – 10 ]. Apart from these optimizing strategies, separator modifications in recent researches have also been demonstrated a promising method to confine large amount of lithium polysulfides in the cathode region. For instance, different carbon materials have been proved to be an excellent modification layer for Li-S battery separator, such as microporous carbon, graphene, and carbon nanotubes, etc.[ 11 – 13 ]. Furthermore, different kinds of polar materials such as metal oxides, metal sulfides etc. have also been demonstrated good modification materials because of their chemical interactions with lithium polysulfides[ 14 – 20 ]. In this work, we deliberately combined a commercial conductive carbon named BP2000 with Fe 2 O 3 via a simple wet impregnation method followed by a high temperature calcination. The Fe 2 O 3 /BP2000 composite is used as a separator coating layer in Li-S battery. The BP2000 constructs excellent conductive network to facilitate the charge transfers inside Li-S battery. Additionally, its rich porous structure is beneficial to adsorb a large amount of polysulfides. Furthermore, the Fe 2 O 3 nano particles embedded in the pores of BP2000 not only have strong chemical interaction with lithium polysulfides, but also catalyze the chemical reactions during cycling. Benefit from its adsorption and catalytic ability, the loss of the active materials in the cathode can be greatly alleviated and the redox kinetics can be also accelerated, therefore the cycle and rate performance of Li-S battery are largely improved. Experimental section 2.1 Synthesis of Fe 2 O 3 /BP2000 composite Fe 2 O 3 /BP2000 composite was prepared by a simple impregnation method followed by a high temperature calcination. In a typical preparation process, 1.5g BP2000 was dispersed homogeneously by a mixture of 120 mL ultra pure water and 30 mL absolute ethyl alcohol. At the same time 0.5695 g Fe(NO 3 ) 3 •9H 2 O was dissolved completely in 10 mL ultra pure water. Then the Fe(NO 3 ) 3 •9H 2 O solution was added dropwisely into the BP2000 suspension, in this procedure Fe 3+ ion can be absorbed by the pores of BP2000. Afterwords, the BP2000 suspension was centrifugated and dried in an air blast drying oven. At last the dried powder was put into a tube furnace and calcined at 900°C for 2 h to obtain Fe 2 O 3 /BP2000 composite. 2.2 Fabrication of the Fe 2 O 3 /BP2000 modified separator The Fe 2 O 3 /BP2000 modified separator was prepared by a simple slurry coating method. Typically, 0.08g Fe 2 O 3 /BP2000, 0.01g super P and 0.01g PVDF were homogeneously dispersed in 4 mL NMP by vigorously stirring. The mixture was then coated onto the PE separator by a doctor blade. After the coating procedure, the Fe 2 O 3 /BP2000 coated PE separator was dried in an air blast drying oven and at last cut into small discs. For comparison purpose, BP2000 coated PE separator was also fabricated by the same procedures. The photo of the Fe 2 O 3 /BP2000 coated PE separator is shown in Figure S1 , and the cross section SEM demonstrates that the coating layer is approximately 10 µm. 2.3 Fabrication of BP2000/S cathode electrode In a typical fabrication procedure, 1 g sublimed sulfur and 4 g BP2000 are mixed and dispersed in 30 mL absolute ethyl alcohol. Then the mixture was put into a 50 mL mill pot and ball milled at 900 r/min for 3 h. Afterwards, the sulfur and BP2000 mixture was dried and put into a vacuum oven and heated at 155°C for 10 h to obtain BP2000/S composite. To fabricate BP2000/S cathode electrode, 0.8 g BP2000/S composite, 0.1 g super P and 0.1 g PVDF were dispersed in 4 g NMP and stirred in a defoaming mixer at 2500 rpm for 3 min. The slurry was then spread onto Al foil and dried at 80°C for 10 h in a vacuum oven, at last the dried Al foil was cut into circle discs at wait for use, the sulfur area density on the cathode electrode was 3 mg cm − 2 . 2.4 Cells assembly and electrochemical measurements BP2000/S cathode electrode, Li-S electrolyte (1 M LiTFSI with 0.1 M LiNO 3 dissolved in DOL/DME solvent), Fe 2 O 3 /BP2000 modified separator and Li anode electrode are assembled into Li-S coin cells in an Ar filled glove box. The cycle and rate performances of the Li-S cells were tested by a LAND battery testing equipment, The cyclic voltammetry (CV) profiles and electrochemical impedance spectroscopy (EIS) curves were conducted via a VMP 3 electrochemical workstation. 2.5 Materials characterization The morphology and nano structure was characterized by field-emission scanning electron microscope (FESEM, NOVA Nano SEM 430) and transmission electron microscope (TEM, Tecnai G2 F20 S-TWIN). Crystal structure characterization were conducted by a X-ray diffractometer (XRD, Rigaku D/Max 2500). The porous structure and specific surface area was determined by a surface area analyzer. Results and discussions Figure 1 shows the XRD patterns of BP2000 and Fe 2 O 3 /BP2000 composite. The XRD pattern of BP2000 shows two broad diffraction peaks at around 26° and 45°, refers to the (002) crystal plane of carbon. Furthermore, the XRD pattern of Fe 2 O 3 /BP2000 composite show obvious diffraction peaks at 18.3°, 30.2°, 35.6°, 37.2°, 43.3°, 53.7°, 57.3°, 62.9°, 71.3°, 74.5° and 77.4°, which match with the crystal faces of (111), (220), (311), (222), (400), (422), (511), (440), (620), (533) and (631) respectively, according to the PDF card JD39-1436 of Fe 2 O 3 , demonstrating the successful preparation of Fe 2 O 3 /BP2000 composite[ 21 ]. Figure 2 (a) and (b) show the SEM images of BP2000 and Fe 2 O 3 /BP2000 composite. The morphology of the two SEM images are approximately the same, demonstrating that Fe 2 O 3 are embedded in the pores of BP2000. In order to further investigate the micro structure of Fe 2 O 3 /BP2000 composite, TEM analysis are carried out and the TEM images are shown in Fig. 2 (c)-(f). Figure 2 (c) shows the TEM image of BP2000, the BP2000 nano particles are approximately 20–50 nm with abundant porous structure. Figure 2 (d) and (e) shows that Fe 2 O 3 nanoparticles are homogeneously dispersed in the pores of BP2000, furthermore, the HRTEM in Fig. 2 (f) clearly shows the lattice fringe of 0.25 nm which matches with the (311) face of Fe 2 O 3 nanoparticles, which demonstrates that Fe 2 O 3 nanoparticles are successfully embedded into the pores of BP2000. We use N 2 adsorption - desorption experiment to estimate the BET specific surface area and pore size distribution of BP2000 and Fe 2 O 3 /BP2000 composite. Figure 3 (a) shows the N 2 adsorption-desorption isotherms of BP2000 and Fe 2 O 3 /BP2000 composite, both of the two isotherms display a type IV hysterrisis curve, demonstrating that BP2000 and Fe 2 O 3 /BP2000 composite are composed of abundant micro and meso pores, which will be benefit for the adsorption for the lithium polysulfides. According to the BET calculation, the specific surface area of BP2000 and Fe 2 O 3 /BP2000 composite are 1229 and 1057 m 2 g − 1 . The specific surface area of BP2000 decrease a little after the combination of Fe 2 O 3 , indicating that Fe 2 O 3 occupied some of the pores. Figure 3 (b) depicts the pore structures of BP2000 and Fe 2 O 3 /BP2000 composite, both of the two materials are composed of pores form 2–10 nm, and most of the pore diameter are around 3.8 nm, the pore volumes of BP2000 and Fe 2 O 3 /BP2000 composite are 2.8 and 2.54 m 3 g − 1 , the decrease of pore volume also demonstrates that Fe 2 O 3 particles are confined by the pores of BP2000. Additionally, the relatively small pore diameter can effectively absorb the soluble lithium polysulfides[ 22 – 23 ]. In order to directly demonstrate the absorption capability of BP2000 and Fe 2 O 3 /BP2000 composite, a L 2 S 6 solution absorption experiment was carried out. A shown in Fig. 4 (a), BP2000 and Fe 2 O 3 /BP2000 were put into Li 2 S 6 solution and held for 8 h. The photo of Li 2 S 6 solution displays a dark yellow color, while the Li 2 S 6 -BP2000 solution displays a light yellow color demonstrating that Li 2 S 6 can be absorbed by BP2000. Furthermore, the Li 2 S 6 - Fe 2 O 3 /BP2000 solution after 8 h absorption displays a transparent color which demonstrates that Fe 2 O 3 /BP2000 has an excellent absorption capability on lithium polysulfides. The Li 2 S 6 solution after absorption experiment was tested by UV spectroscopy, as shown in Fig. 4 (b), the Li 2 S 6 UV-Vis absorption spectrum of Li 2 S 6 - Fe 2 O 3 /BP2000 solution after 8 h absorption displays the lowest absorption peak, indicating its Li 2 S 6 concentration is also the lowest which is mostly absorbed by Fe 2 O 3 /BP2000 composite[ 24 – 25 ]. The advantages of Fe 2 O 3 /BP2000 modified separator was further studied by electrochemical performances. As shown in Fig. 5 (a), CV profiles of the three different batteries show apparently two reduction peaks at around 2.3 and 2.0 V and one oxidation peak at at around 2.4 V. The reduction peak at 2.3 V represents the reduction process of sulfur to soluble lithium polysulfides and the reduction peak at 2.0 V represents the reduction process of soluble lithium polysulfides to end product Li 2 S 2 /Li 2 S. The broad oxidation peak at around 2.4 V represents the gradual oxidation process of Li 2 S 2 /Li 2 S to sulfur. At the same time, the Fe 2 O 3 /BP2000 modified separator battery has the largest current density, indicating its capacity is also the largest. Additionally, the second reduction peak voltage of Fe 2 O 3 /BP2000 sample is a little bit higher than the BP2000 and PE separator sample, demonstrating it has a better reaction kinetics. In order to further demonstrate the catalytic effect of Fe 2 O 3 /BP2000 composite, a symmetric cell experiment was carried out. The assemble process of symmetric cell and its structure diagram is given in the support information. CV measurement results of symmetric cells are shown in Fig. 5 (b), as displayed in the figure, BP2000 and Fe 2 O 3 /BP2000 symmetric cells with Li 2 S 6 electrolyte show obvious current peaks, while the current of Fe 2 O 3 /BP2000 symmetric cell without Li 2 S 6 electrolyte is nearly zero. Additionally, the current peak of Fe 2 O 3 /BP2000 symmetric cell is much larger than that of the BP2000 symmetric cell demonstrating the catalytic effect is mainly caused by the combination of Fe 2 O 3 nano particles[ 26 ]. Figure 6 (a) depicts the discharge/charge profiles of the three samples at 0.1 C, all the batteries show two typical discharge platforms and one charge platform which is consistent with the reduction and oxidation peaks of CV curves. Additionally, the potential gaps of BP2000 and Fe 2 O 3 /BP2000 separator batteries is apparently smaller which indicates the remarkably improved electrochemical kinetics. Long cycle performances were performed to evaluate the discharge/charge capacities and cycle stability of BP2000 and Fe 2 O 3 /BP2000 modified separator. Figure 6 (b) shows the long term cycle performances of different batteries. When the sulfur area density in the cathode is 3 mg cm − 2 , the initial discharge capacities of PE, BP2000 and Fe 2 O 3 /BP2000 separator batteries at 0.1 C are 986, 1280 and 1350 mAh g − 1 respectively, as the current rate adds up to 0.5 C, the discharge capacities of the batteries are 650, 911 and 1140 mAh g − 1 respectively. At the 200 cycles, the discharge capacity of the PE separator battery suffers a sharp decline and the battery can hardly release capacity. By comparison, the BP2000 and Fe 2 O 3 /BP2000 separator batteries show a steady cycle performance for more than 500 cycles, furthermore the Fe 2 O 3 /BP2000 displays a much higher discharge capacity (500 mAh g − 1 ) at the 500 cycle than that of the BP2000 sample (320mAh g − 1 ). The higher discharge capacity of Fe 2 O 3 /BP2000 battery is mainly caused by the combination of Fe 2 O 3 nano particles which can improve the absorption capability of lithium polysulfides. The rate performances of the PE, BP2000 and Fe 2 O 3 /BP2000 samples are shown in Fig. 6 (c). The discharge capacities of the Fe 2 O 3 /BP2000 separator battery at different current rates are much larger than that of the BP2000 separator battery and PE separator battery. Furthermore, the Fe 2 O 3 /BP2000 separator battery displays a highly reversible capacity of 1020 mAh g − 1 at 1 C and gradually recovers to 1250 mAh g − 1 as the current was set back to 0.1 C, indicating its fast redox reaction speed. EIS curves of different separator batteries were collected before cycle. As displayed in Fig. 6 (d), the inset in the X axis are approximately the same demonstrating that the electrolyte environment are approximately the same. Furthermore, the diameter of the semicircle which represents the charge transfer resistance clearly indicates that the use of BP2000 and Fe 2 O 3 /BP2000 separator can apparently decrease the internal resistance of the Li-S battery. This can be attributed to the low conductivity of BP2000. Additionally, the oblique line of Fe 2 O 3 /BP2000 sample in the high frequency region shows the largest slop which indicates the Fe 2 O 3 /BP2000 separator has the fastest Li ion transportation speed which can accelerate the reaction speed[ 27 – 28 ]. Conclusion In summary, the Fe 2 O 3 /BP2000 was successfully prepared by a simple wet-impregnation followed by a high temperature treatment in N 2 atmosphere. XRD, SEM and TEM analysis demonstrate that Fe 2 O 3 nanoparticles with a diameter of 5–30 nm are homogeneously embedded in the pores of BP2000. 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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-3972507","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":285576042,"identity":"387e34ca-dc9f-4ecc-940c-2c9c8abca828","order_by":0,"name":"Yi Lu","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA6UlEQVRIie3RsUoDQRCA4ZGFTTN67QbC+QoLB0HwwCIvMkvkbKIc2FjYSMArssE2j5FHmGNhbdb+yvgGprtK1NqQPTuL/er5mVkWIEn+IZktuf3Ax/zqtWl31Jfx5Ex549TEFxDCXL/bKp7ksCgYS2Ggo+l4J92AwyBoVgtJJ5arB0IHWbOi44l4rrkOkzsxevIdXdyACm/byBa35bGV9xK56ggvQavbWEKaTz+FsYqmNUkxJLnWjCjM5jsBkrMBifLkFPpCY5grYyuMvuX8Zen2P1+pR0277/syz5r18eQX/Nt4kiRJctAXiOxL8GOdLxwAAAAASUVORK5CYII=","orcid":"","institution":"Zhenjiang Custom","correspondingAuthor":true,"prefix":"","firstName":"Yi","middleName":"","lastName":"Lu","suffix":""},{"id":285576044,"identity":"84a75af8-cd45-4f93-8ab0-c5e88f6014f4","order_by":1,"name":"Tao Liu","email":"","orcid":"","institution":"Zhenjiang Custom","correspondingAuthor":false,"prefix":"","firstName":"Tao","middleName":"","lastName":"Liu","suffix":""}],"badges":[],"createdAt":"2024-02-20 10:34:01","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3972507/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3972507/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":53997157,"identity":"e8df9e2a-b794-4b7c-abdc-6d04e49c71c8","added_by":"auto","created_at":"2024-04-03 07:29:40","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":22105,"visible":true,"origin":"","legend":"\u003cp\u003eXRD patterns of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/4cb0112abee6b93b9a4847f8.png"},{"id":53997159,"identity":"fd6cb744-4722-4c20-909c-2ffc065be84a","added_by":"auto","created_at":"2024-04-03 07:29:41","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":1965063,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of (a) BP2000 and (b) Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, (c) TEM image of BP2000, (d)-(e) TEM images of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite. (f) HRTEM image of a single Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3 \u003c/sub\u003enanoparticle\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/11dd231b783632f6e41a47f4.png"},{"id":53997158,"identity":"99b04057-608d-482c-9a50-6c41c502c8f4","added_by":"auto","created_at":"2024-04-03 07:29:41","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":112772,"visible":true,"origin":"","legend":"\u003cp\u003e(a) N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, (b) pore structures of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite.\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/702e91b04ad8841f315a6290.png"},{"id":53997598,"identity":"70eb48e8-95a1-4a0b-92fb-880874db537d","added_by":"auto","created_at":"2024-04-03 07:37:41","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":549545,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e absorption experiments, (b) Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e UV-Vis absorption spectrum of different samples\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/d306f8302fc462ae29d51792.png"},{"id":53997165,"identity":"114d63b9-9362-45ba-a1f5-8fd8dcea327e","added_by":"auto","created_at":"2024-04-03 07:29:41","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":134857,"visible":true,"origin":"","legend":"\u003cp\u003e(a) CV curves of PE, BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator Li-S batteries, (b) BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 symmetric cell experiments.\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/a0f8bdde1fc0308157f77a0d.png"},{"id":53997160,"identity":"ce1048e2-9536-4dc6-a3ea-1a13cc8435dd","added_by":"auto","created_at":"2024-04-03 07:29:41","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":241786,"visible":true,"origin":"","legend":"\u003cp\u003e(a) discharge/charge profiles, (b) long cycle performances, (c) rate performances and (d) EIS curves of PE, BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator Li-S batteries.\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/0e6b5621719c9b04a489078e.png"},{"id":53998047,"identity":"92e2a6cf-0fde-48eb-afc2-c886a3542936","added_by":"auto","created_at":"2024-04-03 07:45:46","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2454698,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/f213933f-c689-49c9-9969-f9b58fadad99.pdf"},{"id":53997162,"identity":"93526c37-0ec1-49ab-b28a-a52027efddaa","added_by":"auto","created_at":"2024-04-03 07:29:41","extension":"docx","order_by":2,"title":"","display":"","copyAsset":false,"role":"supplement","size":1761123,"visible":true,"origin":"","legend":"","description":"","filename":"supportinformation.docx","url":"https://assets-eu.researchsquare.com/files/rs-3972507/v1/d8bd591a226044c8840e5a9b.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Fe 2 O 3 nano particles embedded Fe 2 O 3 /BP2000 composite for Li-S battery","fulltext":[{"header":"Introduction","content":"\u003cp\u003eThe rapid development of electronic devices and electrical vehicles stimulates the demands for high performance secondary batteries. In recent years, Li-S battery has attracted much notice based on the high theoretical capacity of 1675 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for sulfur cathode. What is more, the advantages of natural abundance, cheep price, low pollution make Li\u0026thinsp;\u0026minus;\u0026thinsp;S battery become one of the most promising secondary batteries[\u003cspan additionalcitationids=\"CR2\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. Despite these advantages, the practical use of Li-S battery still faces several challenges. First of all, the insulating nature of sulfur induces low active material utilization. Secondly, the volume difference between sulfur and end product Li\u003csub\u003e2\u003c/sub\u003eS can cause the positive electrode to crack. Thirdly, the migration of soluble lithium polysulfides between cathode and anode which is called \u0026ldquo;shuttle effect\u0026rdquo; can lead to several obstacles such as low Coulombic efficiency, poor durability, Lithium dendrite deposition in the anode, etc.[\u003cspan additionalcitationids=\"CR5\" citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThus, a variety of approaches to address the above obstacles are investigated. For example, various carbon based materials and other materials have been reported to act as the sulfur host to enhance the conductivity of sulfur, confine the soluble lithium polysulfides and alleviate the volume change. Electrolytes are also optimized by changing the solvents, salts, and additives to decrease the solubility of lithium polysulfides or slow down the migration speed of lithium polysulfides. Furthermore, various strategies have been conducted to prevent the lithium dendrite deposition on the Li anode so as to improve its interfacial and structural stability[\u003cspan additionalcitationids=\"CR8 CR9\" citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. Apart from these optimizing strategies, separator modifications in recent researches have also been demonstrated a promising method to confine large amount of lithium polysulfides in the cathode region. For instance, different carbon materials have been proved to be an excellent modification layer for Li-S battery separator, such as microporous carbon, graphene, and carbon nanotubes, etc.[\u003cspan additionalcitationids=\"CR12\" citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. Furthermore, different kinds of polar materials such as metal oxides, metal sulfides etc. have also been demonstrated good modification materials because of their chemical interactions with lithium polysulfides[\u003cspan additionalcitationids=\"CR15 CR16 CR17 CR18 CR19\" citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eIn this work, we deliberately combined a commercial conductive carbon named BP2000 with Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e via a simple wet impregnation method followed by a high temperature calcination. The Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite is used as a separator coating layer in Li-S battery. The BP2000 constructs excellent conductive network to facilitate the charge transfers inside Li-S battery. Additionally, its rich porous structure is beneficial to adsorb a large amount of polysulfides. Furthermore, the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nano particles embedded in the pores of BP2000 not only have strong chemical interaction with lithium polysulfides, but also catalyze the chemical reactions during cycling. Benefit from its adsorption and catalytic ability, the loss of the active materials in the cathode can be greatly alleviated and the redox kinetics can be also accelerated, therefore the cycle and rate performance of Li-S battery are largely improved.\u003c/p\u003e"},{"header":"Experimental section","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Synthesis of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite\u003c/h2\u003e \u003cp\u003eFe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite was prepared by a simple impregnation method followed by a high temperature calcination. In a typical preparation process, 1.5g BP2000 was dispersed homogeneously by a mixture of 120 mL ultra pure water and 30 mL absolute ethyl alcohol. At the same time 0.5695 g Fe(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e•9H\u003csub\u003e2\u003c/sub\u003eO was dissolved completely in 10 mL ultra pure water. Then the Fe(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e•9H\u003csub\u003e2\u003c/sub\u003eO solution was added dropwisely into the BP2000 suspension, in this procedure Fe\u003csup\u003e3+\u003c/sup\u003e ion can be absorbed by the pores of BP2000. Afterwords, the BP2000 suspension was centrifugated and dried in an air blast drying oven. At last the dried powder was put into a tube furnace and calcined at 900°C for 2 h to obtain Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Fabrication of the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator\u003c/h2\u003e \u003cp\u003eThe Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator was prepared by a simple slurry coating method. Typically, 0.08g Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000, 0.01g super P and 0.01g PVDF were homogeneously dispersed in 4 mL NMP by vigorously stirring. The mixture was then coated onto the PE separator by a doctor blade. After the coating procedure, the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 coated PE separator was dried in an air blast drying oven and at last cut into small discs. For comparison purpose, BP2000 coated PE separator was also fabricated by the same procedures. The photo of the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 coated PE separator is shown in Figure \u003cspan refid=\"MOESM1\" class=\"InternalRef\"\u003eS1\u003c/span\u003e, and the cross section SEM demonstrates that the coating layer is approximately 10 µm.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Fabrication of BP2000/S cathode electrode\u003c/h2\u003e \u003cp\u003eIn a typical fabrication procedure, 1 g sublimed sulfur and 4 g BP2000 are mixed and dispersed in 30 mL absolute ethyl alcohol. Then the mixture was put into a 50 mL mill pot and ball milled at 900 r/min for 3 h. Afterwards, the sulfur and BP2000 mixture was dried and put into a vacuum oven and heated at 155°C for 10 h to obtain BP2000/S composite. To fabricate BP2000/S cathode electrode, 0.8 g BP2000/S composite, 0.1 g super P and 0.1 g PVDF were dispersed in 4 g NMP and stirred in a defoaming mixer at 2500 rpm for 3 min. The slurry was then spread onto Al foil and dried at 80°C for 10 h in a vacuum oven, at last the dried Al foil was cut into circle discs at wait for use, the sulfur area density on the cathode electrode was 3 mg cm\u003csup\u003e− 2\u003c/sup\u003e.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4 Cells assembly and electrochemical measurements\u003c/h2\u003e \u003cp\u003eBP2000/S cathode electrode, Li-S electrolyte (1 M LiTFSI with 0.1 M LiNO\u003csub\u003e3\u003c/sub\u003e dissolved in DOL/DME solvent), Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator and Li anode electrode are assembled into Li-S coin cells in an Ar filled glove box. The cycle and rate performances of the Li-S cells were tested by a LAND battery testing equipment, The cyclic voltammetry (CV) profiles and electrochemical impedance spectroscopy (EIS) curves were conducted via a VMP 3 electrochemical workstation.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e2.5 Materials characterization\u003c/h2\u003e \u003cp\u003eThe morphology and nano structure was characterized by field-emission scanning electron microscope (FESEM, NOVA Nano SEM 430) and transmission electron microscope (TEM, Tecnai G2 F20 S-TWIN). Crystal structure characterization were conducted by a X-ray diffractometer (XRD, Rigaku D/Max 2500). The porous structure and specific surface area was determined by a surface area analyzer.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"Results and discussions","content":"\u003cp\u003eFigure \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e shows the XRD patterns of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite. The XRD pattern of BP2000 shows two broad diffraction peaks at around 26° and 45°, refers to the (002) crystal plane of carbon. Furthermore, the XRD pattern of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite show obvious diffraction peaks at 18.3°, 30.2°, 35.6°, 37.2°, 43.3°, 53.7°, 57.3°, 62.9°, 71.3°, 74.5° and 77.4°, which match with the crystal faces of (111), (220), (311), (222), (400), (422), (511), (440), (620), (533) and (631) respectively, according to the PDF card JD39-1436 of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, demonstrating the successful preparation of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite[\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e \u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (a) and (b) show the SEM images of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite. The morphology of the two SEM images are approximately the same, demonstrating that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e are embedded in the pores of BP2000. In order to further investigate the micro structure of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, TEM analysis are carried out and the TEM images are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (c)-(f). Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (c) shows the TEM image of BP2000, the BP2000 nano particles are approximately 20–50 nm with abundant porous structure. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(d) and (e) shows that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nanoparticles are homogeneously dispersed in the pores of BP2000, furthermore, the HRTEM in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(f) clearly shows the lattice fringe of 0.25 nm which matches with the (311) face of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nanoparticles, which demonstrates that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nanoparticles are successfully embedded into the pores of BP2000.\u003c/p\u003e\u003cp\u003e \u003c/p\u003e\u003cp\u003eWe use N\u003csub\u003e2\u003c/sub\u003e adsorption - desorption experiment to estimate the BET specific surface area and pore size distribution of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e(a) shows the N\u003csub\u003e2\u003c/sub\u003e adsorption-desorption isotherms of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, both of the two isotherms display a type IV hysterrisis curve, demonstrating that BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite are composed of abundant micro and meso pores, which will be benefit for the adsorption for the lithium polysulfides. According to the BET calculation, the specific surface area of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite are 1229 and 1057 m\u003csup\u003e2\u003c/sup\u003e g\u003csup\u003e− 1\u003c/sup\u003e. The specific surface area of BP2000 decrease a little after the combination of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e, indicating that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e occupied some of the pores. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e(b) depicts the pore structures of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, both of the two materials are composed of pores form 2–10 nm, and most of the pore diameter are around 3.8 nm, the pore volumes of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite are 2.8 and 2.54 m\u003csup\u003e3\u003c/sup\u003e g\u003csup\u003e− 1\u003c/sup\u003e, the decrease of pore volume also demonstrates that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e particles are confined by the pores of BP2000. Additionally, the relatively small pore diameter can effectively absorb the soluble lithium polysulfides[\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e–\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e \u003c/p\u003e\u003cp\u003eIn order to directly demonstrate the absorption capability of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, a L\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e solution absorption experiment was carried out. A shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e(a), BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 were put into Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e solution and held for 8 h. The photo of Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e solution displays a dark yellow color, while the Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e-BP2000 solution displays a light yellow color demonstrating that Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e can be absorbed by BP2000. Furthermore, the Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e- Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 solution after 8 h absorption displays a transparent color which demonstrates that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 has an excellent absorption capability on lithium polysulfides. The Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e solution after absorption experiment was tested by UV spectroscopy, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e(b), the Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e UV-Vis absorption spectrum of Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e- Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 solution after 8 h absorption displays the lowest absorption peak, indicating its Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e concentration is also the lowest which is mostly absorbed by Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite[\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e–\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e \u003c/p\u003e\u003cp\u003eThe advantages of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator was further studied by electrochemical performances. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e(a), CV profiles of the three different batteries show apparently two reduction peaks at around 2.3 and 2.0 V and one oxidation peak at at around 2.4 V. The reduction peak at 2.3 V represents the reduction process of sulfur to soluble lithium polysulfides and the reduction peak at 2.0 V represents the reduction process of soluble lithium polysulfides to end product Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e2\u003c/sub\u003e/Li\u003csub\u003e2\u003c/sub\u003eS. The broad oxidation peak at around 2.4 V represents the gradual oxidation process of Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e2\u003c/sub\u003e/Li\u003csub\u003e2\u003c/sub\u003eS to sulfur. At the same time, the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator battery has the largest current density, indicating its capacity is also the largest. Additionally, the second reduction peak voltage of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 sample is a little bit higher than the BP2000 and PE separator sample, demonstrating it has a better reaction kinetics.\u003c/p\u003e\u003cp\u003eIn order to further demonstrate the catalytic effect of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite, a symmetric cell experiment was carried out. The assemble process of symmetric cell and its structure diagram is given in the support information. CV measurement results of symmetric cells are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e(b), as displayed in the figure, BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 symmetric cells with Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e electrolyte show obvious current peaks, while the current of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 symmetric cell without Li\u003csub\u003e2\u003c/sub\u003eS\u003csub\u003e6\u003c/sub\u003e electrolyte is nearly zero. Additionally, the current peak of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 symmetric cell is much larger than that of the BP2000 symmetric cell demonstrating the catalytic effect is mainly caused by the combination of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nano particles[\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e \u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(a) depicts the discharge/charge profiles of the three samples at 0.1 C, all the batteries show two typical discharge platforms and one charge platform which is consistent with the reduction and oxidation peaks of CV curves. Additionally, the potential gaps of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator batteries is apparently smaller which indicates the remarkably improved electrochemical kinetics. Long cycle performances were performed to evaluate the discharge/charge capacities and cycle stability of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator.\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(b) shows the long term cycle performances of different batteries. When the sulfur area density in the cathode is 3 mg cm\u003csup\u003e− 2\u003c/sup\u003e, the initial discharge capacities of PE, BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator batteries at 0.1 C are 986, 1280 and 1350 mAh g\u003csup\u003e− 1\u003c/sup\u003e respectively, as the current rate adds up to 0.5 C, the discharge capacities of the batteries are 650, 911 and 1140 mAh g\u003csup\u003e− 1\u003c/sup\u003e respectively. At the 200 cycles, the discharge capacity of the PE separator battery suffers a sharp decline and the battery can hardly release capacity. By comparison, the BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator batteries show a steady cycle performance for more than 500 cycles, furthermore the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 displays a much higher discharge capacity (500 mAh g\u003csup\u003e− 1\u003c/sup\u003e) at the 500 cycle than that of the BP2000 sample (320mAh g\u003csup\u003e− 1\u003c/sup\u003e). The higher discharge capacity of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 battery is mainly caused by the combination of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nano particles which can improve the absorption capability of lithium polysulfides.\u003c/p\u003e\u003cp\u003eThe rate performances of the PE, BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 samples are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(c). The discharge capacities of the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator battery at different current rates are much larger than that of the BP2000 separator battery and PE separator battery. Furthermore, the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator battery displays a highly reversible capacity of 1020 mAh g\u003csup\u003e− 1\u003c/sup\u003e at 1 C and gradually recovers to 1250 mAh g\u003csup\u003e− 1\u003c/sup\u003e as the current was set back to 0.1 C, indicating its fast redox reaction speed.\u003c/p\u003e\u003cp\u003eEIS curves of different separator batteries were collected before cycle. As displayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(d), the inset in the X axis are approximately the same demonstrating that the electrolyte environment are approximately the same. Furthermore, the diameter of the semicircle which represents the charge transfer resistance clearly indicates that the use of BP2000 and Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator can apparently decrease the internal resistance of the Li-S battery. This can be attributed to the low conductivity of BP2000. Additionally, the oblique line of Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 sample in the high frequency region shows the largest slop which indicates the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 separator has the fastest Li ion transportation speed which can accelerate the reaction speed[\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e–\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e].\u003c/p\u003e"},{"header":"Conclusion","content":"\u003cp\u003eIn summary, the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 was successfully prepared by a simple wet-impregnation followed by a high temperature treatment in N\u003csub\u003e2\u003c/sub\u003e atmosphere. XRD, SEM and TEM analysis demonstrate that Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nanoparticles with a diameter of 5–30 nm are homogeneously embedded in the pores of BP2000. Because of the rich porous structure of BP2000 as well as the abundant metallic active sites, the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 displays excellent absorption ability and catalytic effect on lithium polysulfides. At the high sulfur area density of 3 mg cm\u003csup\u003e− 2\u003c/sup\u003e, the Li-S battery using Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 coated separator has a high discharge capacity and can cycle stably for over 500 loops, which demonstrate its application potential.\u003c/p\u003e"},{"header":"Declarations","content":"\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eYi Lu: wrote the main manuscript textTao Liu: prepared figures\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eY. Cao, C. Wu, W. Wang, Y. Li, J. You, B. Zhang, J. Zou, S. Abuelgasim, T. Zhu, J. Wu, J. Zhao, Modification of lithium sulfur batteries by sieving effect: Long term investigation of carbon molecular sieve. J. Energy Storage. \u003cb\u003e54\u003c/b\u003e, 105228 (2022)\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eY. Li, Y. Zhou, Y. Muhammad, J. Zhou, Z. Guo, H. Tan, S. 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Lu, H. Zhang, Cation-doped ZnS catalysts for polysulfide conversion in lithium\u0026ndash;sulfur batteries. Nat. Catal. \u003cb\u003e5\u003c/b\u003e, 555\u0026ndash;563 (2022)\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-porous-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jopo","sideBox":"Learn more about [Journal of Porous Materials](http://link.springer.com/journal/10934)","snPcode":"10934","submissionUrl":"https://submission.nature.com/new-submission/10934/3","title":"Journal of Porous Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Fe2O3/BP2000, modified separator, shuttle effect, lithium polysulfides, lithium sulfur battery","lastPublishedDoi":"10.21203/rs.3.rs-3972507/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3972507/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eShuttle effect of lithium polysulfides in lithium sulfur batteries greatly influenced their commercialization. Therefore, it is urgent to develop a cheep and effective way to alleviate the shuttle effect. Fe is an active transition element which has good catalytic ability, in this work, a simple wet impregnation method was used to make Fe ions infiltrate into the pores of BP2000 (a kind of commercial conductive carbon), then it was calcined in N\u003csub\u003e2\u003c/sub\u003e atmosphere to get a Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 composite and used as a separator modification layer. The Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e nano particles are decorated in the pores of BP2000 which greatly enhanced the absorption ability on lithium polysulfides, additionally it also has excellent catalytic effect on lithium polysulfides, thus the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 layer can be served as a secondary collector to re-engage the polysulfides in the cathode reaction. In this way, the lithium sulfur batteries use the Fe\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/BP2000 modified separator show impressive electrochemical performances.\u003c/p\u003e","manuscriptTitle":"Fe 2 O 3 nano particles embedded Fe 2 O 3 /BP2000 composite for Li-S battery","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-04-03 07:29:36","doi":"10.21203/rs.3.rs-3972507/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-05-03T01:59:16+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-04-09T02:06:29+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-04-09T01:40:16+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-04-07T06:24:47+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"0ec7b269-d2a2-4b26-a410-c4b133dd85b1","date":"2024-04-07T03:37:43+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"1cd9d4d0-76f5-4e35-87a3-4f765435a974","date":"2024-04-05T21:47:19+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"b6bd0ec4-185f-446c-b67e-ffb77b675ce6","date":"2024-04-03T14:30:26+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"df1c9a23-aa08-46a6-950e-c65ab724f376","date":"2024-04-03T13:45:09+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-04-03T13:38:17+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2024-03-30T06:53:57+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2024-03-30T06:53:57+00:00","index":"","fulltext":""},{"type":"submitted","content":"Journal of Porous Materials","date":"2024-02-20T10:06:40+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"journal-of-porous-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"jopo","sideBox":"Learn more about [Journal of Porous Materials](http://link.springer.com/journal/10934)","snPcode":"10934","submissionUrl":"https://submission.nature.com/new-submission/10934/3","title":"Journal of Porous Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"b76c577b-1f72-4119-9d4b-0b66982c4d21","owner":[],"postedDate":"April 3rd, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2024-05-14T17:37:42+00:00","versionOfRecord":[],"versionCreatedAt":"2024-04-03 07:29:36","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-3972507","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3972507","identity":"rs-3972507","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}