CN104900902A - High-performance lithium sulfur battery - Google Patents
High-performance lithium sulfur battery Download PDFInfo
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- CN104900902A CN104900902A CN201510366630.5A CN201510366630A CN104900902A CN 104900902 A CN104900902 A CN 104900902A CN 201510366630 A CN201510366630 A CN 201510366630A CN 104900902 A CN104900902 A CN 104900902A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a high-performance lithium sulfur battery, in particular to a lithium sulfur battery with high specific capacity and long cycle life. The high-performance lithium sulfur battery has the advantages that shortcomings of complicated processes for manufacturing anode materials and membrane materials in existing lithium sulfur batteries and high costs of the existing lithium sulfur batteries can be overcome, the lithium sulfur battery is high in specific capacity, good in recycling performance and low in cost and is safe and nontoxic, and a process for manufacturing the high-performance lithium sulfur battery is mature.
Description
Technical field:
The present invention relates to a kind of high-performance lithium-sulfur cell, especially there is the lithium-sulfur cell of height ratio capacity and long circulation life.
Background technology:
Along with the fast development of science and technology, electronic equipment is widely used in the every field such as scientific research, life, amusement and traffic, and advanced electronic equipment is had higher requirement to energy demand.Current business-like anode material for lithium-ion batteries has LiFePO 4 (160-170mAh/g), cobalt acid lithium (140-160mAh/g), cobalt nickel ion doped (150-220mAh/g) and LiMn2O4 (110-120mAh/g), and this cannot meet the demand in future energy market.For this reason, people are using the lithium-sulfur cell of a new generation as a kind of high-performance secondary cell having development potentiality most, and it has lot of advantages: (1) high theoretical energy density 2600Wh/kg; (2) natural abundance of elementary sulfur in the earth's crust is large, cheap; (3) hypotoxicity, pollution-free.
However, the practical of lithium-sulfur cell is faced with many challenges: (1) elemental sulfur is high-insulation material, and at 25 DEG C, conductivity is about 5 × 10
-30s/cm, this causes sulphur to be difficult to, directly as positive electrode, to add conductive materials in positive pole; (2) in charge and discharge process, sulphur can react the long-chain lithium polysulphides (Li generating and be soluble in electrolyte
2s
x, 4<x≤8), shuttle back and forth to negative pole, on cathode of lithium surface, disproportionated reaction occurs and generate short-chain lithium polysulphides, short-chain lithium polysulphides shuttles back and forth back again positive pole, i.e. " effect of shuttling back and forth ", cause active material to lose, cycle performance declines, and is difficult to reach business-like standard.
For solving above-mentioned challenge, researcher has done many explorations, is mainly directed to design and the preparation of positive pole material with carbon element, adhesive, barrier film and electrolyte.
In positive pole modification, PVP is loaded in hollow carbon nano wire and obtains PVP-C composite material by Yi Cui, and be prepared into lithium sulfur battery anode material with elemental sulfur, obtain heavy-duty battery, discharge-rate is under 0.5C, after 100 circulations, specific discharge capacity is about 810mAh/g (Zheng G, Zhang Q, Cha J J, et al.Amphiphilic surface modification of hollow carbon nanofibers for improved cycle life of lithium-sulfur batteries [J] .Nano letters, 2013, 13 (3): 1265-1270), in diagram modification, Arumugan Manthirn is prepared into modified diaphragm common PP barrier film side coating MPC-PEG (microporous carbon-polyethylene glycol), use the lithium-sulfur cell of this modified diaphragm when discharge-rate is for 0.5C, after 200 circulations, specific discharge capacity is 795mAh/g (Chung S H, Manthiram A.A Polyethylene Glycol ?Supported Microporous Carbon Coating as a Polysulfide Trap for Utilizing Pure Sulfur Cathodes in Lithium – Sulfur Batteries [J] .Advanced Materials, 2014, 26 (43): 7352-7357), effectively improve chemical property.But above two kinds of preparation method's complexity, material expensive, and in charge and discharge process, still have more active material to lose, lithium-sulfur cell commercialization requirement cannot be met.
Summary of the invention:
The object of the invention is to overcome positive electrode in existing lithium-sulfur cell, diaphragm material complicated process of preparation, expensive defect, a kind of lithium-sulfur cell with height ratio capacity and good cycle is provided, and mature preparation process, safety non-toxic, cheap.
A kind of high-performance lithium-sulfur cell provided by the invention, be made up of positive pole, negative pole, barrier film and electrolyte, negative pole is metal lithium sheet, it is characterized in that: the sulphur positive pole being just very added with shitosan, its composition and mass ratio are elemental sulfur: conductive carbon: shitosan: adhesive is 40-70:40-24:10-3:10-3.
The particle size of described elemental sulfur is nanoscale or micron order.
Described shitosan is acid-soluble shitosan or water soluble chitosan.
Described adhesive is selected from the conventional adhesive such as gelatin, polyethylene glycol oxide (PEO), polyvinylpyrrolidone (PVP) or Kynoar (PVDF).
Described conductive carbon is selected from the conventional conductive carbon material such as acetylene black or superconductive carbon black.
The preparation method of sulphur positive pole is: in acetum shitosan being dissolved in 0.5-2wt% or deionized water, and forming concentration is the chitosan solution of 1-2wt%; Homogeneous phase mixing elemental sulfur, conductive carbon, chitosan solution and adhesive, make elemental sulfur: conductive carbon: shitosan: adhesive mass ratio is 40-70:40-24:10-3:10-3, and the slurry of formation is evenly coated on aluminium foil, as lithium sulfur battery anode material after drying.
High-performance lithium-sulfur cell of the present invention also can adopt chitin modified barrier film, and it consists of barrier film, conductive carbon, shitosan and adhesive.Wherein the mass ratio of conductive carbon, shitosan and adhesive is 60-90:20-5:20-5.
Described barrier film is various commercial barrier film known in this area, as PP barrier film etc.
Described shitosan is acid-soluble shitosan or water soluble chitosan.
Described adhesive is selected from the conventional adhesive such as gelatin, polyethylene glycol oxide (PEO), polyvinylpyrrolidone (PVP) or Kynoar (PVDF).
Described conductive carbon is selected from the conventional conductive carbon material such as acetylene black or superconductive carbon black.
The preparation method of modified diaphragm is: in acetum shitosan being dissolved in 0.5-2wt% or deionized water, and forming concentration is the chitosan solution of 1-2wt%; Homogeneous phase mixing conductive carbon, chitosan solution and adhesive, make the mass ratio of conductive carbon, shitosan and adhesive be 60-90:20-5:20-5, be coated on barrier film, as lithium-sulfur cell diaphragm material after drying by the slurry of formation.
High-performance lithium-sulfur cell provided by the invention, negative pole is metal lithium sheet; Electrolyte used with two (trimethyl fluoride sulfonyl) imine lithium for electrolyte, lithium nitrate is additive, and solvent is volume ratio is 1, the 3-dioxolane of 1:1 and the mixed solvent of dimethyl ether, wherein electrolytical concentration is 0.4-2mol/L, and the concentration of additive is 0.1-1mol/L.
The present invention is compared with all kinds of porous carbons/sulphur composite positive pole reported in existing document, anode prepared by the present invention and barrier film equal additive shitosan, containing a large amount of hydroxyl, amino and ehter bond in shitosan, these chemical bonds can effectively adsorb the long-chain lithium polysulphides generated in discharge process, improve the active material utilization of battery, specific discharge capacity and cycle life etc.In addition, shitosan preparation is simple, technical maturity, safety non-toxic, is easy to large-scale production, is conducive to accelerating commercialization process.
Accompanying drawing illustrates:
Fig. 1 is the circulation discharge curve of lithium-sulfur cell under discharge-rate is 0.5C of preparation in embodiment one.This figure shows, in embodiment one, the lithium-sulfur cell of preparation is under discharge-rate is 0.5C, and after 100 circulations, specific discharge capacity still has 680mAh/g, illustrates that it has good cycle performance.
Fig. 2 is the circulation discharge curve of lithium-sulfur cell under discharge-rate is 0.5C of preparation in embodiment six.This figure shows, in embodiment six, the lithium-sulfur cell of preparation is under discharge-rate is 0.5C, and after 100 circulations, specific discharge capacity still has 825mAh/g, illustrates that it has excellent cycle performance.
Embodiment:
Below by embodiment to the introduction specifically of the present invention's do, but protection scope of the present invention is not limited to cited embodiment.
Embodiment one
The first step: prepare positive electrode.
Compound concentration is the acetum of 2wt%, and acid-soluble shitosan is dissolved in this acetum, and forming concentration is the acidic chitosan solution of 2wt%, and acidic chitosan solution uses as additive.By elemental sulfur, acetylene black, chitosan solution and gelatin solution (2wt%) Homogeneous phase mixing, elemental sulfur, acetylene black, the mass ratio of shitosan and gelatin is 63:30:3.5:3.5.By mixture ball milling 5 hours in ball mill.The slurry formed evenly is coated on aluminium foil, and in vacuum drying chamber dry 10 hours.It is that the disk of 1.1cm is for subsequent use that the positive electrode of drying is cut into diameter.
Second step: assembling button lithium-sulfur cell.
With the positive electrode of preparation for anode, with polypropylene (PP) for barrier film, with lithium sheet for negative pole, choosing 0.6mol/L bis-(trimethyl fluoride sulfonyl) imine lithium is electrolyte, 0.4mol/L lithium nitrate does additive, solvent is 1,3-dioxolane and the dimethyl ether mixed solvent of volume ratio 1:1, is assembled into CR2025 button cell in the glove box of argon gas atmosphere.Discharge and recharge cut-ff voltage is respectively 2.8V and 1.7V, carries out charge and discharge cycles respectively under current density is 0.1C, 0.5C and 1C.Under 0.1C (1C=1675mAh/g), first discharge specific capacity is 1128mA/g, and under 0.5C, after 100 circulations, specific discharge capacity still remains on 680mAh/g.
Embodiment two
The first step: prepare positive electrode.
Compound concentration is the acetum of 1wt%, and acid-soluble shitosan is dissolved in this acetum, and forming concentration is the acidic chitosan solution of 1wt%, and acidic chitosan solution uses as additive.By elemental sulfur, acetylene black, chitosan solution and gelatin solution (2wt%) Homogeneous phase mixing, elemental sulfur, acetylene black, the mass ratio of shitosan and gelatin is 42:40:8:10.By mixture ball milling 5 hours in ball mill.The slurry formed evenly is coated on aluminium foil, and in vacuum drying chamber dry 10 hours.It is that the disk of 1.1cm is for subsequent use that the positive electrode of drying is cut into diameter.
Second step: assembling button lithium-sulfur cell.
With the positive electrode of preparation for anode, with polypropylene (PP) for barrier film, with lithium sheet for negative pole, choosing 1mol/L bis-(trimethyl fluoride sulfonyl) imine lithium is electrolyte, 0.5mol/L lithium nitrate does additive, solvent is 1,3-dioxolane and the dimethyl ether mixed solvent of volume ratio 1:1, is assembled into CR2025 button cell in the glove box of argon gas atmosphere.Discharge and recharge cut-ff voltage is respectively 2.8V and 1.7V, carries out charge and discharge cycles respectively under current density is 0.1C, 0.5C and 1C.Under 0.1C (1C=1675mAh/g), first discharge specific capacity is 1205mA/g, and under 0.5C, after 100 circulations, specific discharge capacity still remains on 670mAh/g.
Embodiment three
The first step: prepare positive electrode.
Be dissolved in by water soluble chitosan in deionized water, forming concentration is the chitosan solution of 1wt%.By elemental sulfur, acetylene black, chitosan solution and gelatin solution (2wt%) Homogeneous phase mixing, the mass ratio of elemental sulfur, acetylene black, shitosan and gelatin is 50:32:8:10.By mixture ball milling 5 hours in ball mill.The slurry formed evenly is coated on aluminium foil, and in vacuum drying chamber dry 10 hours.It is that the disk of 1.1cm is for subsequent use that the positive electrode of drying is cut into diameter.
Second step: assembling button lithium-sulfur cell.
With the positive electrode of preparation for anode, second step in the other the same as in Example 2.
Embodiment four
The first step: prepare diaphragm material
Compound concentration is the acetum of 1wt%, and acid-soluble shitosan is dissolved in this acetum, and forming concentration is the acidic chitosan solution of 1wt%, and acidic chitosan solution uses as additive.By acetylene black, chitosan solution and gelatin solution (2wt%) Homogeneous phase mixing, the mass ratio of acetylene black, shitosan and gelatin is made to be 80:10:10.Mixture is ground 5 hours in planetary ball mill.The slurry blade of formation is coated on polypropylene diaphragm (Celagrd 2320), and in vacuum drying chamber dry 10 hours.The diaphragm material of drying is cut into the disk that diameter is 1.9cm, and the amount containing active material is 0.2mg/cm
2, coat thickness is 1.5 μm, namely can be used as battery separator material, for subsequent use.
Second step: with the diaphragm material prepared for battery diaphragm, with the just very anode of preparation in embodiment three, with lithium sheet for negative pole, choosing 0.6mol/L bis-(trimethyl fluoride sulfonyl) imine lithium is electrolyte, 0.4mol/L lithium nitrate does additive, solvent is 1,3-dioxolane and the dimethyl ether mixed solvent of volume ratio 1:1, is assembled into CR2025 button cell in the glove box of argon gas atmosphere.Discharge and recharge cut-ff voltage is respectively 2.8V and 1.7V, is 0.1C (1C=1675mAh/g) respectively, carries out charge and discharge cycles under 0.5C and 1C in current density.Under 0.5C, after 100 circulations, specific discharge capacity still remains on 720mAh/g.
Embodiment five
The first step: prepare diaphragm material
Compound concentration is the acetum of 2wt%, and acid-soluble shitosan is dissolved in this acetum, and forming concentration is the acidic chitosan solution of 1.5wt%, and acidic chitosan solution uses as additive.By acetylene black, chitosan solution and gelatin solution (2wt%) Homogeneous phase mixing, the mass ratio of acetylene black, shitosan and gelatin is made to be 70:10:20.Mixture is ground 5 hours in planetary ball mill.The slurry blade of formation is coated on polypropylene diaphragm (Celagrd 2320), and in vacuum drying chamber dry 10 hours.The diaphragm material of drying is cut into the disk that diameter is 1.9cm, and the amount containing active material is 0.2mg/cm
2, coat thickness is 1.5 μm, namely can be used as battery separator material, for subsequent use.
Second step: with the diaphragm material prepared for battery diaphragm, with the just very anode of preparation in embodiment two, with lithium sheet for negative pole, choosing 0.6mol/L bis-(trimethyl fluoride sulfonyl) imine lithium is electrolyte, 0.4mol/L lithium nitrate does additive, solvent is 1,3-dioxolane and the dimethyl ether mixed solvent of volume ratio 1:1, is assembled into CR2025 button cell in the glove box of argon gas atmosphere.Discharge and recharge cut-ff voltage is respectively 2.8V and 1.7V, is 0.1C (1C=1675mAh/g) respectively, carries out charge and discharge cycles under 0.5C and 1C in current density.Under 0.5C, after 100 circulations, specific discharge capacity still remains on 740mAh/g.
Embodiment six
The first step: prepare diaphragm material.
Compound concentration is the acetum of 2wt%, and acid-soluble shitosan is dissolved in this acetum, and forming concentration is the acidic chitosan solution of 1.5wt%, and acidic chitosan solution uses as additive.By acetylene black, chitosan solution and gelatin solution (2wt%) Homogeneous phase mixing, the ratio of acetylene black, shitosan and gelatin is made to be 70:10:20.Mixture is ground 5 hours in planetary ball mill.The slurry blade of formation is coated on polypropylene diaphragm (Celagrd 2320), and in vacuum drying chamber dry 10 hours.The diaphragm material of drying is cut into the disk that diameter is 1.9cm, and the amount containing active material is 0.2mg/cm
2, coat thickness is 1.5 μm, namely can be used as battery separator material, for subsequent use.
Second step: with the just very anode of preparation in embodiment one, with the diaphragm material of preparation for battery diaphragm, with lithium sheet for negative pole, choosing 0.6mol/L bis-(trimethyl fluoride sulfonyl) imine lithium is electrolyte, 0.4mol/L lithium nitrate does additive, solvent is 1,3-dioxolane and the dimethyl ether mixed solvent of volume ratio 1:1, is assembled into CR2025 button cell in the glove box of argon gas atmosphere.Discharge and recharge cut-ff voltage is respectively 2.8V and 1.7V, carries out charge and discharge cycles respectively under current density is 0.1C, 0.5C and 1C.Under 0.5C (1C=1675mAh/g), after 100 circulations, specific discharge capacity still remains on 825mAh/g.
Claims (8)
1. a high-performance lithium-sulfur cell, is made up of positive pole, negative pole, barrier film, electrolyte, and negative pole is metal lithium sheet, it is characterized in that: the sulphur positive pole being just very added with shitosan.
2. high-performance lithium-sulfur cell according to claim 1, is characterized in that: the composition and the mass ratio that add the sulphur positive pole of shitosan are elemental sulfur: conductive carbon: shitosan: adhesive=40-70:40-24:10-3:10-3.
3. high-performance lithium-sulfur cell according to claim 2, is characterized in that: the particle size of described elemental sulfur is nanoscale or micron order; Shitosan is acid-soluble shitosan or water soluble chitosan; Adhesive is selected from gelatin, polyethylene glycol oxide, polyvinylpyrrolidone or Kynoar; Conductive carbon is selected from acetylene black or superconductive carbon black.
4. the high-performance lithium-sulfur cell according to claim 1 or 2 or 3, is characterized in that: the preparation method of sulphur positive pole is: in acetum shitosan being dissolved in 0.5-2wt% or deionized water, and forming concentration is the chitosan solution of 1-2wt%; Homogeneous phase mixing elemental sulfur, conductive carbon, chitosan solution and adhesive, make elemental sulfur, conductive carbon, shitosan and adhesive mass ratio be that the slurry that 40-70:40-24:10-3:10-3 is formed evenly is coated on aluminium foil, as sulphur positive pole after drying.
5. high-performance lithium-sulfur cell according to claim 1, it is characterized in that: the barrier film that high-performance lithium-sulfur cell adopts is chitin modified barrier film, modified diaphragm consist of barrier film, shitosan, adhesive and conductive carbon, wherein the mass ratio of conductive carbon, shitosan and adhesive is 60-90:20-5:20-5.
6. high-performance lithium-sulfur cell according to claim 5, is characterized in that: shitosan is acid-soluble shitosan or water soluble chitosan; Adhesive is selected from gelatin, polyethylene glycol oxide, polyvinylpyrrolidone or Kynoar; Conductive carbon is selected from acetylene black or superconductive carbon black.
7. the high-performance lithium-sulfur cell according to claim 5 or 6, is characterized in that: the preparation method of modified diaphragm is: in acetum shitosan being dissolved in 0.5-2wt% or deionized water, and forming concentration is the chitosan solution of 1-2wt%; Homogeneous phase mixing conductive carbon, chitosan solution and adhesive make the mass ratio of conductive carbon, shitosan and adhesive be 60-90:20-5:20-5, are coated on barrier film by the slurry of formation, obtained modified diaphragm after dry.
8. high-performance lithium-sulfur cell according to claim 1, it is characterized in that: electrolyte with two (trimethyl fluoride sulfonyl) imine lithium for electrolyte, lithium nitrate is additive, solvent is volume ratio is 1 of 1:1, the mixed solvent of 3-dioxolane and dimethyl ether, wherein electrolytical concentration is 0.4-2mol/L, and the concentration of additive is 0.1-1mol/L.
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Cited By (4)
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| CN107572486A (en) * | 2017-09-04 | 2018-01-12 | 北京化工大学 | A kind of nano-sulfur particles, preparation and its preparation of lithium-sulphur cell positive electrode |
| CN108155383A (en) * | 2017-11-29 | 2018-06-12 | 中山大学 | A kind of lithium-sulfur cell binding agent and preparation method thereof and lithium-sulphur cell positive electrode |
| CN109346647A (en) * | 2018-10-11 | 2019-02-15 | 中山大学 | A kind of preparation method and application of multi-functional lithium-sulfur cell diaphragm |
| CN114230836A (en) * | 2021-12-18 | 2022-03-25 | 河北金力新能源科技股份有限公司 | Modified lithium-sulfur battery diaphragm and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107572486A (en) * | 2017-09-04 | 2018-01-12 | 北京化工大学 | A kind of nano-sulfur particles, preparation and its preparation of lithium-sulphur cell positive electrode |
| CN107572486B (en) * | 2017-09-04 | 2020-05-19 | 北京化工大学 | Nano sulfur particles, preparation and preparation of lithium-sulfur battery positive electrode |
| CN108155383A (en) * | 2017-11-29 | 2018-06-12 | 中山大学 | A kind of lithium-sulfur cell binding agent and preparation method thereof and lithium-sulphur cell positive electrode |
| CN108155383B (en) * | 2017-11-29 | 2020-07-28 | 中山大学 | Binder for lithium-sulfur battery, preparation method of binder and lithium-sulfur battery anode |
| CN109346647A (en) * | 2018-10-11 | 2019-02-15 | 中山大学 | A kind of preparation method and application of multi-functional lithium-sulfur cell diaphragm |
| CN114230836A (en) * | 2021-12-18 | 2022-03-25 | 河北金力新能源科技股份有限公司 | Modified lithium-sulfur battery diaphragm and preparation method thereof |
| CN114230836B (en) * | 2021-12-18 | 2023-10-20 | 河北金力新能源科技股份有限公司 | Modified lithium-sulfur battery diaphragm and preparation method thereof |
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Application publication date: 20150909 |