CN111916616A - Composite diaphragm for lithium-sulfur battery and preparation method and application thereof - Google Patents
Composite diaphragm for lithium-sulfur battery and preparation method and application thereof Download PDFInfo
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- CN111916616A CN111916616A CN201910381903.1A CN201910381903A CN111916616A CN 111916616 A CN111916616 A CN 111916616A CN 201910381903 A CN201910381903 A CN 201910381903A CN 111916616 A CN111916616 A CN 111916616A
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a composite diaphragm for a lithium-sulfur battery, and a preparation method and application thereof, wherein the preparation method comprises the following steps: coating aramid fiber slurry on one side of a base film to obtain an aramid fiber coating layer on the base film; coating a second slurry on the aramid fiber coating layer to obtain the composite diaphragm for the lithium-sulfur battery, wherein the preparation method of the aramid fiber slurry comprises the following steps: adding a dispersing agent into a first solvent under the condition of stirring, and then adding aramid fiber, a second solvent, an emulsifier and an adhesive to obtain aramid fiber slurry, wherein the preparation method of the second slurry comprises the following steps: and uniformly mixing the carbon conductor and the lithium conducting polymer, adding a third solvent, a polymer binder and a wetting agent, and uniformly stirring to obtain a second slurry. According to the invention, the aramid fiber slurry is coated on the surface of the base film, so that the heat resistance and the mechanical property of the base film are improved, and the cycle service life of the base film is prolonged.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to a composite diaphragm for a lithium-sulfur battery, and a preparation method and application thereof.
Background
In recent years, the application range of lithium ion batteries is becoming wider and wider, and thus, the demand for lithium ion batteries is also becoming higher and higher. The elemental sulfur has extremely high theoretical capacity and energy density, and has a series of advantages of no toxicity, environmental friendliness, wide raw material source, low cost and the like. Therefore, lithium sulfur batteries are considered to be the most promising energy storage system currently. However, due to the problems of solvent shuttle of the S positive electrode, dendritic growth of the metal Li negative electrode, and low flash point of the ether electrolyte, the lithium-sulfur battery still faces the challenges of high safety, long service life and high specific energy which are difficult to be coordinated, and the commercialization process of the lithium-sulfur battery is severely restricted.
The separator, as one of the important materials of lithium ion batteries, is an important determinant factor of battery capacity, cycle capacity and safety performance. Traditional lithium battery diaphragm adopts micropore polyethylene or polypropylene membrane more, but simple polyolefin diaphragm has thermal stability not good, easily arouses the battery safety problem, and to lithium sulphur battery, the produced lithium sulphur polymer of charge-discharge can be through this type diaphragm, can exert an influence to the cyclicity and the coulombic efficiency of battery. Therefore, the development of a high-performance composite separator of other materials and polyolefin to enhance the thermal stability and simultaneously enable the high-performance composite separator to have the functions of sulfur interception and lithium conduction becomes an important aspect for promoting the development of lithium-sulfur batteries.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a composite diaphragm for a lithium-sulfur battery.
Another object of the present invention is to provide a composite separator for a lithium sulfur battery obtained by the above preparation method.
Another object of the present invention is to provide a use of a composite separator for a lithium sulfur battery for reducing the thermal shrinkage of the separator.
The invention also aims to provide application of the composite diaphragm for the lithium-sulfur battery in improving tensile strength of the diaphragm.
It is another object of the present invention to provide the use of a composite separator for a lithium sulfur battery to increase the cycle life of the battery.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a composite diaphragm for a lithium-sulfur battery comprises the following steps:
step 1, coating aramid fiber slurry on one side of a base film in a thickness of 0.5-2 microns, soaking for 3-15 seconds, and drying to obtain an aramid fiber coating layer on the base film;
step 2, coating a second sizing agent on the aramid fiber coating layer in a thickness of 0.5-4 mu m, drying to obtain the composite diaphragm for the lithium-sulfur battery, wherein,
the preparation method of the aramid fiber slurry comprises the following steps: adding a dispersing agent into a first solvent under the condition of stirring, adding aramid fiber, a second solvent, an emulsifier and an adhesive after uniformly stirring, and uniformly stirring to obtain aramid fiber slurry, wherein the ratio of the first solvent to the dispersing agent to the aramid fiber to the second solvent to the emulsifier to the adhesive is (50-80): (0.05-3): (2-8): (5-30): (0.5-2): (0.5 to 3); the first solvent is N-methyl pyrrolidone (NMP), dimethyl sulfoxide (DMSO), dimethyl formamide (DMF) or dimethyl acetamide (DMAC), the dispersing agent is triethyl phosphate, the second solvent is ethanol, isopropanol or dichloromethane, the emulsifier is polyvinyl alcohol, sodium polyacrylate or polyacrylamide, and the adhesive is one or a mixture of polyethylene oxide, cinnamic acid, sodium hydroxymethyl cellulose and polyurethane;
the preparation method of the second slurry comprises the following steps: uniformly mixing a carbon conductor and a lithium conducting polymer, adding a third solvent, uniformly mixing, adding a polymer binder and a wetting agent, and uniformly stirring to obtain the second slurry, wherein the third solvent is a mixture of water and ethanol, and the ratio of water to ethanol in the third solvent is (1-10): 1; the ratio of the carbon conductor, the lithium conducting polymer, the third solvent, the polymer binder and the wetting agent is (0.5-2): (1-6): (80-200): (0.05-2): (0.1-2), the carbon conductor is graphite, the lithium conducting polymer is one or more of polyacrylic acid, sulfonated polyether sulfone and polymethyl methacrylate, the polymer binder is polyacrylate, and the wetting agent is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, mercaptan, hydrazide, mercaptan acetal and polyoxyethylene alkylated ether.
In the above technical solution, the base film is a polyolefin film.
In the above technical scheme, the aramid fiber is meta-aramid fiber or para-aramid fiber.
In the technical scheme, the molecular weight of the aramid fiber is 0.5-10 ten thousand.
In the above technical scheme, the graphite is graphene, natural graphite or artificial graphite.
In the technical scheme, the drying temperature is 40-80 ℃, and the drying time is 0.1-40 s.
In the technical scheme, the ratio of the first solvent to the dispersing agent to the aramid fiber to the second solvent to the emulsifier to the binder is (50-75): (0.5-1.5): (2-6): (5-25): (0.7-1): (1-2).
In the technical scheme, the ratio of the carbon conductor, the lithium conducting polymer, the third solvent, the polymer binder and the wetting agent is (0.5-2): (2-6): (80-180): (0.5-1.5): (0.4-1.5).
The composite diaphragm for the lithium-sulfur battery obtained by the preparation method.
The composite diaphragm for the lithium-sulfur battery is applied to reducing the thermal shrinkage rate of the diaphragm.
The composite diaphragm for the lithium-sulfur battery is applied to improving the tensile strength of the diaphragm.
The composite diaphragm for the lithium-sulfur battery is applied to prolonging the cycle service life of the battery.
According to the invention, the aramid fiber slurry is coated on the surface of the base film, so that the heat resistance and the mechanical property of the base film are improved, and the cycle service life of the base film is prolonged.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The medicine purchase source is sold in the market.
The high-speed dispersion machine manufacturer is Ningde Jiatuo intelligent equipment Limited company, and the rotating speed is 1000 r/min;
the mixer is double planet power mixer, the model: HY-DLH43L, manufacturer: the rotational speed of the stirrer is 1200 rpm, Guangzhou Hongshang mechanical science and technology company;
the sand mill is a full ceramic nanometer grinding machine, and has the model: PT-5L, the manufacturer is a Noo mechanical equipment Co., Ltd, available from Dongguan;
test equipment for voltage decomposition: withstand voltage insulation analyzer, model: AN9636HS, manufacturer: tsingapore Evoo;
test equipment for heat shrinkage: a high temperature test chamber;
in the following embodiments, the aramid fiber is meta-aramid fiber, and the molecular weight of the meta-aramid fiber is 0.5 to 10 ten thousand.
Examples 1 to 4
A preparation method of a composite diaphragm for a lithium-sulfur battery comprises the following steps:
step 1, coating aramid fiber slurry on one side of a polyolefin film by a roller with the thickness of 1 mu m, taking the side as a positive electrode side, soaking in water for 10s, drying at 70 ℃ for 0.5s, and obtaining an aramid fiber coating layer on the polyolefin film;
step 2, coating a second sizing agent (coating method: roller coating) on the aramid fiber coating layer in a thickness of 1 mu m, and drying at 70 ℃ for 0.5s to obtain the composite diaphragm for the lithium-sulfur battery;
the preparation method of the aramid fiber slurry comprises the following steps: slowly and uniformly adding a dispersing agent into a first solvent under the stirring condition, wherein the dispersing agent is triethyl phosphate, stirring for 1 hour by using a high-speed dispersion machine, adding aramid fibers, stirring for 2 hours by using a stirring machine, adding a second solvent and an emulsifying agent, dispersing for 2 hours by using the high-speed dispersion machine, adding an adhesive after dispersing, and dispersing for 2 hours at a high speed by using a sand mill to obtain aramid fiber slurry; the mass ratio of the first solvent, the dispersant, the aramid fiber, the second solvent, the emulsifier, and the binder is defined as a first slurry material ratio, and the first slurry material ratio is shown in table 1.
The preparation method of the second slurry comprises the following steps: uniformly mixing graphene and a lithium conducting polymer, adding a third solvent, stirring for 3 hours by using a high-speed dispersion machine, adding a polymer binder and a wetting agent under the stirring condition after dispersion, and stirring for 2 hours to be uniform by using a sand mill to obtain a second slurry, wherein the polymer binder is polymethyl acrylate;
the third solvent is a mixture of water and ethanol, and the ratio of the water to the ethanol in the third solvent is 3:1 in parts by volume; the mass ratio between the graphene, the lithium conducting polymer, the third solvent, the polymer binder and the wetting agent is defined as a second slurry material ratio, and the second slurry material ratio is shown in table 1.
The raw materials in examples 1 to 4 are shown in Table 1.
TABLE 1
The composite separator for a lithium-sulfur battery obtained in example 1 had a decomposition voltage of 4.7V, a thermal shrinkage of 0.35% at 130 ℃ for 1 hour, and a tensile strength of 1980Kg/cm2. The battery is assembled by adopting sulfur as a positive electrode and a lithium sheet as a negative electrode, the capacity retention rate is 79% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.74% after the battery is cycled for 20 circles.
The composite separator for a lithium-sulfur battery obtained in example 2 had a decomposition voltage of 4.8V, a heat shrinkage of 0.6% at 130 ℃ for 1 hour, and a tensile strength of 1920Kg/cm2. The battery is assembled by adopting sulfur as a positive electrode and a lithium sheet as a negative electrode, the capacity retention rate is 76.2% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.5% after the battery is cycled for 20 circles.
The composite separator for a lithium-sulfur battery obtained in example 3 had a decomposition voltage of 4.7V, a thermal shrinkage of 0.57% at 130 ℃ for 1 hour, and a tensile strength of 1975Kg/cm2. The battery is assembled by adopting sulfur as a positive electrode and a lithium sheet as a negative electrode, the capacity retention rate is 78% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.2% after the battery is cycled for 20 circles.
The composite separator for a lithium-sulfur battery obtained in example 4 had a decomposition voltage of 4.9V, a heat shrinkage at 130 ℃ for 1 hour of 0.64%, and a tensile strength of 1925Kg/cm2. The battery is assembled by adopting sulfur as a positive electrode and a lithium sheet as a negative electrode, the capacity retention rate is 80% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.5% after the battery is cycled for 20 circles.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. A preparation method of a composite diaphragm for a lithium-sulfur battery is characterized by comprising the following steps:
step 1, coating aramid fiber slurry on one side of a base film in a thickness of 0.5-2 microns, soaking for 3-15 seconds, and drying to obtain an aramid fiber coating layer on the base film;
step 2, coating a second sizing agent on the aramid fiber coating layer in a thickness of 0.5-4 mu m, drying to obtain the composite diaphragm for the lithium-sulfur battery, wherein,
the preparation method of the aramid fiber slurry comprises the following steps: adding a dispersing agent into a first solvent under the condition of stirring, adding aramid fiber, a second solvent, an emulsifier and an adhesive after uniformly stirring, and uniformly stirring to obtain aramid fiber slurry, wherein the ratio of the first solvent to the dispersing agent to the aramid fiber to the second solvent to the emulsifier to the adhesive is (50-80): (0.05-3): (2-8): (5-30): (0.5-2): (0.5 to 3); the first solvent is N-methyl pyrrolidone, dimethyl sulfoxide, dimethylformamide or dimethylacetamide, the dispersing agent is triethyl phosphate, the second solvent is ethanol, isopropanol or dichloromethane, the emulsifying agent is polyvinyl alcohol, sodium polyacrylate or polyacrylamide, and the adhesive is one or a mixture of polyethylene oxide, phenylacrylic acid, sodium hydroxymethyl cellulose and polyurethane;
the preparation method of the second slurry comprises the following steps: uniformly mixing a carbon conductor and a lithium conducting polymer, adding a third solvent, uniformly mixing, adding a polymer binder and a wetting agent, and uniformly stirring to obtain the second slurry, wherein the third solvent is a mixture of water and ethanol, and the ratio of water to ethanol in the third solvent is (1-10): 1; the ratio of the carbon conductor, the lithium conducting polymer, the third solvent, the polymer binder and the wetting agent is (0.5-2): (1-6): (80-200): (0.05-2): (0.1-2), the carbon conductor is graphite, the lithium conducting polymer is one or more of polyacrylic acid, sulfonated polyether sulfone and polymethyl methacrylate, the polymer binder is polyacrylate, and the wetting agent is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, mercaptan, hydrazide, mercaptan acetal and polyoxyethylene alkylated ether.
2. The production method according to claim 1, wherein the graphite is graphene, natural graphite, or artificial graphite.
3. The method according to claim 2, wherein the drying temperature is 40 to 80 ℃ and the drying time is 0.1 to 40 seconds.
4. The preparation method of claim 3, wherein the ratio of the first solvent, the dispersing agent, the aramid fiber, the second solvent, the emulsifier and the binder is (50-75) in parts by mass: (0.5-1.5): (2-6): (5-25): (0.7-1): (1-2).
5. The preparation method according to claim 4, wherein the ratio of the carbon-based conductor, the lithium conducting polymer, the third solvent, the polymer binder and the wetting agent is (0.5-2): (2-6): (80-180): (0.5-1.5): (0.4-1.5).
6. The preparation method of claim 5, wherein the base film is a polyolefin film, the aramid fiber is meta-aramid fiber or para-aramid fiber, and the molecular weight of the aramid fiber is 0.5-10 ten thousand.
7. The composite separator for a lithium-sulfur battery obtained by the production method according to claims 1 to 6.
8. Use of the composite separator for lithium sulfur battery according to claim 7 for reducing the thermal shrinkage of the separator.
9. Use of the composite separator for lithium sulfur battery according to claim 7 for improving tensile strength of the separator.
10. Use of a composite separator for a lithium sulfur battery according to claim 7 to increase the cycle life of the battery.
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Cited By (1)
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| CN112909425A (en) * | 2021-01-20 | 2021-06-04 | 河北金力新能源科技股份有限公司 | High-efficiency long-life lithium-sulfur battery diaphragm and preparation method thereof |
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Application publication date: 20201110 |