CN113206344A - Functional diaphragm for lithium-sulfur battery and preparation method and application thereof - Google Patents
Functional diaphragm for lithium-sulfur battery and preparation method and application thereof Download PDFInfo
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- CN113206344A CN113206344A CN202010078337.XA CN202010078337A CN113206344A CN 113206344 A CN113206344 A CN 113206344A CN 202010078337 A CN202010078337 A CN 202010078337A CN 113206344 A CN113206344 A CN 113206344A
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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
Abstract
The invention discloses a functional diaphragm for a lithium-sulfur battery and a preparation method and application thereof, wherein the preparation method comprises the following steps: coating the first slurry on the positive electrode side of the base film to obtain a first coating layer, and coating the second slurry on the negative electrode side of the base film to form a second coating layer to obtain the functional diaphragm for the lithium-sulfur battery, wherein the preparation method of the first slurry comprises the following steps: mixing a dispersing agent and a first solvent, uniformly stirring, adding a carbon conductor and a first binder, uniformly stirring, and sanding to obtain a first slurry; the preparation method of the second slurry comprises the following steps: and adding unsaturated carboxylic acid and a second binder into a second solvent, and uniformly stirring to obtain a second slurry, wherein the unsaturated carboxylic acid is an acrylic acid. The preparation method can improve the ionic conductivity of the diaphragm, and is beneficial to reducing the polarization of the battery, thereby improving the rate capability of the battery.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to a functional diaphragm for a lithium-sulfur battery, and a preparation method and application thereof.
Background
The lithium-sulfur battery has the advantages of high energy density, high theoretical capacity and the like, and in addition, the rapid growth of the market is promoted by the characteristics of abundant and easily available raw materials, low cost and the like. However, the lithium-sulfur battery still has the problems of poor battery cycle performance, low rate performance and poor safety and stability performance, and the problems are closely related to the characteristics of the battery diaphragm.
The power lithium ion battery mainly comprises a positive electrode, a negative electrode, electrolyte, a diaphragm and a shell. The diaphragm plays a role in blocking the electronic conductance of positive and negative electrodes in the battery and allowing liquid ions to freely pass through, so that the ion conduction is realized, and the diaphragm is an important determinant factor of the battery, the cycle capacity and the safety performance.
During discharge, the sulfur on the positive electrode is discharged from the annular S8Lithium polysulphides (Li2Sx, x ═ 8, 6, 4 and 2) were converted into linear structures. In Li2S8、Li2S6、Li2S4And Li2S2Among lithium polysulfides, lithium polysulfides having a high sulfur oxidation number (Li2Sx, usually x)>4) Particularly easily dissolved in a hydrophilic electrolyte. Due to the concentration difference, lithium polysulfide dissolved in the electrolyte diffuses far from the positive electrode, i.e., a "shuttle effect" is generated. The "shuttle effect" causes lithium polysulfide to be lost from the positive electrode, so that active substances are reduced, the utilization rate of sulfur is reduced, and capacity is reduced. The pore structure of the traditional lithium battery diaphragm can not effectively prevent lithium polysulfide from shuttling, and in addition, the defects of low hydrophobicity, low polarity, low surface energy and the like of the traditional diaphragm cause low liquid absorption rate and poor liquid retention of the diaphragm, thereby further causing low ionic conductivity and influencing the performance of the battery.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a preparation method of a functional diaphragm for a lithium-sulfur battery.
Another object of the present invention is to provide a functional separator for a lithium-sulfur battery obtained by the above preparation method.
The purpose of the invention is realized by the following technical scheme.
A method for preparing a functional separator for a lithium-sulfur battery includes the following steps:
coating a first slurry on a positive electrode side of a base film to obtain a first coating layer on the base film, coating a second slurry on a negative electrode side of the base film to form a second coating layer to obtain the functional separator for a lithium-sulfur battery,
the preparation method of the first slurry comprises the following steps: mixing a dispersing agent and a first solvent, uniformly stirring, adding a carbon conductor and a first binder, uniformly stirring, and sanding to obtain the first slurry, wherein the dispersing agent is one or a mixture of more than two of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol, the carbon conductor is graphene, Super-p or carbon black, and the first binder is PVDF (polyvinylidene fluoride) or polyacrylates;
the preparation method of the second slurry comprises the following steps: and adding unsaturated carboxylic acid and a second binder into a second solvent, and uniformly stirring to obtain the second slurry, wherein the unsaturated carboxylic acid is an acrylic acid, and the second binder is polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) or polyethylene oxide (PEO).
In the technical scheme, the first solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is (1-20) in parts by mass: 1, preferably (1-15): 1.
in the technical scheme, the second solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is (1-15) in parts by mass: (1-6), preferably (1-10): (1-5).
In the technical scheme, the acrylic acid is acrylic acid, crotonic acid or octadecenoic acid.
In the technical scheme, the dispersant accounts for 0.5-7 wt% of the first solvent.
In the technical scheme, the ratio of the carbon conductor to the first binder is (10-90) by mass: (0.5-5).
In the above technical solution, the sum of the mass of the carbon-based conductor and the first binder is 1 to 25 wt% of the sum of the mass of the dispersant and the mass of the first solvent.
In the above technical scheme, in the preparation method of the first slurry, the stirring time is 10-40 min.
In the technical scheme, the sanding time is 20-60 min.
In the technical scheme, the coating mode is roll coating.
In the technical scheme, the thickness of the first coating is 1-8 micrometers.
In the technical scheme, the ratio of the unsaturated carboxylic acid to the second binder is (25-60) in parts by mass: (0.2-4).
In the technical scheme, the mass sum of the unsaturated carboxylic acid and the second binder is 3-20 wt% of the second solvent.
In the above technical scheme, in the preparation method of the second slurry, the stirring time is 10-50 min.
In the technical scheme, the thickness of the second coating is 1-8 microns.
In the above technical scheme, the base film is a polyolefin film, and the polyolefin film is a polyethylene film or a polypropylene film.
The functional separator for a lithium-sulfur battery obtained by the above preparation method.
The functional diaphragm for the lithium-sulfur battery is applied to improving the capacity retention rate and/or the coulombic efficiency of the lithium-sulfur battery.
The invention has the following beneficial effects:
according to the invention, the functional layer is introduced into the surface of the polyolefin film, on the one hand, a nuclear negative electricity network formed by unsaturated carboxylic acid can inhibit the polysulfide with electronegativity from diffusing to the negative electrode through the separator. Meanwhile, the existence of the carbon conductor is beneficial to polysulfide to carry out redox reaction, so that high sulfide is reduced into low sulfide, and the low sulfide is not dissolved in electrolyte, so that shuttle effect cannot be generated. Namely, the generation of polysulfide can be prevented, and the shuttle effect is avoided; on the other hand, the lithium ion transference number of the diaphragm is improved, so that the ion conductivity of the diaphragm can be improved, the polarization of the battery is favorably reduced, and the rate capability of the battery is improved.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The sanding equipment is full ceramic nanometer grinding machine, model: PT-5L, a Producer of Dongguan City Deno mechanical Equipment Co., Ltd
The mixer is double planet power mixer, the model: HY-DLH43L, manufacturer: guangzhou Hongyang mechanical science and technology Co Ltd
Example 1
A method for preparing a functional separator for a lithium-sulfur battery includes the following steps:
and coating the first slurry on the positive electrode side of the base film to obtain a first coating layer, coating the second slurry on the negative electrode side of the base film to form a second coating layer to obtain the functional diaphragm for the lithium-sulfur battery, wherein the coating mode is roller coating, the thickness of the first coating layer is 2 micrometers, the thickness of the second coating layer is 2 micrometers, and the base film is a polyethylene film.
The preparation method of the first slurry comprises the following steps: mixing a dispersing agent and a first solvent, wherein the dispersing agent is 5 wt% of the first solvent, stirring for 20min to be uniform, adding a carbon conductor and a first binder, stirring for 20min to be uniform, and sanding for 20min to obtain a first slurry, wherein the ratio of the carbon conductor to the first binder is 12: 0.6, the sum of the mass of the carbon-based conductor and the first binder is 7 wt% of the sum of the mass of the dispersant and the first solvent. The first solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 3: 1; the dispersant is polyacrylic ammonium salt, the carbon conductor is carbon black, and the carbon conductor can form reduction sites for sulfur ions to prevent polysulfide from being generated. The first binder is PVDF (polyvinylidene fluoride).
The preparation method of the second slurry comprises the following steps: adding unsaturated carboxylic acid and a second binder into a second solvent, and stirring for 10min to be uniform to obtain a second slurry, wherein the ratio of the unsaturated carboxylic acid to the second binder is 10: 1, the sum of the mass of the unsaturated carboxylic acid and the second binder is 4 wt% of the second solvent. The second solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 1: 1. the unsaturated carboxylic acid is acrylic acid, and the polysulfide having electronegativity can be inhibited from diffusing into the negative electrode through the separator by a negative nuclear network formed by the unsaturated carboxylic acid. The carboxyl contained in the unsaturated carboxylic acid can promote the dissociation of lithium salt, increase the number of free ions and be beneficial to improving the ionic conductivity of the diaphragm; in addition, the charge negative electric network also provides a quick channel for the migration of lithium ions, improves the lithium ion migration number of the diaphragm, and is beneficial to reducing the polarization of the battery, thereby improving the rate capability of the battery. The second binder is polyvinylpyrrolidone (PVP).
Example 2
A method for preparing a functional separator for a lithium-sulfur battery includes the following steps:
and coating the first slurry on the positive electrode side of the base film to obtain a first coating layer, and coating the second slurry on the negative electrode side of the base film to form a second coating layer to obtain the functional diaphragm for the lithium-sulfur battery, wherein the coating mode is roller coating, the thickness of the first coating layer is 2.5 micrometers, the thickness of the second coating layer is 2 micrometers, and the base film is a polyethylene film.
The preparation method of the first slurry comprises the following steps: mixing a dispersing agent and a first solvent, wherein the dispersing agent is 5 wt% of the first solvent, stirring for 30min to be uniform, adding a carbon conductor and a first binder, stirring for 30min to be uniform, and sanding for 36min to obtain a first slurry, wherein the ratio of the carbon conductor to the first binder is 30: 2.5, the sum of the mass of the carbon-based conductor and the first binder is 10 wt% of the sum of the mass of the dispersant and the first solvent. The first solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 9: 1; the dispersing agent is trimethyl ammonium hydrochloride, the carbon conductor is graphene, and the first binder is polymethyl acrylate.
The preparation method of the second slurry comprises the following steps: adding unsaturated carboxylic acid and a second binder into a second solvent, and stirring for 10min until the mixture is uniform to obtain a second slurry, wherein the ratio of the unsaturated carboxylic acid to the second binder is 25: 2, the mass sum of the unsaturated carboxylic acid and the second binder is 7 wt% of the second solvent. The second solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 3: 1. the unsaturated carboxylic acid is crotonic acid. The second binder is polyvinyl alcohol (PVA).
Example 3
A method for preparing a functional separator for a lithium-sulfur battery includes the following steps:
and coating the first slurry on the positive electrode side of the base film to obtain a first coating layer, coating the second slurry on the negative electrode side of the base film to form a second coating layer to obtain the functional diaphragm for the lithium-sulfur battery, wherein the coating mode is roller coating, the thickness of the first coating layer is 3 micrometers, the thickness of the second coating layer is 2 micrometers, and the base film is a polypropylene film.
The preparation method of the first slurry comprises the following steps: mixing a dispersing agent and a first solvent, wherein the dispersing agent is 5 wt% of the first solvent, stirring for 40min to be uniform, adding a carbon conductor and a first binder, stirring for 40min to be uniform, and sanding for 40min to obtain a first slurry, wherein the ratio of the carbon conductor to the first binder is 10: 3, the sum of the mass of the carbon-based conductor and the first binder is 15 wt% of the sum of the mass of the dispersant and the first solvent. The first solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 15: 1; the dispersing agent is polyethylene glycol, the carbon conductor is Super-p, and the first adhesive is polyethylacrylate.
The preparation method of the second slurry comprises the following steps: adding unsaturated carboxylic acid and a second binder into a second solvent, and stirring for 10min until the mixture is uniform to obtain a second slurry, wherein the ratio of the unsaturated carboxylic acid to the second binder is 15: 2, the sum of the mass of the unsaturated carboxylic acid and the second binder is 12 wt% of the second solvent. The second solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is 9: 4. the unsaturated carboxylic acid is octadecenoic acid. The second binder is polyethylene oxide (PEO).
The functional separator for lithium sulfur batteries obtained in examples 1 to 3 was tested as follows:
the decomposition voltage of the functional separator for lithium-sulfur battery obtained in example 1 was 4.7V, 12The thermal shrinkage rate of 1.0 percent at 0 ℃ for 1 hour and the tensile strength of 1450Kg/cm2Ion conductivity: 1.4X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 98% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.23% after the battery is cycled for 20 circles.
The decomposition voltage of the functional separator for a lithium-sulfur battery obtained in example 2 was 4.7V, the thermal shrinkage at 120 ℃ for 1 hour was 1.2%, and the tensile strength was 1490Kg/cm2Ion conductivity: 1.5X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 97% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 98.48% after the battery is cycled for 20 circles.
The decomposition voltage of the functional separator for a lithium-sulfur battery obtained in example 3 was 4.7V, the thermal shrinkage at 120 ℃ for 1 hour was 0.9%, and the tensile strength was 1550Kg/cm2Ion conductivity: 1.3X 10-3s/cm-1. The sulfur positive electrode and the lithium negative electrode are adopted to assemble the battery, the capacity retention rate is 97% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 97.57% 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 functional diaphragm for a lithium-sulfur battery is characterized by comprising the following steps:
coating a first slurry on a positive electrode side of a base film to obtain a first coating layer on the base film, coating a second slurry on a negative electrode side of the base film to form a second coating layer to obtain the functional separator for a lithium-sulfur battery,
the preparation method of the first slurry comprises the following steps: mixing a dispersing agent and a first solvent, uniformly stirring, adding a carbon conductor and a first binder, uniformly stirring, and sanding to obtain the first slurry, wherein the dispersing agent is one or a mixture of more than two of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol, the carbon conductor is graphene, Super-p or carbon black, and the first binder is PVDF or polyacrylate;
the preparation method of the second slurry comprises the following steps: and adding unsaturated carboxylic acid and a second binder into a second solvent, and uniformly stirring to obtain the second slurry, wherein the unsaturated carboxylic acid is an acrylic acid, and the second binder is polyvinylpyrrolidone, polyvinyl alcohol or polyethylene oxide.
2. The preparation method according to claim 1, wherein the dispersant is 0.5 to 7 wt% of the first solvent;
the ratio of the carbon conductor to the first binder is (10-90) in parts by mass: (0.5 to 5);
the mass sum of the carbon conductor and the first binder is 1-25 wt% of the mass sum of the dispersant and the first solvent;
the ratio of the unsaturated carboxylic acid to the second binder is (25-60) in parts by mass: (0.2-4); the mass sum of the unsaturated carboxylic acid and the second binder is 3-20 wt% of the second solvent.
3. The preparation method according to claim 2, wherein the second solvent is a mixture of water and alcohol, and the ratio of water to alcohol is (1-15) in parts by mass: (1-6), preferably (1-10): (1-5); the first solvent is a mixture of water and alcohol, and the ratio of the water to the alcohol is (1-20) in parts by mass: 1, preferably (1-15): 1.
4. the method according to claim 3, wherein the acrylic acid is acrylic acid, crotonic acid or octadecenoic acid.
5. The method of claim 4, wherein the first coating layer has a thickness of 1 to 8 μm; the thickness of the second coating is 1-8 microns.
6. The method according to claim 5, wherein in the method for preparing the first slurry, the stirring time is 10 to 40 min; the sanding time is 20-60 min; in the preparation method of the second slurry, the stirring time is 10-50 min.
7. The method according to claim 6, wherein the coating is performed by roll coating.
8. The production method according to claim 7, wherein the base film is a polyolefin film, and the polyolefin film is a polyethylene film or a polypropylene film.
9. The functional separator for a lithium-sulfur battery obtained by the production method according to any one of claims 1 to 8.
10. Use of the functional separator for lithium-sulfur battery according to claim 9 for improving the capacity retention and/or coulombic efficiency of lithium-sulfur battery.
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