CN110556494A - High-conductivity slurry for lithium-sulfur battery, and separator and application based on high-conductivity slurry - Google Patents
High-conductivity slurry for lithium-sulfur battery, and separator and application based on high-conductivity slurry Download PDFInfo
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- CN110556494A CN110556494A CN201910780415.8A CN201910780415A CN110556494A CN 110556494 A CN110556494 A CN 110556494A CN 201910780415 A CN201910780415 A CN 201910780415A CN 110556494 A CN110556494 A CN 110556494A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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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
- 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
- H01M50/411—Organic 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
- 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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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 high-conductivity slurry for a lithium-sulfur battery, a diaphragm based on the high-conductivity slurry and application of the high-conductivity slurry, wherein the preparation method of the high-conductivity slurry for the lithium-sulfur battery comprises the following steps: mixing water and ethanol, adding a dispersing agent, uniformly stirring to obtain a first mixed solution, mixing a second mixed solution with the first mixed solution, uniformly stirring, and then placing the mixture into a sand mill for sand milling for 30-90 min to obtain the high-conductivity slurry for the lithium-sulfur battery, wherein the second mixed solution is a mixture of an ammonia lithium-conducting polymer, tannic acid, a carbon conductor and a pore-forming additive. According to the invention, the functional layer is introduced to the surface of the polyolefin diaphragm, so that on one hand, the generation of polysulfide is prevented, and the shuttle effect is avoided; on the other hand, the introduction of the functional layer can improve the polarity of the surface of the diaphragm, thereby improving the electrolyte wettability of the diaphragm, promoting the migration of lithium ions, improving the ionic conductivity and the lithium ion migration number of the diaphragm, and finally improving the cycle performance and the rate performance of the battery.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to high-conductivity slurry for a lithium-sulfur battery, a diaphragm based on the high-conductivity slurry and application of the diaphragm.
Background
The lithium-sulfur battery, namely the battery with the positive electrode (cathode) being sulfur and the negative electrode (anode) being metal lithium, has the theoretical specific capacity of 1675mAh/g and the theoretical specific energy of 2600 Wh/kg. The poor conductivity of the sulfur of the positive electrode can not be directly used as the positive electrode, and the sulfur is generally mixed with a conductive agent to increase the conductivity, wherein the conductive agent is Super P, acetylene black and the like, and the dosage is different from 10 to 50 percent. The sulfur of the positive electrode becomes a polysulfide compound dissolved in the electrolyte during discharge, and the polysulfide compound passes through the separator to the negative electrode of lithium, reacts with lithium and returns to the positive electrode side, and the process is called shuttle effect. The shuttle effect is the obstacle to the maximum cycling stability of lithium-sulfur batteries. The negative electrode lithium generates dendritic crystals in the circulation process, the dendritic crystals grow too much to pierce the diaphragm to cause internal short circuit, and the dendritic crystals fall off to become dead lithium. The polyolefin material has the advantages of stable physical and chemical properties, water resistance, low cost, good mechanical properties, stable electrochemical properties and the like, and is widely applied to the diaphragm industry, but the defects of low hydrophobicity, low polarity, low surface energy and the like cause low liquid absorption rate, poor liquid retention property, low ionic conductivity and influence on the battery performance.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a preparation method of high-conductivity slurry for a lithium-sulfur battery.
The invention also aims to provide the high-conductivity slurry for the lithium-sulfur battery, which is obtained by the preparation method, and can overcome the defect that the traditional battery diaphragm cannot inhibit the shuttle effect, improve the surface polarity of the diaphragm and improve the liquid absorption and retention capacity of the diaphragm.
It is another object of the present invention to provide a battery using the separator.
The purpose of the invention is realized by the following technical scheme.
A preparation method of high-conductivity slurry for a lithium-sulfur battery comprises the following steps:
1) Mixing water and ethanol, adding a dispersing agent, and uniformly stirring to obtain a first mixed solution, wherein the ratio of the water to the ethanol to the dispersing agent is (1-20): 1: (0.01-0.1), wherein the dispersant is one of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol;
2) Mixing the second mixed solution with the first mixed solution, placing the mixture into a sand mill for sand milling for 30-90 min after uniform stirring to obtain the high-conductivity slurry for the lithium-sulfur battery, wherein the second mixed solution is a mixture of an ammonia lithium-conducting polymer, tannic acid, a carbon conductor and a pore-forming additive, and the ammonia lithium-conducting polymer, tannic acid, the carbon conductor and the pore-forming additive are in a ratio of (5-60) in parts by mass: (5-14): (10-40): (0.5-7), the second mixed solution is 1-25 wt% of the first mixed solution, the ammonia lithium-conducting polymer is ammonium polyvinyl alcohol phosphate and/or ammonium polyphosphate, the carbon conductor is graphene, Super-p or carbon black, and the pore-forming additive is one of lithium chloride, polyvinylpyrrolidone and sodium nitrate.
The high-conductivity slurry for the lithium-sulfur battery obtained by the preparation method.
A separator is prepared by coating the high-conductivity slurry for lithium-sulfur batteries on the positive electrode side of a polyolefin film, drying and then coating the polyolefin film, wherein the polyolefin film and the coating positioned on the polyolefin film are the separator.
In the technical scheme, the thickness of the coating is 1-8 microns.
In the above technical scheme, the polyolefin film is a polyethylene film or a polypropylene film.
in the technical scheme, the coating mode is roll coating.
A battery using the separator.
In the technical scheme, the sulfur is the positive electrode of the battery, and the lithium sheet is the negative electrode of the battery.
According to the invention, the functional layer (coating) is introduced to the surface of the polyolefin diaphragm (polyolefin film), so that on one hand, the generation of polysulfide is prevented, and the shuttle effect is avoided; on the other hand, the introduction of the functional layer can improve the polarity of the surface of the diaphragm, thereby improving the electrolyte wettability of the diaphragm, promoting the migration of lithium ions, improving the ionic conductivity and the lithium ion migration number of the diaphragm, and finally improving the cycle performance and the rate performance of the battery.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The mixers used in the following examples are double planetary power mixers, type: HY-DLH43L, manufacturer: guangzhou Hongshang mechanical science and technology, Inc.;
The sanding equipment used in the following examples was an all ceramic nano grinder, model: PT-5L, the manufacturer is a Noo mechanical equipment Co., Ltd.
Comparative example
1) Mixing water and ethanol, adding a dispersing agent, and stirring for 2min to be uniform to obtain a first mixed solution, wherein the ratio of the water to the ethanol to the dispersing agent is 3: 1: 0.02, the dispersant is polyacrylic acid ammonium salt;
2) Mixing the third mixed solution with the first mixed solution, stirring for 40min by a stirrer, and then putting the mixture into a sand mill for sand milling for 1 hour to obtain slurry, wherein the third mixed solution is a mixture of an ammonia lithium-conducting polymer, polyvinylpyrrolidone (PVP), a carbon conductor and a pore-forming additive, and the ratio of the ammonia lithium-conducting polymer, the PVP, the carbon conductor and the pore-forming additive is 10: 3: 10: 0.6, the third mixed solution is 7 wt% of the first mixed solution, the ammonia lithium-conducting polymer is ammonium polyvinyl alcohol phosphate, the carbon conductor is Super-p, and the pore-forming additive is polyethylene glycol.
The implementation effect is as follows:
And (2) coating the slurry obtained in the comparative example on the positive electrode side of a polyolefin film in a roll coating mode, drying for 0.5min at 70 ℃ to obtain a coating with the thickness of 2 microns on the polyolefin film, wherein the polyolefin film and the coating positioned on the polyolefin film are diaphragms, the polyolefin film is a polypropylene film, tests show that the decomposition voltage of the diaphragm is 4.6V, the thermal shrinkage rate of the diaphragm at 130 ℃ for 1 hour is 1.4%, the tensile strength is 1550Kg/cm 2, the liquid absorption rate is 200%, the ionic conductivity is 1.55 multiplied by 10 -3 s/cm -1, sulfur is adopted as a positive electrode, a lithium sheet is adopted as a negative electrode, a battery is assembled, the capacity retention rate is 78% after the battery is cycled for 100 circles at the rate of 0.5C, and the average coulombic efficiency is 90.84% after the battery is cycled for 20 circles.
Example 1
a preparation method of high-conductivity slurry for a lithium-sulfur battery comprises the following steps:
1) mixing water and ethanol, adding a dispersing agent, and stirring for 2min to be uniform to obtain a first mixed solution, wherein the ratio of the water to the ethanol to the dispersing agent is 3: 1: 0.01, the dispersant is polyacrylic acid ammonium salt;
2) Mix second mixed solution and first mixed solution, put into the sand mill sanding for 1 hour after stirring 40min to even with the mixer, obtain lithium sulphur battery and use high conductance thick liquids, wherein, the second mixed solution is the mixture of lithium polymer, tannic acid, carbon class conductor and pore-forming additive is led to the ammonia class, and according to the mass fraction, the ratio that lithium polymer, tannic acid, carbon class conductor and pore-forming additive are led to the ammonia class is 5: 5: 10: 0.6, the second mixed solution is 5 wt% of the first mixed solution, the ammonia lithium-conducting polymer is ammonium polyvinyl alcohol phosphate, the carbon conductor is Super-p, and the pore-forming additive is lithium chloride.
the carbon-based conductor can form a reduction site for sulfur ions to prevent polysulfide from being generated; the ammonia polymer has desolvation effect on lithium ions and can promote the transmission of the lithium ions, and the high-conductivity slurry for the lithium-sulfur battery is prepared from the two substances.
The tannic acid is a plant polyphenol, has higher molecular polarity and good affinity with electrolyte, has better adhesion effect on various base materials, adopts a roller coating mode to prepare the high-conductivity coating diaphragm meeting the requirements of the lithium ion battery, and solves the problem that the coating is easy to fall off.
Example 2
A preparation method of high-conductivity slurry for a lithium-sulfur battery comprises the following steps:
1) Mixing water and ethanol, adding a dispersing agent, and stirring for 2min to be uniform to obtain a first mixed solution, wherein the ratio of the water to the ethanol to the dispersing agent is 8: 1: 0.045, the dispersant is trimethylammonium hydrochloride;
2) Mixing the second mixed solution with the first mixed solution, stirring for 40min with a stirrer, and then placing into a sand mill for sand milling for 1 hour after the mixture is uniform to obtain the high-conductivity slurry for the lithium-sulfur battery, wherein the second mixed solution is a mixture of an ammonia lithium-conducting polymer, tannic acid, a carbon conductor and a pore-forming additive, and the ratio of the ammonia lithium-conducting polymer, tannic acid, the carbon conductor and the pore-forming additive is 37: 14: 34: 6.8, the second mixed solution is 10 wt% of the first mixed solution, the ammonia lithium-conducting polymer is ammonium polyphosphate, the carbon conductor is carbon black, and the pore-forming additive is polyvinylpyrrolidone.
Example 3
A preparation method of high-conductivity slurry for a lithium-sulfur battery comprises the following steps:
1) mixing water and ethanol, adding a dispersing agent, and stirring for 2min to be uniform to obtain a first mixed solution, wherein the ratio of the water to the ethanol to the dispersing agent is 15: 1: 0.08, the dispersant is polyethylene glycol;
2) mixing the second mixed solution with the first mixed solution, stirring for 40min with a stirrer, and then placing into a sand mill for sand milling for 1 hour after the mixture is uniform to obtain the high-conductivity slurry for the lithium-sulfur battery, wherein the second mixed solution is a mixture of an ammonia lithium-conducting polymer, tannic acid, a carbon conductor and a pore-forming additive, and the ratio of the ammonia lithium-conducting polymer, tannic acid, the carbon conductor and the pore-forming additive is 64: 9: 30: and 3, the second mixed solution accounts for 16 wt% of the first mixed solution, the ammonia lithium-conducting polymer is ammonium polyvinyl alcohol phosphate, the carbon conductor is graphene, and the pore-forming additive is sodium nitrate.
Example 4
A diaphragm is formed by coating the high-conductivity slurry for the lithium-sulfur battery obtained in the example 1 on the positive electrode side of a polyolefin film in a roll coating mode, a coating with the thickness of 1.3 micrometers is obtained on the polyolefin film after drying at 70 ℃ for 0.5min, the polyolefin film and the coating on the polyolefin film are diaphragms, wherein the polyolefin film is a polypropylene film, the decomposition voltage of the diaphragm is 4.8V, the thermal shrinkage rate of the diaphragm at 130 ℃ for 1 hour is 1.1%, the tensile strength is 1650Kg/cm 2, the liquid absorption rate is 330%, the ionic conductivity is 1.85 x 10 -3 s/cm -1, the battery is assembled by adopting sulfur as the positive electrode and a lithium sheet as the negative electrode, the capacity retention rate is 93% after the battery is cycled for 100 circles at the rate of 0.5 ℃, and the average coulombic efficiency is 99.84% after the battery is cycled for 20 circles.
Example 5
A diaphragm is formed by coating the high-conductivity slurry for the lithium-sulfur battery obtained in the example 2 on the positive electrode side of a polyolefin film in a roll coating mode, a coating with the thickness of 2 micrometers is obtained on the polyolefin film after drying at 70 ℃ for 0.5min, the polyolefin film and the coating on the polyolefin film are diaphragms, wherein the polyolefin film is a polyethylene film, the decomposition voltage of the diaphragm is 4.9V, the thermal shrinkage rate of the diaphragm at 130 ℃ for 1 hour is 0.9%, the tensile strength 1720Kg/cm 2, the liquid absorption rate is 370%, the ionic conductivity is 1.82 x 10 - 3 s/cm -1, the battery is assembled by adopting sulfur as the positive electrode and a lithium sheet as the negative electrode, the capacity retention rate is 97% after the battery is cycled for 100 circles at the rate of 0.5 ℃, and the average coulombic efficiency is 99.87% after the battery is cycled for 20 circles.
Example 6
A diaphragm is formed by coating the high-conductivity slurry for the lithium-sulfur battery obtained in the example 3 on the positive side of a polyolefin film in a roll coating mode, a coating with the thickness of 4 micrometers is obtained on the polyolefin film after drying at 70 ℃ for 0.5min, the polyolefin film and the coating on the polyolefin film are diaphragms, wherein the polyolefin film is a polypropylene film, the diaphragm is tested to have the decomposition voltage of 4.77V, the thermal shrinkage rate of 1 hour at 130 ℃ is 1.2%, the tensile strength is 1590Kg/cm 2, the liquid absorption rate is 354%, the ionic conductivity is 1.79 x 10 - 3 s/cm -1, the battery is assembled by adopting sulfur as the positive electrode and a lithium sheet as the negative electrode, the capacity retention rate is 94.3% after the battery is cycled for 100 circles at the magnification of 0.5 ℃, and the average coulombic efficiency is 99.74% after the battery is cycled for 20 circles.
Compared with a comparative example, the polyolefin diaphragm coated by the high-conductivity slurry has higher liquid absorption rate due to the enhanced surface polarity, so that the ionic conductivity is improved; the capacity retention rate is higher after 100 cycles of circulation under the multiplying power of 0.5C, which shows that the polyolefin diaphragm battery coated by the high-conductivity slurry has stable performance, the generation of polysulfide and the shuttle effect of polysulfide in the charge-discharge reaction process are well inhibited, and the electrochemical reaction activity of the lithium-sulfur battery is further improved. Thereby greatly improving the cycle stability and capacity retention rate of the lithium-sulfur battery.
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 (8)
1. A preparation method of high-conductivity slurry for a lithium-sulfur battery is characterized by comprising the following steps:
1) Mixing water and ethanol, adding a dispersing agent, and uniformly stirring to obtain a first mixed solution, wherein the ratio of the water to the ethanol to the dispersing agent is (1-20): 1: (0.01-0.1), wherein the dispersant is one of polyacrylic acid ammonium salt, trimethylammonium hydrochloride and polyethylene glycol;
2) Mixing the second mixed solution with the first mixed solution, placing the mixture into a sand mill for sand milling for 30-90 min after uniform stirring to obtain the high-conductivity slurry for the lithium-sulfur battery, wherein the second mixed solution is a mixture of an ammonia lithium-conducting polymer, tannic acid, a carbon conductor and a pore-forming additive, and the ammonia lithium-conducting polymer, tannic acid, the carbon conductor and the pore-forming additive are in a ratio of (5-60) in parts by mass: (5-14): (10-40): (0.5-7), the second mixed solution is 1-25 wt% of the first mixed solution, the ammonia lithium-conducting polymer is ammonium polyvinyl alcohol phosphate and/or ammonium polyphosphate, the carbon conductor is graphene, Super-p or carbon black, and the pore-forming additive is one of lithium chloride, polyvinylpyrrolidone and sodium nitrate.
2. The high-conductivity paste for lithium-sulfur batteries obtained by the preparation method according to claim 1.
3. A separator, wherein the high-conductivity paste for lithium sulfur batteries according to claim 1 or 2 is applied to the positive electrode side of a polyolefin film, and dried to obtain a coating layer on the polyolefin film, and the polyolefin film and the coating layer thereon are the separator.
4. the separator of claim 3, wherein the coating has a thickness of 1 to 8 microns.
5. the separator of claim 3 or 4, wherein said polyolefin film is a polyethylene film or a polypropylene film.
6. The separator of claim 5, wherein said coating is by roll coating.
7. A battery using the separator according to any one of claims 3 to 6.
8. the battery of claim 7, wherein the sulfur is a positive electrode and the lithium plate is a negative electrode.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112952292A (en) * | 2020-12-23 | 2021-06-11 | 重庆大学 | Composite diaphragm capable of being used for metal lithium battery and metal sodium battery, and preparation method and application thereof |
| CN113067096A (en) * | 2019-12-16 | 2021-07-02 | 河北金力新能源科技股份有限公司 | Functional diaphragm for lithium-sulfur battery and preparation method and application thereof |
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| CN113067096A (en) * | 2019-12-16 | 2021-07-02 | 河北金力新能源科技股份有限公司 | Functional diaphragm for lithium-sulfur battery and preparation method and application thereof |
| CN113067096B (en) * | 2019-12-16 | 2022-11-01 | 河北金力新能源科技股份有限公司 | Functional diaphragm for lithium-sulfur battery and preparation method and application thereof |
| CN112952292A (en) * | 2020-12-23 | 2021-06-11 | 重庆大学 | Composite diaphragm capable of being used for metal lithium battery and metal sodium battery, and preparation method and application thereof |
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