CN108847468B - Water-based PVDF-coated lithium ion battery diaphragm and preparation method thereof - Google Patents
Water-based PVDF-coated lithium ion battery diaphragm and preparation method thereof Download PDFInfo
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- CN108847468B CN108847468B CN201811055652.XA CN201811055652A CN108847468B CN 108847468 B CN108847468 B CN 108847468B CN 201811055652 A CN201811055652 A CN 201811055652A CN 108847468 B CN108847468 B CN 108847468B
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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 preparation method of a lithium ion battery diaphragm coated with aqueous PVDF, which comprises the following preparation steps: adding a dispersing agent and a thickening agent into water, stirring uniformly, adding PVDF (polyvinylidene fluoride) to enable the PVDF to be dissolved into the water, and preparing a suspension; adding the aqueous UV resin, the aqueous binder, the photoinitiator and the polymerization inhibitor into the residual water, uniformly dispersing, introducing the PVDF suspension, and uniformly dispersing to prepare the PVDF slurry; and coating the PVDF slurry on one side or two sides of the lithium ion battery base film subjected to corona treatment to form a point matrix type distribution coating, and curing to obtain a finished product. The advantages are that: by adopting the water-based UV light curing technology, the coating can be dried immediately, the energy consumption is lower, and the deformation problem of the diaphragm caused by heat and tension is not worried about. The drying time of the diaphragm coating can be reduced to 8-15s, and continuous and stable large-scale production is facilitated.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery diaphragm coated with aqueous PVDF and a preparation method of the lithium ion battery diaphragm coated with the aqueous PVDF.
Background
Compared with a steel shell and aluminum shell battery cell, the lithium ion soft package battery cell has the advantages of light weight, large capacity, small internal resistance, flexible design, safety and the like, and is widely applied to 3c consumer electronics and power battery products. However, the positive and negative electrode interfaces of the battery are not limited by hard shells, and the graphite is easy to deform due to expansion in the charging and discharging processes, so that the positive and negative electrode interfaces are easy to be unstable when deformation occurs, and the battery performance is poor.
At present, in order to improve the interfaces of the positive electrode and the negative electrode of the battery, composite glue coating improvement is mainly adopted in the industry, and the positive electrode and the negative electrode are firmly bonded together through glue, so that the expansion of graphite is limited in the charging and discharging process. The composite glue coating mainly comprises PVDF, acrylic glue, polyacrylonitrile polymer and the like. The PVDF is divided into an oily system and a water-based system, the oily system is mainly characterized in that the PVDF is dissolved by a solvent, coated on a base film and then enters an extraction tank for pore forming, and the process is complex, high in cost and not environment-friendly. The aqueous PVDF is prepared by mainly melting PVDF powder into water to form turbid liquid, and transferring the turbid liquid to a substrate through processes such as micro gravure, spraying and the like. But the coating of the micro-gravure preparation process is compact and easy to block ion channels. The coating prepared by the spraying process is distributed in discrete islands, the thickness is uneven, the island size is not uniform, and the final adhesion exertion effect is poor. Acrylic glue and polyacrylonitrile polymer are easy to block ion channels due to large swelling and strict control of morphology distribution, and are less in application.
Disclosure of Invention
The purpose of the invention is: aiming at the defects, the water-based PVDF coated lithium ion battery diaphragm and the preparation method thereof are provided, wherein the diaphragm has regular shape distribution, good adhesive property, environmental friendliness, low cost and convenience for large-scale continuous production.
In order to achieve the purpose, the invention adopts the technical scheme that:
the lithium ion battery diaphragm coated by the water-based PVDF consists of a lithium ion battery base film and coatings on one side or two sides of the base film, wherein the coatings consist of PVDF slurry, and the PVDF slurry consists of the following components in parts by weight:
the PVDF is one of homopolymer or copolymer, the molecular weight of the PVDF is 50-80 ten thousand, and the particle size of the PVDF is 150-300 nm.
The water-based UV curing resin is one or more of UP resin, PUA resin or EA resin.
The water-based binder is one or more of acrylic acid polymer and polyurethane.
The thickener is one or more of carboxymethyl cellulose, hydroxymethyl cellulose, bentonite or attapulgite clay.
The photoinitiator is one of benzophenone, carbonyl compound, azo compound or organic sulfur compound.
The auxiliary agent comprises one or more of a defoaming agent, a flatting agent, a polymerization inhibitor and a dispersing agent.
The lithium ion battery base film is one of a polyethylene film, a polypropylene film or a polypropylene/polyethylene/polypropylene composite film, a polyimide film, a polyvinylidene fluoride film and a non-woven fabric film with the thickness of 5-25um and the porosity of 36-45%.
A preparation method of a lithium ion battery diaphragm coated by aqueous PVDF comprises the following preparation steps: a. adding a dispersing agent and a thickening agent in an auxiliary agent into a part of water, uniformly stirring, slowly adding PVDF, and completely melting PVDF into water through a kneading process to prepare a PVDF suspension;
b. adding the aqueous UV resin, the aqueous binder, the photoinitiator and the polymerization inhibitor in the auxiliary agent into the rest water according to the proportion, uniformly dispersing, introducing the PVDF suspension, and uniformly dispersing to prepare the PVDF slurry.
c. And (3) coating the PVDF slurry on one side or two sides of the lithium ion battery base film subjected to corona treatment by utilizing one of flexible plate printing, gravure printing, silk screen printing or letterpress printing to form a dot matrix type distribution coating, and curing by UV curing and baking for 8-15s at the temperature of 25-45 ℃ to obtain a finished product.
The thickness of the coating is 2-6um, and the gram weight of the coating is 0.4-1.8g/m2The spot size of the coating is 300-1500 um.
Compared with the prior art, the invention achieves the technical effects that: 1. the PVDF-coated lithium ion battery diaphragm prepared by the invention adopts a water-based UV light curing technology, realizes matrix type point distribution by one process of letterpress, flexography and silk-screen printing, improves the distribution uniformity, thickness controllability and spot size consistency of a coating, simultaneously, the air permeability of a base film is not increased by the coating with uniform gap distribution, the PVDF-coated lithium ion battery diaphragm is more smooth in contact with the positive electrode and the negative electrode of a battery cell, the bonding force is more easily exerted, and the positive electrode and the negative electrode interfaces of the battery cell are improved;
2. the PVDF powder is coated on the base material by adopting a water-based UV photocuring technology, and due to the curing crosslinking effect, the film forming effect is better, the binding force between the coating and the base material is better, and the process capability of the diaphragm is improved;
3. by adopting the water-based UV light curing technology, the coating can be dried immediately, the energy consumption is lower, and the deformation problem of the diaphragm caused by heat and tension is not worried about. The drying time of the diaphragm coating can be reduced to 8-15s, and continuous and stable large-scale production is facilitated.
Detailed Description
The invention is further described below with reference to the following examples:
the first embodiment is as follows:
the invention relates to a water-based PVDF coated lithium ion battery diaphragm, which consists of a lithium ion battery base film and coatings on one side or two sides of the base film, wherein the coatings consist of PVDF slurry, and the PVDF slurry consists of the following components in parts by weight: 9 parts of polyvinylidene fluoride (PVDF) copolymer; the preferable part of the aqueous UV curing resin is UP resin, and 15 parts of the aqueous UV curing resin is UP resin; the water-based binder is acrylic acid polymer, and is preferably 4 parts; the preferable thickening agent is carboxymethyl cellulose 0.6 part; 63 parts of water; the photoinitiator is preferably benzophenone and is preferably 7 parts; 0.09 part of dispersant as an auxiliary agent and 1 part of polymerization inhibitor.
Wherein the molecular weight of the polyvinylidene fluoride copolymer of PVDF is 50-80 ten thousand, and the particle size is 150-300 nm.
The lithium ion battery base film is a polyethylene film with the thickness of 5um and the porosity of 36 percent.
A preparation method of a lithium ion battery diaphragm coated by aqueous PVDF comprises the following preparation steps: a. adding a dispersing agent and carboxymethyl cellulose in the auxiliary agent into 22 parts of water, uniformly stirring, slowly adding polyvinylidene fluoride copolymer, and completely melting the polyvinylidene fluoride copolymer into the water through a kneading process to prepare polyvinylidene fluoride copolymer suspension;
b. adding UP resin, acrylic polymer, benzophenone and a polymerization inhibitor in an auxiliary agent into the residual 41 parts of water according to a ratio, uniformly dispersing, introducing polyvinylidene fluoride copolymer suspension, and uniformly dispersing to prepare polyvinylidene fluoride copolymer slurry;
c. printing PVDF polyvinylidene fluoride copolymer slurry on one side or two sides of a polyethylene film subjected to corona treatment by using a flexible board to form a dot matrix type distribution coating, and curing by UV curing and baking for 8s at the temperature of 25 ℃ to obtain a finished product.
The thickness of the coating is 2um, and the gram weight of the coating is 0.4g/m2The spot size of the coating is 300 um.
Example two:
the invention relates to a water-based PVDF coated lithium ion battery diaphragm, which consists of a lithium ion battery base film and coatings on one side or two sides of the base film, wherein the coatings consist of PVDF slurry, and the PVDF slurry consists of the following components in parts by weight: 8 parts of polyvinylidene fluoride (PVDF) copolymer; the water-based UV curing resin is PUA resin, and preferably 17 parts; the water-based binder is acrylic acid polymer, preferably 5 parts; the preferable thickener is hydroxymethyl cellulose 0.8 part; 60 parts of water; the photoinitiator is preferably a carbonyl compound and is preferably 8 parts; 0.09 part of dispersant as an auxiliary agent and 2 parts of polymerization inhibitor.
The PVDF is polyvinylidene fluoride copolymer, the molecular weight of the PVDF is 50-80 ten thousand, and the particle size of the PVDF is 150-300 nm.
The lithium ion battery base film is a polypropylene film with the thickness of 15um and the porosity of 40 percent.
A preparation method of a lithium ion battery diaphragm coated by aqueous PVDF comprises the following preparation steps: a. adding a dispersing agent and hydroxymethyl cellulose in an auxiliary agent into 30 parts of water, uniformly stirring, slowly adding polyvinylidene fluoride copolymer, and completely melting the polyvinylidene fluoride copolymer into the water through a kneading process to prepare polyvinylidene fluoride copolymer suspension;
b. adding PUA resin, acrylic acid polymer, carbonyl compound and polymerization inhibitor into the rest 30 parts of water according to a ratio, uniformly dispersing, introducing polyvinylidene fluoride copolymer suspension, and uniformly dispersing to prepare polyvinylidene fluoride copolymer slurry;
c. and (2) screen printing polyvinylidene fluoride copolymer slurry on one side or two sides of the polypropylene film subjected to corona treatment to form a point matrix type distribution coating, and curing by UV curing and baking at the temperature of 35 ℃ for 12s to obtain a finished product.
The coating thickness is 4um, and the coating gram weight is 1g/m2The spot size of the coating is 800 um.
Example three:
the invention relates to a water-based PVDF coated lithium ion battery diaphragm, which consists of a lithium ion battery base film and coatings on one side or two sides of the base film, wherein the coatings consist of PVDF slurry, and the PVDF slurry consists of the following components in parts by weight: 6 parts of polyvinylidene fluoride (PVDF) copolymer; the preferable part of the aqueous UV curing resin is EA resin, and 15 parts of the aqueous UV curing resin is; the water-based binder is acrylic acid polymer, and is preferably 2 parts; the thickener is attapulgite clay, and preferably 1 part; 65 parts of water; the photoinitiator is preferably an azo compound, preferably 6 parts; 0.09 part of dispersant as an auxiliary agent and 2.5 parts of polymerization inhibitor.
The lithium ion battery base film is a polyimide film with the thickness of 25um and the porosity of 45 percent.
A preparation method of a lithium ion battery diaphragm coated by aqueous PVDF comprises the following preparation steps: a. adding a dispersing agent and attapulgite clay in the auxiliary agent into 30 parts of water, uniformly stirring, slowly adding polyvinylidene fluoride copolymer, and completely melting the polyvinylidene fluoride copolymer into the water through a kneading process to prepare polyvinylidene fluoride copolymer suspension;
b. adding EA resin, acrylic polymer, azo compound and polymerization inhibitor in the auxiliary agent into the rest 35 parts of water according to the proportion, uniformly dispersing, introducing polyvinylidene fluoride copolymer suspension, and uniformly dispersing to prepare polyvinylidene fluoride copolymer slurry;
c. coating polyvinylidene fluoride copolymer slurry on one side or two sides of a polyimide film subjected to corona treatment by utilizing relief printing to form a point matrix type distribution coating, and curing by UV curing and baking for 15s at the temperature of 45 ℃ to obtain a finished product.
The thickness of the coating is 6um, and the gram weight of the coating is 1.8g/m2The spot size of the coating is 1500 um.
Example four:
comparison with the control group: a. weighing 83 parts of water, adding 0.09 part of dispersing agent and 0.6 part of sodium carboxymethylcellulose, uniformly stirring, adding 9 parts of PVDF powder, dispersing and stirring, then 6 parts of acrylate, uniformly stirring and dispersing, and preparing PVDF slurry;
b. and (2) selecting a 12-micron corona polyethylene diaphragm with the porosity of 38%, coating the PVDF slurry on one side of the base film in a micro-gravure printing mode at the coating speed of 15m/min and the oven temperature of 40 ℃, and drying to obtain the PVDF-coated lithium ion battery diaphragm. The thickness of the PVDF-coated lithium ion battery separator is 16um, and the thickness of the coating is 4 um;
the PVDF-coated lithium ion battery membranes obtained from the above invention and comparative examples were tested for performance and the data are shown in the following Table one:
as can be seen from the data in the table, the air permeability differences of the three types of membranes obtained in the 3 embodiments of the invention are not large, and the membranes have the best base material peeling strength and positive electrode peeling strength, and the embodiment 2 has stronger advantages in air permeability and peeling strength compared with the micro-gravure process of a conventional formula system, and meanwhile, the drying time is greatly reduced and the energy consumption is saved by adopting the UV curing technology.
Compared with the prior art, the invention achieves the technical effects that: 1. the PVDF-coated lithium ion battery diaphragm prepared by the invention adopts a water-based UV light curing technology, realizes matrix type point distribution by one process of letterpress, flexography and silk-screen printing, improves the distribution uniformity, thickness controllability and spot size consistency of a coating, simultaneously, the air permeability of a base film is not increased by the coating with uniform gap distribution, the PVDF-coated lithium ion battery diaphragm is more smooth in contact with the positive electrode and the negative electrode of a battery cell, the bonding force is more easily exerted, and the positive electrode and the negative electrode interfaces of the battery cell are improved;
2. the PVDF powder is coated on the base material by adopting a water-based UV photocuring technology, and due to the curing crosslinking effect, the film forming effect is better, the binding force between the coating and the base material is better, and the process capability of the diaphragm is improved;
3. by adopting the water-based UV light curing technology, the coating can be dried immediately, the energy consumption is lower, and the deformation problem of the diaphragm caused by heat and tension is not worried about. The drying time of the diaphragm coating can be reduced to 8-15s, and continuous and stable large-scale production is facilitated.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. A water-based PVDF coated lithium ion battery separator, characterized by: the coating consists of a lithium ion battery base film and coatings on one side or two sides of the base film, wherein the coatings consist of PVDF slurry, and the PVDF slurry consists of the following components in parts by weight:
6-9 parts of PVDF;
15-20 parts of water-based UV curing resin;
2-5 parts of a water-based binder;
0-1 part of thickening agent;
35-65 parts of water;
6-8 parts of a photoinitiator;
0-3 parts of an auxiliary agent;
the PVDF slurry forms a matrix type point distribution coating on one side or two sides of the lithium ion battery base film in one coating mode of flexible plate printing, intaglio printing, silk screen printing or relief printing;
the thickness of the coating is 2-6 um;
the thickener is one or more of carboxymethyl cellulose, hydroxymethyl cellulose, bentonite or attapulgite clay.
2. The aqueous PVDF-coated lithium ion battery separator of claim 1, wherein: the PVDF is one of homopolymer or copolymer, the molecular weight of the PVDF is 50-80 ten thousand, and the particle size of the PVDF is 150-300 nm.
3. The aqueous PVDF-coated lithium ion battery separator of claim 1, wherein: the water-based UV curing resin is one or more of UP resin, PUA resin or EA resin.
4. The aqueous PVDF-coated lithium ion battery separator of claim 1, wherein: the water-based binder is one or more of acrylic acid polymer and polyurethane.
5. The aqueous PVDF-coated lithium ion battery separator of claim 1, wherein: the photoinitiator is one of benzophenone, carbonyl compound, azo compound or organic sulfur compound.
6. The aqueous PVDF-coated lithium ion battery separator of claim 1, wherein: the auxiliary agent comprises one or more of a defoaming agent, a flatting agent, a polymerization inhibitor and a dispersing agent.
7. The aqueous PVDF-coated lithium ion battery separator of claim 1, wherein: the lithium ion battery base film is one of a polyethylene film, a polypropylene film or a polypropylene/polyethylene/polypropylene composite film, a polyimide film, a polyvinylidene fluoride film and a non-woven fabric film with the thickness of 5-25um and the porosity of 36-45%.
8. The method of making the aqueous PVDF-coated lithium ion battery separator of any of claims 1-7, wherein: the preparation method comprises the following steps:
a. adding a dispersing agent and a thickening agent in an auxiliary agent into a part of water, uniformly stirring, slowly adding PVDF, and completely melting PVDF into water through a kneading process to prepare a PVDF suspension;
b. adding aqueous UV resin, aqueous binder, photoinitiator and polymerization inhibitor in the auxiliary agent into the rest water according to a certain proportion, uniformly dispersing, introducing PVDF suspension, and uniformly dispersing to prepare PVDF slurry;
c. and (3) coating the PVDF slurry on one side or two sides of the lithium ion battery base film subjected to corona treatment by utilizing one of flexible plate printing, gravure printing, silk screen printing or letterpress printing to form a dot matrix type distribution coating, and curing by UV curing and baking for 8-15s at the temperature of 25-45 ℃ to obtain a finished product.
9. The method of claim 8 for preparing a waterborne PVDF-coated lithium ion battery separator, wherein: the gram weight of the coating is 0.4-1.8g/m2, and the spot size of the coating is 300-1500 um.
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| CN109524603B (en) * | 2018-11-26 | 2020-08-25 | 深圳市星源材质科技股份有限公司 | Functional diaphragm and preparation method thereof |
| CN109605967A (en) * | 2018-12-25 | 2019-04-12 | 太仓金煜电子材料有限公司 | A kind of production method of ultra-thin print film |
| CN111490213A (en) * | 2019-01-25 | 2020-08-04 | 辽源鸿图锂电隔膜科技股份有限公司 | High-safety water-based PVDF (polyvinylidene fluoride) diaphragm slurry and preparation method thereof |
| CN110085790A (en) * | 2019-05-06 | 2019-08-02 | 江苏安瑞达新材料有限公司 | The preparation process of the lithium battery dotted coating diaphragm of Low ESR high-adhesion |
| CN112223931A (en) * | 2019-11-19 | 2021-01-15 | 江苏上达电子有限公司 | Primary curing method for printing ink |
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| CN112018311A (en) * | 2020-09-10 | 2020-12-01 | 青岛蓝科途膜材料有限公司 | Lithium ion battery diaphragm, preparation method and application thereof |
| CN115477876A (en) * | 2021-06-16 | 2022-12-16 | 深圳市星源材质科技股份有限公司 | Coating slurry, coating diaphragm and preparation method of coating diaphragm |
| CN114512766B (en) * | 2022-02-17 | 2023-08-22 | 浙江巨圣氟化学有限公司 | Preparation method of lithium battery diaphragm by adopting VDF polymer water-based coating liquid |
| CN114566755B (en) * | 2022-02-17 | 2023-08-18 | 浙江巨圣氟化学有限公司 | Preparation method of fluorine-containing polymer diaphragm for lithium battery |
| CN117937044A (en) * | 2024-03-22 | 2024-04-26 | 深圳市旭然电子有限公司 | Battery diaphragm coating process and battery diaphragm prepared by same |
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