CN107528038B - Mixed slurry for preparing composite diaphragm and preparation method of composite diaphragm - Google Patents
Mixed slurry for preparing composite diaphragm and preparation method of composite diaphragm Download PDFInfo
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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
- H01M50/44—Fibrous material
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- H—ELECTRICITY
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- 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
- H01M50/431—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
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- 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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Abstract
The invention discloses a mixed slurry for preparing a composite diaphragm, which comprises 5-45% of nano-gel by mass percent; 5-45% of attapulgite nano ceramic fiber; 1.5 to 5 percent of binder; 0.5 to 1.5 percent of dispersant; 0.1-0.5% of surfactant, solvent and the balance. The invention also discloses a preparation method of the composite diaphragm.
Description
Technical Field
The invention relates to the field of lithium batteries and the like, in particular to mixed slurry for preparing a composite diaphragm and a preparation method of the composite diaphragm.
Background
Lithium ion batteries are becoming the research focus of new power technologies due to their advantages such as high energy density and long cycle life. The lithium ion battery has been widely used in a plurality of fields such as digital electronic products and new energy automobiles, and is internationally recognized as a novel energy carrier with great application prospect and market value. In recent years, China is developing the lithium ion battery industry greatly, the capacity of the lithium ion battery is increasing continuously, but the safety problem of the lithium ion battery is concerned by people more and more.
The lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm and an electrolyte, wherein the diaphragm is used as a barrier between the positive electrode and the negative electrode, plays a vital role in the performance of the lithium ion battery, and the performance of the diaphragm directly influences the capacity and the cycle life of the battery, particularly the safety performance of the battery. Polyolefin diaphragms such as single-layer Polyethylene (PE), single-layer polypropylene (PP), and PP/PE/PP three-layer diaphragms are susceptible to shrinkage or perforation under high current intensity, high temperature, or lithium dendrite growth conditions, thereby causing short-circuiting of the positive and negative electrodes. At present, the diaphragm can not meet the application requirement. The method of coating ceramic particle layer or attapulgite nano ceramic fiber on polyolefin and other base material to make composite diaphragm is widely adopted. Patent CN105514328A coats ceramic particles on the surface of the polyolefin diaphragm, and utilizes the inorganic particle layer on the surface of the diaphragm to enhance the mechanical properties such as puncture resistance and thermal stability of the diaphragm and improve the safety performance of the battery. However, the ceramic particles with a nearly spherical shape easily block the pore channels in the original polyolefin separator, thereby blocking the ion conduction channels, and causing obvious loss of the capacity and the cycle life of the battery. Patent ZL201410746094.7 coats attapulgite nanometer ceramic fiber rod-shaped material on the surface of the polyolefin diaphragm, and improves the thermal stability and ion conduction capability of the diaphragm. But the adhesion between the fiber rod-shaped material and the polyolefin material is poor, and the adhesion between the attapulgite nano ceramic fiber diaphragm and the lithium ion battery pole piece is very low, which is not beneficial to the processing and transportation of the battery.
In order to meet the increasing demand of lithium ion batteries for high-performance diaphragms, it is necessary to develop diaphragms with higher structural stability, good ionic conductivity, excellent electrolyte absorption and retention, strong adhesion between the diaphragms and pole pieces, and the like.
Disclosure of Invention
The purpose of the invention is: the mixed slurry for preparing the composite diaphragm is provided to improve the mechanical property and the heat shrinkage property of the diaphragm, simultaneously enable the composite diaphragm to have excellent electrolyte absorption and retention capacity, and improve the adhesive force between the composite diaphragm and a lithium battery pole piece.
The technical scheme for realizing the purpose is as follows: a mixed slurry for preparing a composite diaphragm comprises 5-45% of nano-gel by mass percent; 5-45% of attapulgite nano ceramic fiber; 1.5 to 5 percent of binder; 0.5 to 1.5 percent of dispersant; 0.1-0.5% of surfactant, solvent and the balance.
In a preferred embodiment of the present invention, the nano-gel is a spherical structure, and the diameter is 100 nm to 150 nm; the nanometer glue is one or a combination of polyvinylidene fluoride, polytetrafluoroethylene, vinylidene fluoride and hexafluoropropylene copolymer.
In a preferred embodiment of the invention, the average length of the attapulgite nano ceramic fiber is 0.5 to 2 microns, and the average diameter is 0.05 to 0.3 micron.
In a preferred embodiment of the present invention, the binder is one or a mixture of more of polyacrylates, polyvinyl alcohol, ethylene-vinyl acetate copolymer, polyvinyl acetate, styrene-butadiene latex, styrene-acrylic latex, pure benzene latex, or polyurethane.
In a preferred embodiment of the invention, the dispersant is one or more of water-soluble polybranched alcohol, sodium carboxymethylcellulose, triethyl phosphate, polyacrylic acid, sodium polyacrylate, polyethylene glycol, polyethylene oxide and hydroxyethyl cellulose.
In a preferred embodiment of the present invention, the surfactant is one or a mixture of several of fluorinated alkyl methoxy ether alcohol, fluorinated alkyl ethoxy ether alcohol, polyoxyethylene alkyl amide and fatty alcohol-polyoxyethylene ether.
The second object of the present invention is to: a method for preparing a composite separator is provided.
The technical scheme for realizing the purpose is as follows: a preparation method of a composite diaphragm comprises the following steps: step S1) preparing the mixed slurry of any one of claims 1 to 6; step S2) coating the mixed slurry on the surface of a porous polymer film to form a diaphragm layer of nano-colloid and attapulgite nano-ceramic fibers; step S3), drying to obtain the composite diaphragm.
In a preferred embodiment of the present invention, the step S1) includes the following steps: step S11), dissolving the attapulgite nano ceramic fiber and a dispersing agent in a solvent, and fully stirring; step S12), adding the nano-gel, the adhesive and the surfactant into the solution obtained in the step S11), and fully mixing and stirring to obtain the mixed slurry.
In a preferred embodiment of the present invention, the porous polymer film is one of a polyethylene-based film, a polypropylene/polyethylene/polypropylene composite-based film, a polyimide-based film, a nano-gel-based film, a polyethylene non-woven fabric-based film, a polypropylene non-woven fabric-based film, or a polyimide non-woven fabric-based film.
In a preferred embodiment of the present invention, the nano-colloids in the membrane layer and the attapulgite nano-ceramic fibers are randomly stacked and arranged, and pores with an average pore diameter of 0.05 to 1 micron are formed.
The invention has the advantages that: according to the mixed slurry for preparing the composite diaphragm and the preparation method of the composite diaphragm, the composite diaphragm is prepared through a coating process, and due to the fact that the attapulgite nano ceramic fibers are uniformly dispersed and stacked in the composite diaphragm, the in-plane tensile strength of the diaphragm is improved, the mechanical property and the thermal stability of the diaphragm are improved, and the safety of a battery is enhanced. Due to the existence of the nanometer glue, the cohesiveness of the diaphragm and the battery pole piece is enhanced, so that the hardness of the pole piece is increased, the battery is firmer, and the processing and the transportation are convenient. The nanometer glue and the attapulgite nanometer ceramic fiber are mixed and coated, so that the adhesive force of the attapulgite nanometer ceramic fiber on the porous polymer film is improved, and the risk of falling of ceramic powder in the transportation and use processes of the ceramic composite diaphragm is reduced. The prepared composite diaphragm has the advantages that the coating peeling strength and the tensile strength are obviously improved, the mechanical property and the thermal shrinkage property are improved, and the adhesive force between the composite diaphragm and the lithium battery pole piece is improved. Meanwhile, the composite diaphragm has excellent electrolyte liquid absorption and retention capacity through the porosity.
Drawings
The invention is further explained below with reference to the figures and examples.
Fig. 1 is a surface scanning electron microscope picture of composite membrane sample S3 of example 3 of the present invention.
Detailed Description
The following description of the embodiments refers to the accompanying drawings for illustrating the specific embodiments in which the invention may be practiced.
A mixed slurry for preparing a composite diaphragm comprises 5-45% of nano-gel by mass percent; 5-45% of attapulgite nano ceramic fiber; 1.5 to 5 percent of binder; 0.5 to 1.5 percent of dispersant; 0.1-0.5% of surfactant, solvent and the balance.
The nanometer glue is of a spherical structure, and the diameter of the nanometer glue is 100-150 nanometers; the nanometer glue is one or a combination of polyvinylidene fluoride, polytetrafluoroethylene, vinylidene fluoride and hexafluoropropylene copolymer. In the specific formulation, the mass fraction of the nano-gel is usually about 10%.
The average length of the attapulgite nano ceramic fiber is between 0.5 and 2 microns, and the average diameter is between 0.05 and 0.3 micron. In the specific mixing process, the mass fraction of the attapulgite nano ceramic fiber is about 20 percent.
The binder is one or a mixture of more of polyacrylate, polyvinyl alcohol, ethylene-vinyl acetate copolymer, polyvinyl acetate, styrene-butadiene latex, styrene-acrylic latex, pure benzene latex or polyurethane. In the specific formulation, the mass fraction of the binder is usually about 3%.
The dispersing agent is one or a combination of more of water-soluble polybranched alcohol, sodium carboxymethylcellulose, triethyl phosphate, polyacrylic acid, sodium polyacrylate, polyethylene glycol, polyethylene oxide and hydroxyethyl cellulose. In the specific formulation, the mass fraction of the dispersant is usually about 1%.
The surfactant is one or a mixture of more of fluoroalkyl methoxy ether alcohol, fluoroalkyl ethoxy ether alcohol, polyoxyethylene alkyl amide and fatty alcohol-polyoxyethylene ether. In the specific formulation, the mass fraction of the binder is usually about 0.3%.
Deionized water is usually selected as the solvent, and is pollution-free and beneficial to environmental protection.
A preparation method of a composite diaphragm comprises the following steps: step S1) preparing the mixed slurry; the step S1) includes the steps of: step S11), dissolving the attapulgite nano ceramic fiber and a dispersing agent in a solvent, and fully stirring; step S12), adding the nano-gel, the adhesive and the surfactant into the solution obtained in the step S11), and fully mixing and stirring to obtain the mixed slurry.
Step S2) coating the mixed slurry on the surface of a porous polymer film to form a diaphragm layer of the nano-colloid and the attapulgite nano-ceramic fibers. In the present invention, the coating may be applied to both sides of the porous polymer film or to one side of the porous polymer film. The porous polymer film is one of a polyethylene base film, a polypropylene/polyethylene/polypropylene composite base film, a polyimide base film, a nanometer glue base film, a polyethylene non-woven base film, a polypropylene non-woven base film or a polyimide non-woven base film. Step S3), drying to obtain the composite diaphragm. The nanometer glue and the attapulgite nanometer ceramic fiber in the diaphragm layer are randomly stacked and arranged, pores with the average pore diameter of 0.05-0.5 micrometer are formed, and the thickness of the diaphragm layer ranges from 9-20 micrometers.
The following will specifically describe the preparation method of the composite separator of the present invention with reference to specific examples.
Example 1 this example is a common method of making membranes, alumina particle membranes.
20g of alumina particles, 0.6g of sodium carboxymethylcellulose and 40g of deionized water are stirred in a high-speed disperser at 3000 rpm for 1 hour. 0.5g of fluoroalkyl methoxy ether alcohol, 0.4g of sodium carboxymethylcellulose, 3g of polyacrylate and 16g of deionized water were again added and stirred at 2000 rpm for 3 hours. The resulting slurry was single-side coated on a 12 micron thick polyethylene film using a microgravure coater and dried at 60 ℃ to give a composite membrane of alumina particles having a total thickness of 16 microns, labeled as S1.
Example 2, this example is a method for preparing a composite membrane of a nano-gel and alumina particles.
20g of alumina particles, 0.6g of sodium carboxymethylcellulose and 40g of deionized water are stirred in a high-speed disperser at 3000 rpm for 1 hour. 10g of the nano-latex emulsion, 0.5g of the fluoroalkyl methoxy ether alcohol, 0.4g of the sodium carboxymethyl cellulose, 3g of the polyacrylate and 16g of deionized water were added again, and the mixture was stirred at 2000 rpm for 3 hours. The slurry was single-side coated on a 12 μm thick polyethylene film using a microgravure coater and dried at 60 ℃ to obtain a composite membrane of a nanogel and alumina particles having a total thickness of 16 μm, which was labeled as S2.
Example 3 this example is a method of making a composite separator of the present invention.
Step S11) 20g of attapulgite nano ceramic fiber powder, 0.6g of sodium carboxymethyl cellulose and 30g of deionized water were stirred in a high-speed disperser at a rotation speed of 3000 rpm for 1 hour.
Step S12), adding 10g of nano latex emulsion, 0.5g of fluoroalkyl methoxy ether alcohol, 0.4g of sodium carboxymethyl cellulose, 3.5g of polyvinyl acetate and 10g of deionized water again, and stirring at 2000 rpm for 3 hours to obtain mixed slurry.
Step S2) the resulting mixed slurry was double-coated on a 12 μm thick polyethylene film using a microgravure coater to form a separator layer.
Step S3), drying at the temperature of 60 ℃ to obtain the composite diaphragm of the nanometer glue and the attapulgite nanometer ceramic fiber with the total thickness of 16 microns, and marking as S3.
The composite separators of examples 1 to 3 were subjected to the performance test below, and the test results are shown in table 1 below.
Table 1: and (3) testing the performance of each of the composite diaphragm samples S1, S2 and S3.
As can be seen from table 1, after the composite separator of example 3 is assembled into a battery core and is subjected to liquid injection and hot pressing, the peel strength between the separator and the pole piece is the highest, and the thermal shrinkage performance is better than that of the composite separators of examples 1 and 2. The peel strength of the coating and the tensile strength of the diaphragm are also obviously improved. Therefore, the mechanical property and the thermal shrinkage property of the composite diaphragm obtained by the method are improved, and the adhesive force between the composite diaphragm and the lithium battery pole piece is improved. Meanwhile, the composite diaphragm has excellent electrolyte liquid absorption and retention capacity through the porosity.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The mixed slurry for preparing the composite diaphragm is characterized by comprising the following components in percentage by mass
The nanometer glue is of a spherical structure, and the diameter of the nanometer glue is 100-150 nanometers; wherein the nanometer glue is one or a combination of polyvinylidene fluoride, vinylidene fluoride and hexafluoropropylene copolymer;
the surfactant is one or a mixture of more of fluoroalkyl methoxy ether alcohol, fluoroalkyl ethoxy ether alcohol, polyoxyethylene alkyl amide and fatty alcohol-polyoxyethylene ether;
the nano-colloids in the diaphragm layer and the attapulgite nano-ceramic fibers are randomly stacked and arranged, and pores with the average pore diameter of 0.05-0.5 micrometer are formed.
2. The mixed slurry for preparing the composite diaphragm of claim 1, wherein the attapulgite nano ceramic fibers have an average length of 0.5 to 2 micrometers and an average diameter of 0.05 to 0.3 micrometers.
3. The mixed slurry for preparing the composite diaphragm as claimed in claim 1, wherein the binder is one or a mixture of more of polyacrylate, polyvinyl alcohol, ethylene-vinyl acetate copolymer, polyvinyl acetate, styrene-butadiene latex, styrene-acrylic latex, pure benzene latex, or polyurethane.
4. The mixing slurry for preparing a composite separator according to claim 1, wherein the dispersant is one or more of water-soluble polybranched alcohol, sodium carboxymethylcellulose, triethyl phosphate, polyacrylic acid, sodium polyacrylate, polyethylene glycol, polyethylene oxide, and hydroxyethyl cellulose.
5. The preparation method of the composite diaphragm is characterized by comprising the following steps:
step S1) preparing the mixed slurry of any one of claims 1 to 4;
step S2) coating the mixed slurry on the surface of a porous polymer film to form a diaphragm layer of nano-colloid and attapulgite nano-ceramic fibers;
step S3), drying to obtain the composite diaphragm.
6. The method of manufacturing a composite separator according to claim 5, comprising the steps of: the step S1) includes the steps of:
step S11), dissolving the attapulgite nano ceramic fiber and a dispersing agent in a solvent, and fully stirring;
step S12), adding the nano-gel, the adhesive and the surfactant into the solution obtained in the step S11), and fully mixing and stirring to obtain the mixed slurry.
7. The method of claim 5, wherein the porous polymer film is one of a polyethylene-based film, a polypropylene/polyethylene/polypropylene composite-based film, a polyimide-based film, a nano-gel-based film, a polyethylene non-woven fabric-based film, a polypropylene non-woven fabric-based film, or a polyimide non-woven fabric-based film.
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| CN108963163B (en) * | 2018-08-01 | 2021-08-10 | 河北金力新能源科技股份有限公司 | Oily PVDF slurry, preparation process and coating method thereof |
| CN109167013A (en) * | 2018-08-31 | 2019-01-08 | 深圳市星源材质科技股份有限公司 | Coating fluid, lithium ion battery separator and lithium ion battery for lithium ion battery |
| CN109148794B (en) * | 2018-08-30 | 2021-03-23 | 上海力信能源科技有限责任公司 | Oily ceramic slurry for diaphragm, preparation method of oily ceramic slurry and diaphragm |
| CN109167005A (en) * | 2018-08-31 | 2019-01-08 | 深圳市星源材质科技股份有限公司 | Composite diaphragm and preparation method thereof |
| CN109192910A (en) * | 2018-09-11 | 2019-01-11 | 江苏清陶能源科技有限公司 | A kind of oiliness coating and nano ceramic fibers composite diaphragm and preparation method thereof |
| CN108854577A (en) * | 2018-09-14 | 2018-11-23 | 天津工业大学 | A kind of preparation method of the tubular membrane of PI non-woven cloth support tube |
| CN110724415A (en) * | 2019-09-02 | 2020-01-24 | 深圳市劢全新材料科技有限责任公司 | Composition, preparation method and application of composition in battery diaphragm coating material |
| KR20210031080A (en) * | 2019-09-11 | 2021-03-19 | 주식회사 엘지화학 | Separator for Secondary Battery with Excellent Electrolyte Impregnation |
| CN113410574A (en) * | 2020-11-19 | 2021-09-17 | 华东理工大学 | Polyvinyl alcohol-attapulgite composite nanofiber membrane and preparation method thereof |
| CN114784451A (en) * | 2022-04-27 | 2022-07-22 | 湖南烁普新材料有限公司 | Lithium ion battery diaphragm slurry, preparation method thereof and lithium ion battery composite diaphragm |
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| CN104681819B (en) * | 2014-12-25 | 2017-02-08 | 江苏清陶能源科技有限公司 | Attapulgite clay slurry for lithium ion batteries |
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