CN114843703A - Battery diaphragm with irregular-shaped particle coating and preparation method thereof - Google Patents
Battery diaphragm with irregular-shaped particle coating and preparation method thereof Download PDFInfo
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- CN114843703A CN114843703A CN202210550603.3A CN202210550603A CN114843703A CN 114843703 A CN114843703 A CN 114843703A CN 202210550603 A CN202210550603 A CN 202210550603A CN 114843703 A CN114843703 A CN 114843703A
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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
- H01M50/431—Inorganic 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
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/443—Particulate material
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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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- Inorganic Chemistry (AREA)
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Abstract
The invention relates to a battery diaphragm with an irregular-shaped particle coating and a preparation method thereof, and the battery diaphragm comprises a diaphragm base film and a coating coated on the surface of the diaphragm base film, wherein irregular-shaped particles are uniformly distributed in the coating; the structure of the irregular-shaped particles comprises spherical particles with PMMA coated on the surfaces of inorganic particles and a polymer layer which is formed by swelling and polymerizing the PMMA coated on the surfaces of the spherical particles, wherein the glass transition temperature of the polymer layer is more than 85 ℃; dispersing the irregular-shaped particles in water, adding an aqueous thickening agent, an aqueous adhesive and an aqueous wetting agent under stirring, uniformly stirring to obtain slurry, uniformly coating the slurry on one side or two sides of the diaphragm substrate, drying, and rolling to obtain the battery diaphragm with the irregular-shaped particle coating. The hot-pressing peeling strength between the coating and the pole piece is good, and the heat resistance is good.
Description
Technical Field
The invention relates to the technical field of battery separators with coatings, in particular to a battery separator with an irregular-shaped particle coating and a preparation method thereof.
Background
The battery diaphragm is one of four main constituent materials of a lithium battery, and mainly has the functions of separating a positive electrode from a negative electrode and adsorbing electrolyte to allow lithium ions to pass through. For the lithium battery of the 3C product, only a polyolefin diaphragm, such as a PP diaphragm, a PE diaphragm and the like, is used, and the battery performance can be basically met. However, in recent years, with the vigorous development of the new energy automobile industry, higher requirements are put on the performance of the separator used in the power battery, such as adhesion between the separator and the pole piece, better heat resistance and the like.
The polyolefin diaphragm is the most widely applied lithium battery diaphragm at present, but the existing polyolefin diaphragm on the market has the problems of insufficient electrophilic electrolyte performance and poor heat resistance. In order to solve the problems of insufficient performance and poor heat resistance of electrophilic electrolyte of polyolefin membranes, the main current solution is to coat a PVDF coating on one or both sides of the polyolefin membrane after coating ceramic, and the PVDF has the problems of high price, short supply and the like. With such a large background, more and more suppliers are beginning to look for materials that can replace PVDF. PMMA (polymethyl methacrylate) is one of hot spots due to the affinity to electrolyte, low price and easy control of glass transition temperature.
In order to synchronously finish ceramic coating and adhesive coating, the main method at present is to coat inorganic particles by PMMA, and common regular spherical coating particles can well realize one-time coating to ensure that a coating film and a pole piece have higher cohesiveness, but the heat resistance of the coating film is difficult to further improve, so that a battery has larger potential safety hazard.
Disclosure of Invention
In order to solve the technical problem of poor heat resistance of the polyolefin diaphragm, the battery diaphragm with the irregular-shaped particle coating and the preparation method thereof are provided. The hot-pressing peeling strength between the coating and the pole piece is good, and the heat resistance is good.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a battery diaphragm with irregular-shaped particle coating comprises a diaphragm base film and a coating layer coated on the surface of the diaphragm base film, wherein irregular-shaped particles are uniformly distributed in the coating layer;
the structure of the irregular-shaped particles comprises spherical particles with PMMA coated on the surface of inorganic particles and a polymer layer polymerized after the PMMA coated on the surface is partially swelled, wherein the glass transition temperature of the polymer layer is more than 85 ℃.
Further, the inorganic particles are titanium dioxide, silicon dioxide or aluminum oxide, and thus the spherical particles may be TiO 2 The surface is coated with PMMA, SiO 2 Surface coated with PMMA or Al 2 O 3 Coating PMMA on the surface; the polymer layer is polyacrylonitrile; the membrane base membrane is a polyolefin membrane and can be of a single-side coating or double-side coating structure.
Further, the preparation of the irregularly shaped particles comprises the following steps: dispersing spherical particles with PMMA coated on the surfaces of inorganic particles in water, adding a polymerizable monomer solvent for swelling at normal temperature after nitrogen is deoxidized, then heating to 60-120 ℃, adding an initiator for polymerization reaction, and obtaining irregular-shaped particles after solid-liquid separation.
Still further, the spherical particles are TiO 2 The surface is coated with PMMA, SiO 2 Surface coated with PMMA or Al 2 O 3 Coating PMMA on the surface; the polymerizable monomer solvent is acrylonitrile; the initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, potassium persulfate, benzoyl peroxide tert-butyl ester and methyl ethyl ketone peroxide.
Further, the swelling time is 30min-4 h; the temperature of the polymerization reaction is 65-90 ℃ and the time is 1-5 h; the time for deoxidizing the nitrogen is at least 10 min.
Still further, the solid content of a dispersion liquid formed after the spherical particles are dispersed in water is 6-10 wt%; the dosage proportion of the spherical particles, the polymerizable monomer solvent and the initiator is as follows; (15-25):(1-5):(0.0025-0.02).
Still further, the irregularly shaped particlesThe coating layer is formed by coating slurry on the surface of the base membrane of the diaphragm in an amount of 2-5g/m, wherein the coating slurry accounts for 10-50 wt% of the slurry for forming the coating layer 2 Preferably, the coating amount is 3g/m 2 。
In another aspect, the present invention provides a method for preparing the battery separator with the irregular-shaped particle coating layer, including the following steps: dispersing the irregular-shaped particles in water, adding an aqueous thickening agent, an aqueous adhesive and an aqueous wetting agent under stirring, uniformly stirring to obtain slurry, uniformly coating the slurry on one side or two sides of the diaphragm substrate, drying, and rolling to obtain the battery diaphragm with the irregular-shaped particle coating.
Further, the slurry comprises, by mass, 100%, 10-50% of the irregularly-shaped particles, 30-40% of the aqueous thickener, 3-8% of the aqueous binder, 0.05-0.5% of the aqueous wetting agent, and the balance of water; the stirring speed is 200-800rpm, and the stirring time is 30min-5 h.
Further, the aqueous thickener is carboxymethyl cellulose; the aqueous adhesive is an acrylic adhesive; the aqueous wetting agent is a mixture of an ethoxylated alcohol and acetylene glycol.
The beneficial technical effects are as follows: existing ordinary spherical TiO 2 The PMMA particle coated battery diaphragm can meet the requirement of high hot-pressing peeling strength between the PMMA particle coated battery diaphragm and a pole piece, but the heat resistance of the coated film is poor, and the shrinkage of the PMMA particle coated battery diaphragm can cause direct contact short circuit of a positive electrode and a negative electrode when the temperature is increased in the use process of the battery, so that the battery has great potential safety hazard. The invention is in the spherical TiO 2 The surface of PMMA particle is polymerized into irregular TiO after being partially swelled by adopting polymerizable solvent monomer 2 The PMMA/PAN particles have larger contact area than the spherical particles in irregular shapes, can be arranged in a coating layer more closely, can well resist the shrinkage force of the base film generated by heating when being heated, so that the thermal shrinkage rate of the diaphragm is lower, the heat resistance of the diaphragm is improved, and the safety of the battery is ensured.
Drawings
FIG. 1 shows irregularly shaped TiO 2 /PMMA/PASynthetic technique scheme for N particles.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The experimental methods of the following examples, which are not specified under specific conditions, are generally determined according to national standards; if no corresponding national standard exists, the method is carried out according to the universal international standard or the standard requirement proposed by related enterprises. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
Example 1
A battery diaphragm with an irregular-shaped particle coating comprises a PP (polypropylene) base film and a coating coated on the surface of the PP base film, irregular-shaped particles are uniformly distributed in the coating, and the structure of the irregular-shaped particles comprises TiO 2 Spherical particles coated with PMMA (hereinafter abbreviated as TiO) 2 PMMA) and a PAN polymer layer polymerized after partial swelling of the surface-coated PMMA, the irregularly shaped particles being abbreviated to TiO 2 /PMMA/PAN。
Wherein the irregularly shaped particlesThe preparation method comprises the following steps: adding TiO into the mixture 2 PMMA spherical particles are dispersed in water to form a dispersion with a solids content of 8 wt.%, N 2 Bubbling for 30min, removing oxygen, adding AN, swelling at normal temperature, heating to 65 ℃, adding KPS initiator to carry out polymerization reaction for 2h, and polymerizing reaction raw material TiO 2 The mass ratio of PMMA spherical particles to AN to KPS is 20:1:0.02, cooling is carried out after the reaction is finished, and TiO is obtained after solid-liquid separation 2 the/PMMA/PAN irregular-shaped particles are shown in a technical scheme as figure 1;
wherein the TiO is 2 The preparation process of PMMA spherical particles is TiO 2 As core, soap-free emulsion polymerization to give core-shell TiO 2 PMMA particles: deionized water, N, was added to a 250mL three-necked flask 2 Bubbling for 0.5h, adding TiO according to the mass ratio of 99:1 2 And KH-570 (deionized water: (TiO)) 2 + KH-570) ═ 9:1, mass ratio), stirring at 35 ℃ for 0.5 h; TiO according to mass ratio 2 MMA monomer and NaSS (sodium p-styrene sulfonate) are slowly added into MMA and NaSS (3: 2: 0.04) to react for 2 hours at 35 ℃, MMA and KPS solution are slowly added into the reactor according to the mass ratio of MMA to KPS being 1:0.015, the temperature is raised to 65 ℃ to carry out polymerization reaction for 2 hours, and then the mixture is cooled and centrifugally washed for 2 times to obtain TiO 2 PMMA particles.
Preparation of battery separator with irregular-shaped particle coating: adding TiO into the mixture 2 Dispersing the PMMA/PAN irregular-shaped particles in water, stirring at the speed of 400-600rpm for 30-60min, adding the aqueous thickener carboxymethyl cellulose, and continuing stirring for 60 min; adding a water-based acrylic acid adhesive, stirring at the speed of 200-300rpm for 30-60min, adding a mixture of water-based wetting agent ethoxylated alcohol and acetylene glycol, continuously stirring for 30-60min, and uniformly stirring to obtain slurry, wherein the TiO is 100% of the slurry in percentage by mass 2 20% of/PMMA/PAN irregularly-shaped particles, 35% of the aqueous thickening agent, 4% of the aqueous binder, 0.1% of the aqueous wetting agent and the balance of water;
and uniformly coating the slurry on one side of a diaphragm substrate, drying and rolling to obtain the battery diaphragm with the irregular-shaped particle coating.
Example 2
This implementationExample battery separator having irregular-shaped particle coating layer the structure was the same as that of example 1, except that, in the preparation of the battery separator having irregular-shaped particle coating layer, the slurry was 100% by mass of the TiO 2 25% of/PMMA/PAN irregular-shaped particles, 30% of water-based thickening agent, 4% of water-based adhesive, 0.2% of water-based wetting agent and the balance of water.
Example 3
The structure of the battery separator having a coating layer of irregularly shaped particles of this example was the same as that of example 1, except that, in the preparation of the battery separator having a coating layer of irregularly shaped particles, the slurry was 100% by mass of the TiO 2 25% of/PMMA/PAN irregular-shaped particles, 35% of water-based thickening agent, 8% of water-based adhesive, 0.3% of water-based wetting agent and the balance of water.
Comparative example 1
The battery separator of this comparative example was constructed as in example 1, except that TiO was used 2 PMMA spherical particle replacing TiO 2 Irregular shaped particles of/PMMA/PAN (i.e. in obtaining TiO) 2 No AN added after PMMA spherical particles and no subsequent swelling-polymerization process), the TiO is calculated according to 100 percent of mass 2 25% of PMMA spherical particles, 30% of water-based thickening agent, 7% of water-based adhesive, 0.3% of water-based wetting agent and the balance of water.
The separators of the above examples and comparative examples were subjected to performance tests, and the results are shown in table 1.
TABLE 1 separator Properties of examples and comparative examples
As can be seen from Table 1, comparative examples 1, 2, and 3 and comparative example 1 have TiO 2 The coating diaphragm of/PMMA/PAN irregular-shaped particles can be matched with the coating diaphragm with common spherical TiO under the condition of controlling the same areal density 2 The PMMA particle coating diaphragm achieves the same effect of adhering the pole piece.From the results of the thermal shrinkage test, it was found that TiO was used 2 The thermal shrinkage rate of the coating diaphragm of the/PMMA/PAN irregular-shaped particles is smaller than that of the coating diaphragm of the common spherical TiO 2 Coated membranes of PMMA particles, i.e. with TiO 2 The heat resistance of the/PMMA/PAN irregular-shaped coating diaphragm is relatively good.
In conclusion, compared with the common spherical TiO 2 PMMA coated diaphragm and special-shaped TiO prepared by the invention 2 The PMMA/PAN coated diaphragm has higher hot-pressing peeling strength and better heat resistance.
The above only shows the case of titanium dioxide as a coating for the preparation of irregularly shaped particles, and the skilled person in the art, in the face of the same technical problem, can also choose other inorganic particles to prepare, such as silica, alumina, etc. as mentioned in the present application.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. The battery separator with the irregular-shaped particle coating is characterized by comprising a separator base film and a coating coated on the surface of the separator base film, wherein irregular-shaped particles are uniformly distributed in the coating;
the structure of the irregular-shaped particles comprises spherical particles with PMMA coated on the surface of inorganic particles and a polymer layer polymerized after the PMMA coated on the surface is partially swelled, wherein the glass transition temperature of the polymer layer is more than 85 ℃.
2. The battery separator having a coating of irregularly shaped particles of claim 1, wherein the inorganic particles are titanium dioxide, silicon dioxide, or aluminum oxide; the polymer layer is polyacrylonitrile; the diaphragm basement membrane is a polyolefin diaphragm.
3. The battery separator with a coating of irregularly shaped particles of claim 1, wherein the preparation of the irregularly shaped particles comprises the steps of:
dispersing spherical particles with PMMA coated on the surfaces of inorganic particles in water, adding a polymerizable monomer solvent for swelling at normal temperature after nitrogen is deoxidized, then heating to 60-120 ℃, adding an initiator for polymerization reaction, and obtaining irregular-shaped particles after solid-liquid separation.
4. The battery separator having a coating of irregularly shaped particles of claim 3 in which the spherical particles are TiO 2 The surface is coated with PMMA, SiO 2 Surface coated with PMMA or Al 2 O 3 Coating PMMA on the surface; the polymerizable monomer solvent is acrylonitrile; the initiator is one or more of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, ammonium persulfate, potassium persulfate, benzoyl peroxide tert-butyl ester and methyl ethyl ketone peroxide.
5. The battery separator with the coating of irregularly shaped particles of claim 3, wherein the swelling time is 30min to 4 h; the temperature of the polymerization reaction is 65-90 ℃ and the time is 1-5 h; the time for deoxidizing the nitrogen is at least 10 min.
6. The battery separator having a coating of irregularly shaped particles of claim 5, wherein the dispersion of the spherical particles in water has a solids content of 6 to 10 wt.%; the mass ratio of the spherical particles, the polymerizable monomer solvent and the initiator is (15-25): 1-5): 0.0025-0.02.
7. The battery separator having a coating layer of irregularly shaped particles as claimed in any of claims 1 to 5, wherein the irregularly shaped particles are present in the slurry forming the coating layer in a proportion of 10 to 50 wt.%, and the slurry is formed by a slurryThe coating amount of the material on the surface of the diaphragm base film is 2-5g/m 2 。
8. The method for preparing a battery separator with a coating of irregularly shaped particles according to any of claims 1 to 7, comprising the following steps: dispersing the irregular-shaped particles in water, adding an aqueous thickening agent, an aqueous adhesive and an aqueous wetting agent under stirring, uniformly stirring to obtain slurry, uniformly coating the slurry on one side or two sides of the diaphragm substrate, drying, and rolling to obtain the battery diaphragm with the irregular-shaped particle coating.
9. The preparation method according to claim 8, wherein the slurry comprises, by mass, 100%, 10 to 50% of the irregularly shaped particles, 30 to 40% of the aqueous thickener, 3 to 8% of the aqueous binder, 0.05 to 0.5% of the aqueous wetting agent, and the balance of water; the stirring speed is 200-800rpm, and the stirring time is 30min-5 h.
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| CN202210550603.3A CN114843703B (en) | 2022-05-18 | 2022-05-18 | Battery separator with irregularly-shaped particle coating and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449141A (en) * | 2015-12-24 | 2016-03-30 | 深圳中兴创新材料技术有限公司 | Preparation method of battery diaphragm and battery membrane |
| CN112142995A (en) * | 2020-08-24 | 2020-12-29 | 深圳市德立新材料科技有限公司 | Organic-inorganic composite grape particle structure material, slurry, diaphragm and preparation method |
| CN113131094A (en) * | 2021-03-01 | 2021-07-16 | 东莞市溢兴新材料科技有限公司 | High-adhesion polymer coating diaphragm and preparation method thereof |
| CN114361706A (en) * | 2021-12-29 | 2022-04-15 | 上海恩捷新材料科技有限公司 | Coated diaphragm and preparation method thereof |
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- 2022-05-18 CN CN202210550603.3A patent/CN114843703B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105449141A (en) * | 2015-12-24 | 2016-03-30 | 深圳中兴创新材料技术有限公司 | Preparation method of battery diaphragm and battery membrane |
| CN112142995A (en) * | 2020-08-24 | 2020-12-29 | 深圳市德立新材料科技有限公司 | Organic-inorganic composite grape particle structure material, slurry, diaphragm and preparation method |
| CN113131094A (en) * | 2021-03-01 | 2021-07-16 | 东莞市溢兴新材料科技有限公司 | High-adhesion polymer coating diaphragm and preparation method thereof |
| CN114361706A (en) * | 2021-12-29 | 2022-04-15 | 上海恩捷新材料科技有限公司 | Coated diaphragm and preparation method thereof |
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