CN111224043A - PVDF ceramic modified diaphragm and preparation method thereof - Google Patents
PVDF ceramic modified diaphragm and preparation method thereof Download PDFInfo
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- CN111224043A CN111224043A CN202010053295.4A CN202010053295A CN111224043A CN 111224043 A CN111224043 A CN 111224043A CN 202010053295 A CN202010053295 A CN 202010053295A CN 111224043 A CN111224043 A CN 111224043A
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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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of lithium battery diaphragms, and particularly relates to a PVDF ceramic modified diaphragm and a preparation method thereof. The PVDF ceramic modified diaphragm comprises: the PVDF ceramic modified layer is positioned on the surface of the base membrane layer; wherein the PVDF ceramic modified layer is suitable for being grafted to the surface of the base membrane layer through a crosslinking mode. According to the PVDF ceramic modified diaphragm and the preparation method thereof, the PVDF and the ceramic are modified together to modify the base film, and the chemical bond is used for connecting instead of bonding with the binder, so that the risk of falling off of a PVDF ceramic modified layer is eliminated, the heat resistance, the electrolyte affinity and the bonding force with a pole piece of the modified diaphragm are ensured, and the good and stable electrical property of a lithium ion battery is guaranteed.
Description
Technical Field
The invention belongs to the technical field of lithium battery diaphragms, and particularly relates to a PVDF ceramic modified diaphragm and a preparation method thereof.
Background
Lithium ion batteries are increasingly used in the field of power, such as electric vehicles; the method is applied to the 3C field, such as mobile phones and tablet computers; the electric tool is applied to the field of electric tools, such as various handheld electric tools. Along with the expansion of the application range, the market has higher and higher requirements on the performance of the lithium ion battery, and further, higher requirements are provided for the lithium ion battery diaphragm.
Due to poor electrolyte affinity, poor adhesion with a pole piece and poor heat resistance of the lithium ion battery diaphragm, the lithium ion battery has high internal resistance, the diaphragm is easy to separate from the pole piece, and internal short circuit is easy to generate in the charging and discharging processes of the lithium ion battery, so that the charging and discharging efficiency, the cycle life and other performances and safety performances of the battery are reduced. In the industry, ceramic coatings are mostly used for increasing the heat resistance and the affinity to electrolyte of base films, PVDF (polyvinylidene fluoride) coatings are coated on the ceramic coatings to improve the adhesion between the base films and pole pieces, but a plurality of coatings are accumulated through adhesives, when the adhesives fail in the electrolyte for a long time, the coatings fall off, and then the electrical property and the safety performance of the battery are greatly reduced.
The invention provides a novel solution, the PVDF and the ceramic are changed to modify the base membrane together, and the chemical bond is used for connecting instead of bonding with the binder, so that the risk of falling off of the modified coating is eliminated, the heat resistance, the electrolyte affinity and the bonding force with the pole piece of the modified diaphragm are ensured, and the good and stable electrical property of the lithium ion battery is ensured.
Disclosure of Invention
The invention aims to provide a PVDF ceramic modified diaphragm and a preparation method thereof.
In order to solve the above technical problems, the present invention provides a PVDF ceramic modified membrane, comprising: the PVDF ceramic modified layer is positioned on the surface of the base membrane layer; wherein the PVDF ceramic modified layer is suitable for being grafted to the surface of the base membrane layer through a crosslinking mode.
Further, the base film layer includes a polyolefin separator containing a C — H bond; the crosslinking mode comprises the following steps: c atoms of C-H bonds in the base film layer and C atoms in the cross-linking agent form C-C bonds; c atoms in the cross-linking agent and C atoms in the PVDF ceramic modified layer form C-C bonds, namely the PVDF ceramic modified layer is grafted to the surface of the base membrane layer; and PVDF particles in the PVDF ceramic modified layer are connected with a cross-linking agent through C-C bonds to form a three-dimensional network structure.
Further, the PVDF ceramic modified layer comprises the following raw materials in parts by mass: PVDF particles: 1-30 parts; ceramic particles: 5-45 parts; a crosslinking agent: 0.1-30 parts; solvent: 50-95 parts; other auxiliary agents: 0.1-20 parts; wherein the mass ratio of the PVDF particles to the ceramic particles is 1: (0.5-20).
Further, the PVDF particles include: PVDF single particles or PVDF multi-particle aggregates; wherein the particle size of the PVDF single particles is 0.1-0.5 μm; the particle size of the PVDF multi-particle aggregate is 0.5-5 mu m.
Further, the ceramic particles include: ceramic single particles or ceramic multi-particle agglomerates; wherein the particle size of the ceramic single particles is 0.1-2 μm; the particle size of the ceramic multi-particle aggregate is 0.5-5 mu m.
Further, the cross-linking agent contains carbon, fluorine and hydrogen elements.
Further, the solvent comprises any one of deionized water, acetone and N-methyl pyrrolidone; the other auxiliary agents comprise one or more of a dispersing agent, a wetting agent, a stabilizing agent and a defoaming agent.
Further, the porosity of the three-dimensional network structure is 30-80%; the aperture of the three-dimensional reticular structure is 0.01-0.1 mu m; and the thickness of the three-dimensional network structure is 0.1-5 μm.
Further, the peel strength of the three-dimensional reticular structure and the base film layer is not lower than 50N/m; the thermal shrinkage of the PVDF ceramic modified membrane at 130 ℃/1h is not more than 4%.
In another aspect, the invention further provides a preparation method of the PVDF ceramic modified membrane, which comprises the following steps: preparing PVDF ceramic modified emulsion; and coating the PVDF ceramic modified emulsion on a base membrane, and drying to form a PVDF ceramic modified layer so as to obtain the PVDF ceramic modified membrane.
The PVDF ceramic modified diaphragm has the beneficial effects that the PVDF ceramic modified layer is grafted to the surface of the base membrane layer in a cross-linking mode, the base membrane is modified by changing PVDF and ceramic together, and chemical bond connection is used for replacing bonding of a bonding agent, so that the risk of falling off of the PVDF ceramic modified layer is eliminated, the PVDF ceramic modified diaphragm has the advantages of good electrolyte affinity, heat resistance, stronger bonding force with an electrode plate and the like, and a lithium ion battery prepared by the diaphragm has higher charge and discharge efficiency and better cycle performance.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, not all of the embodiments. 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.
Example 1
This example 1 provides a PVDF ceramic modified membrane, including: the PVDF ceramic modified layer is positioned on the surface of the base membrane layer; wherein the PVDF ceramic modified layer is suitable for being grafted to the surface of the base membrane layer through a crosslinking mode. According to the PVDF ceramic modified diaphragm, the PVDF and ceramic are modified together to modify the base membrane, and chemical bond connection is used for replacing bonding of a binder, so that the risk of falling off of a PVDF ceramic modified layer is eliminated.
Specifically, the base film layer comprises a polyolefin separator containing C-H bonds; the crosslinking mode comprises the following steps: c atoms of C-H bonds in the base film layer and C atoms in the cross-linking agent form C-C bonds; c atoms in the cross-linking agent and C atoms in the PVDF ceramic modified layer form C-C bonds, namely the PVDF ceramic modified layer is grafted to the surface of the base membrane layer; and PVDF particles in the PVDF ceramic modified layer are connected with the cross-linking agent through C-C bonds to form a three-dimensional network structure, so that the connection mode of the PVDF ceramic modified layer and the base film is changed, the adhesion force of the diaphragm and the electrode plate is improved, and the PVDF ceramic modified layer is not easy to fall off. The PVDF particles in the PVDF ceramic modified layer have different sizes, the particles are connected through a cross-linking agent, and C atoms among the PVDF particles can also form C-C bonds with the cross-linking agent, so that the PVDF ceramic modified layer forms a three-dimensional network structure taking the PVDF particles as a support.
Optionally, the PVDF ceramic modification layer comprises the following raw materials in parts by mass: PVDF particles: 1-30 parts; ceramic particles: 5-45 parts; a crosslinking agent: 0.1-30 parts; solvent: 50-95 parts; other auxiliary agents: 0.1-20 parts; wherein the mass ratio of the PVDF particles to the ceramic particles is 1: (0.5-20).
Among them, the ceramic particles include, but are not limited to, silicon oxide, aluminum oxide, calcium oxide, titanium oxide, magnesium oxide, zinc oxide, chromium oxide, zinc oxide. When the diaphragm is heated and has a contraction tendency, the ceramic particles provide a supporting function, reduce the contraction and improve the heat resistance of the diaphragm and the safety of the battery.
In this embodiment, the PVDF particles include: PVDF single particles or PVDF multi-particle aggregates; wherein the particle size of the PVDF single particles is 0.1-0.5 μm; the particle size of the PVDF multi-particle aggregate is 0.5-5 mu m.
Optionally, the particle size of the PVDF single particle is 0.1 μm; the particle size of the PVDF multi-particle aggregate is 0.5 mu m.
Optionally, the particle size of the PVDF single particle is 0.5 μm; the particle size of the PVDF multi-particle aggregate is 5 mu m.
Optionally, the particle size of the PVDF single particle is 0.3 μm; the particle size of the PVDF multi-particle aggregate is 3 mu m.
In this embodiment, the ceramic particles include: ceramic single particles or ceramic multi-particle agglomerates; wherein the particle size of the ceramic single particles is 0.1-2 μm; the particle size of the ceramic multi-particle aggregate is 0.5-5 mu m.
Optionally, the particle size of the ceramic single particles is 0.1 μm; the particle size of the ceramic multi-particle aggregate is 0.5 mu m.
Optionally, the particle size of the ceramic single particle is 2 μm; the particle size of the ceramic multi-particle aggregate is 5 mu m.
Optionally, the particle size of the ceramic single particles is 1 μm; the particle size of the ceramic multi-particle aggregate is 3 mu m.
Optionally, the cross-linking agent contains carbon, fluorine and hydrogen elements. The C atoms in the crosslinking agent can easily react with the C atoms in the PVDF ceramic modified layer or the base film layer through the carbon, fluorine and hydrogen elements contained in the crosslinking agent.
Optionally, the solvent includes any one of deionized water, acetone, and N-methylpyrrolidone. The solvent can uniformly disperse the PVDF particles and the ceramic particles, and the PVDF particles and the other components in the PVDF ceramic modified emulsion are fully contacted to form uniform and stable PVDF ceramic modified emulsion.
Optionally, the other auxiliary agents comprise one or more of a dispersing agent, a wetting agent, a stabilizing agent and a defoaming agent. The uniformity, the wettability and the stability of the PVDF ceramic modified emulsion can be adjusted by other additives so as to ensure the performance of the PVDF ceramic modified emulsion.
In this embodiment, the porosity of the three-dimensional network structure is 30-80%; the aperture of the three-dimensional reticular structure is 0.01-0.1 mu m; and the thickness of the three-dimensional network structure is 0.1-5 μm.
In the embodiment, the porosity and the pore size of the three-dimensional network structure can be adjusted by different particle size combinations, modified layer densities and crosslinking degrees of PVDF particles and ceramic particles; the PVDF with large particle size has high content of particles, small modified layer density, low crosslinking degree, large gaps among the particles, less connection and large porosity and pore size; the PVDF particles with small particle size have high content, high modified layer density, high crosslinking degree, small gaps among the particles, more connections, and small porosity and pore size.
In this embodiment, the thickness of the three-dimensional network structure is suitable for being adjusted by the number of the cumulative PVDF single particles or the particle size of the PVDF multi-particle aggregate, the number of the cumulative ceramic single particles, or the particle size of the ceramic multi-particle aggregate. The three-dimensional network structure consists of PVDF particles and ceramic particles, when the particle size of the particles is small, the bulk density of the particles in unit area, namely the number of the stacked layers of the particles, is changed by controlling the surface density of the particles, so as to change the thickness of the PVDF ceramic modified layer, wherein the minimum thickness of the PVDF ceramic modified layer is the particle size of a single-layer particle; when the particle size is large, the larger particles play a supporting role, and the particle size is expressed by the thickness of the PVDF ceramic modified layer.
In the embodiment, the peel strength of the three-dimensional reticular structure and the base film layer is not lower than 50N/m; the thermal shrinkage of the PVDF ceramic modified membrane at 130 ℃/1h is not more than 4%.
Example 2
The embodiment 2 provides a preparation method of a PVDF ceramic modified membrane, which includes: preparing PVDF ceramic modified emulsion; and coating the PVDF ceramic modified emulsion on a base membrane, and drying to form a PVDF ceramic modified layer so as to obtain the PVDF ceramic modified membrane.
Optionally, the PVDF ceramic modified emulsion comprises the following raw materials in parts by mass: PVDF particles: 1-30 parts; ceramic particles: 5-45 parts; a crosslinking agent: 0.1-30 parts; solvent: 50-95 parts; other auxiliary agents: 0.1-20 parts. The other auxiliary agents comprise one or more of a dispersing agent, a wetting agent, a stabilizing agent and a defoaming agent. And mechanically mixing the raw materials, and uniformly stirring to obtain the PVDF ceramic modified emulsion.
In this embodiment, the coating method includes, but is not limited to, top coating, wherein the top coating process includes, but is not limited to, micro gravure coating and dip coating.
In this embodiment, the drying method includes, but is not limited to, drying and long-wave illumination, wherein the drying temperature is not lower than 80 ℃; the illumination wavelength is not less than 200 nm.
Example 3
1kg of PVDF ceramic particles, 10kg of ceramic particles, 30kg of cross-linking agent, 50kg of deionized water, 5kg of dispersing agent and 10kg of wetting agent are mixed to form the PVDF ceramic modified emulsion. Coating the PVDF ceramic modified emulsion on a base film through a micro-gravure, and drying to form a PVDF ceramic modified layer so as to obtain a PVDF ceramic modified diaphragm; the three-dimensional network structure of the PVDF ceramic modified diaphragm has the following characteristics: the porosity of the three-dimensional network structure is 30%; the aperture of the three-dimensional net structure is 0.03 mu m; the thickness of the three-dimensional network structure was 0.8. mu.m.
Example 4
15kg of PVDF granules, 15kg of ceramic granules, 10kg of a cross-linking agent, 60kg of acetone, 5kg of a stabilizer and 5kg of a defoaming agent were mixed to form a PVDF ceramic modified emulsion. Dipping the PVDF ceramic modified emulsion on a base membrane, and forming a PVDF ceramic modified layer after long-wave illumination, thereby obtaining a PVDF ceramic modified diaphragm; the three-dimensional network structure of the PVDF ceramic modified diaphragm has the following characteristics: the porosity of the three-dimensional network structure is 80%; the aperture of the three-dimensional net structure is 0.05 mu m; the thickness of the three-dimensional network structure was 3 μm.
Example 5
30kg of PVDF granules, 20kg of ceramic granules, 0.1kg of a crosslinking agent, 75kg of N-methylpyrrolidone and 0.1kg of a dispersing agent were mixed to form a PVDF ceramic modified emulsion. Coating the PVDF ceramic modified emulsion on a base film through a micro-gravure, and drying to form a PVDF ceramic modified layer so as to obtain a PVDF ceramic modified diaphragm; the three-dimensional network structure of the PVDF ceramic modified diaphragm has the following characteristics: the porosity of the three-dimensional network structure is 60%; the aperture of the three-dimensional net structure is 0.01 mu m; the thickness of the three-dimensional network structure was 0.1. mu.m.
Example 6
20kg of PVDF granules, 45kg of ceramic granules, 2.5kg of a cross-linking agent, 80kg of acetone, 2kg of a stabilizer and 3kg of a dispersant are mixed to form a PVDF ceramic modified emulsion. Dipping the PVDF ceramic modified emulsion on a base membrane, and forming a PVDF ceramic modified layer after long-wave illumination, thereby obtaining a PVDF ceramic modified diaphragm; the three-dimensional network structure of the PVDF ceramic modified diaphragm has the following characteristics: the porosity of the three-dimensional network structure is 50%; the aperture of the three-dimensional net structure is 0.1 mu m; the thickness of the three-dimensional network structure was 5 μm.
Example 7
10kg of PVDF particles, 5kg of ceramic particles, 5kg of cross-linking agent, 95kg of deionized water, 10kg of wetting agent and 10kg of defoaming agent are mixed to form the PVDF ceramic modified emulsion. Coating the PVDF ceramic modified emulsion on a base film through a micro-gravure, and drying to form a PVDF ceramic modified layer so as to obtain a PVDF ceramic modified diaphragm; the three-dimensional network structure of the PVDF ceramic modified diaphragm has the following characteristics: the porosity of the three-dimensional network structure is 55%; the aperture of the three-dimensional net structure is 0.07 mu m; the thickness of the three-dimensional network structure was 4 μm.
In summary, according to the PVDF ceramic modified diaphragm and the preparation method thereof, the PVDF ceramic modified layer is grafted to the surface of the base membrane layer in a cross-linking manner, the base membrane is modified by changing the PVDF and the ceramic together, and the chemical bond connection is used to replace the adhesive bonding, so that the risk of the PVDF ceramic modified layer falling off is eliminated, the PVDF ceramic modified diaphragm has the advantages of good electrolyte affinity, heat resistance, stronger adhesive force with an electrode plate and the like, and the lithium ion battery prepared by the diaphragm has higher charge and discharge efficiency and better cycle performance.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A PVDF ceramic modified membrane, comprising:
the PVDF ceramic modified layer is positioned on the surface of the base membrane layer; wherein
The PVDF ceramic modified layer is suitable for being grafted to the surface of the base membrane layer in a crosslinking mode.
2. The PVDF-modified membrane of claim 1,
the base film layer includes a polyolefin separator having a C-H bond;
the crosslinking mode comprises the following steps:
c atoms of C-H bonds in the base film layer and C atoms in the cross-linking agent form C-C bonds;
the C atoms in the cross-linking agent form C-C bonds with the C atoms in the PVDF ceramic modified layer, i.e.
Grafting a PVDF ceramic modified layer to the surface of a base membrane layer; and
PVDF particles in the PVDF ceramic modified layer are connected with a cross-linking agent through C-C bonds to form a three-dimensional network structure.
3. The PVDF ceramic modified membrane of claim 2,
the PVDF ceramic modified layer comprises the following raw materials in parts by mass:
the PVDF particles are: 1-30 parts;
ceramic particles: 5-45 parts;
the cross-linking agent: 0.1-30 parts;
solvent: 50-95 parts;
other auxiliary agents: 0.1-20 parts; wherein
The mass ratio of the PVDF particles to the ceramic particles is 1: (0.5-20).
4. The PVDF ceramic modified membrane of claim 3,
the PVDF particles comprise: PVDF single particles or PVDF multi-particle aggregates; wherein
The particle size of the PVDF single particles is 0.1-0.5 mu m;
the particle size of the PVDF multi-particle aggregate is 0.5-5 mu m.
5. The PVDF ceramic modified membrane of claim 3,
the ceramic particles include: ceramic single particles or ceramic multi-particle agglomerates; wherein
The granularity of the single ceramic particles is 0.1-2 mu m;
the particle size of the ceramic multi-particle aggregate is 0.5-5 mu m.
6. The PVDF ceramic modified membrane of claim 3,
the cross-linking agent contains carbon, fluorine and hydrogen elements.
7. The PVDF ceramic modified membrane of claim 3,
the solvent comprises any one of deionized water, acetone and N-methyl pyrrolidone;
the other auxiliary agents comprise one or more of a dispersing agent, a wetting agent, a stabilizing agent and a defoaming agent.
8. The PVDF ceramic modified membrane of claim 2,
the porosity of the three-dimensional network structure is 30-80%;
the aperture of the three-dimensional reticular structure is 0.01-0.1 mu m; and
the thickness of the three-dimensional reticular structure is 0.1-5 μm.
9. The PVDF ceramic modified membrane of claim 2,
the peel strength of the three-dimensional reticular structure and the base film layer is not lower than 50N/m;
the thermal shrinkage of the PVDF ceramic modified membrane at 130 ℃/1h is not more than 4%.
10. A preparation method of a PVDF ceramic modified diaphragm is characterized by comprising the following steps:
preparing PVDF ceramic modified emulsion;
and coating the PVDF ceramic modified emulsion on a base membrane, and drying to form a PVDF ceramic modified layer so as to obtain the PVDF ceramic modified membrane.
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| CN202010053295.4A CN111224043A (en) | 2020-01-17 | 2020-01-17 | PVDF ceramic modified diaphragm and preparation method thereof |
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| CN202010053295.4A CN111224043A (en) | 2020-01-17 | 2020-01-17 | PVDF ceramic modified diaphragm and preparation method thereof |
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| CN101989651A (en) * | 2009-07-29 | 2011-03-23 | 现代自动车株式会社 | Method for preparing cross-linked ceramic-coated separator containing ionic polymer, ceramic-coated separator prepared by the method, and lithium secondary battery using the same |
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| CN109360921A (en) * | 2018-09-17 | 2019-02-19 | 湖北江升新材料有限公司 | A kind of lithium ion battery ceramic diaphragm and manufacturing method |
| CN110277529A (en) * | 2019-06-28 | 2019-09-24 | 新乡市中科科技有限公司 | A kind of high multiplying power lithium ion battery functional composite membrane and preparation method thereof |
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| US20130130091A1 (en) * | 2007-05-30 | 2013-05-23 | Prologium Holding Inc. | Electricity supply element and ceramic separator thereof |
| CN101989651A (en) * | 2009-07-29 | 2011-03-23 | 现代自动车株式会社 | Method for preparing cross-linked ceramic-coated separator containing ionic polymer, ceramic-coated separator prepared by the method, and lithium secondary battery using the same |
| CN108690416A (en) * | 2017-03-29 | 2018-10-23 | 宋承原 | Macromolecule-ceramic hybrid coating composition and the accumulator separation film manufacturing method for using above-mentioned composition |
| CN109360921A (en) * | 2018-09-17 | 2019-02-19 | 湖北江升新材料有限公司 | A kind of lithium ion battery ceramic diaphragm and manufacturing method |
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