CN110048057B - Surface-modified PMMA/PVDF hybrid-coated lithium battery composite diaphragm and preparation method thereof - Google Patents
Surface-modified PMMA/PVDF hybrid-coated lithium battery composite diaphragm and preparation method thereof Download PDFInfo
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- CN110048057B CN110048057B CN201910228370.3A CN201910228370A CN110048057B CN 110048057 B CN110048057 B CN 110048057B CN 201910228370 A CN201910228370 A CN 201910228370A CN 110048057 B CN110048057 B CN 110048057B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—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
- H01M50/411—Organic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- 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 discloses a lithium battery composite diaphragm coated with a surface modified PMMA/PVDF mixture and a preparation method thereof; the composite diaphragm of the lithium battery comprises a battery diaphragm and a PMMA/PVDF mixed coating coated on one side or two sides of the battery diaphragm, wherein the PMMA/PVDF mixed coating comprises PMMA particles subjected to surface modification by a coupling agent and PVDF particles subjected to surface modification by the coupling agent. The invention adopts the coupling agent to modify the surfaces of PMMA and PVDF, solves the problems of nonuniform mixing and easy sedimentation of PMMA and PVDF, enables the coated film surface to be flat and high in yield, effectively improves the mechanical property and the adhesiveness of the diaphragm, increases the absorption of electrolyte and improves the ionic conductivity.
Description
Technical Field
The invention belongs to the field of lithium battery diaphragm materials, and particularly relates to a surface-modified PMMA/PVDF hybrid-coated lithium battery composite diaphragm and a preparation method thereof.
Background
The lithium battery has the advantages of high energy density, long cycle life and the like as a novel secondary battery, the application range of the lithium battery is continuously expanded, the lithium battery is widely applied to portable electronic devices, electric tools, energy storage and power automobiles, and particularly, the lithium battery is increasingly applied to the power automobiles along with the rapid development of new energy industries. However, the frequent occurrence of safety accidents of lithium batteries increasingly attracts people's attention. The diaphragm is used as an important component of the lithium battery, can effectively prevent the positive electrode and the negative electrode from contacting to generate short circuit, and has very important influence on the safety of the lithium battery, so that the performance of the lithium battery is improved and the safety requirement has higher requirement on the performance of the diaphragm.
The polyolefin diaphragm is the most widely used diaphragm of the lithium battery at present, but the existing polyolefin diaphragm in the market has the problems of insufficient adhesive property and electrolyte affinity. In order to improve the adhesion and electrolyte wettability of the polyolefin diaphragm, the main solution at present is to coat a PVDF coating on one or both surfaces of the polyolefin diaphragm, and the coating can improve the adhesion of the diaphragm to a certain extent and has good wettability with the electrolyte. With the development of lithium batteries, the requirement on the adhesion of the diaphragm is higher and higher, and a single PVDF coating cannot meet the corresponding requirement, so that the search for a next-generation high-end diaphragm with excellent adhesion performance becomes urgent.
Polymethyl methacrylate (PMMA), also known as acrylic, acrylic or organic glass, has high strength and excellent tensile and impact resistance. And the PMMA is mixed with the PVDF, so that the crystallinity of the PVDF can be influenced, the absorption of electrolyte is increased, the ionic conductivity is improved, and the mechanical property and the adhesion of the diaphragm can be improved.
However, the effect of mixing and coating PMMA and PVDF is not ideal, and the main problems are that the compatibility effect is poor, the PMMA and PVDF are easy to settle and are not uniformly mixed in the mixing process, the film surface is uneven in the coating process, and the yield is low.
Disclosure of Invention
In view of the above, the invention aims to provide a surface-modified PMMA/PVDF mixed coating lithium battery composite diaphragm and a preparation method thereof, which can effectively solve the problems that PVDF bonding performance is insufficient, crystallinity affects ion conductivity, PMMA electrolyte infiltration consistency is poor, and the like, and can also solve the problems that PMMA and PVDF are not uniformly mixed and are easy to settle.
In order to achieve the purpose, the invention provides the following technical scheme:
the surface-modified PMMA/PVDF hybrid-coated lithium battery composite membrane comprises a battery membrane and a PMMA/PVDF hybrid coating coated on one side or two sides of the battery membrane, wherein the PMMA/PVDF hybrid coating comprises PMMA particles subjected to surface modification by a coupling agent and PVDF particles subjected to surface modification by the coupling agent.
In the PMMA/PVDF mixed coating, the weight ratio of PMMA particles modified by the surface of the coupling agent to PVDF particles modified by the surface of the coupling agent can be adjusted according to the requirements of the application condition of the diaphragm, and the preferable weight ratio is 1:9-9: 1.
The coupling agent can be various conventional coupling agents, and as a preferable technical scheme, the coupling agent is selected from silane coupling agents, such as KH-550, KH-570, KH-580 and the like.
The PMMA/PVDF hybrid coating layer preferably has a thickness of 0.1-4 μm.
The battery diaphragm is a polyolefin-based diaphragm or a ceramic diaphragm coated with an inorganic ceramic particle coating on the polyolefin-based diaphragm; that is, the PMMA/PVDF hybrid coating may be directly coated on the polyolefin base film, or may be coated on the ceramic separator including the inorganic ceramic particle coating.
The polyolefin base film can be various conventional polyolefin base films, and as a preferred technical scheme, the polyolefin base film is a polyethylene film, a polypropylene film or a polypropylene/polyethylene/polypropylene composite film with the thickness of 5-40 mu m and the porosity of 30-80%.
The inorganic ceramic particles can be various conventional inorganic ceramic particles, and as a preferred technical scheme, the inorganic ceramic particles are one or more of aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide, magnesium oxide, zinc oxide and barium oxide, and the average particle size of the inorganic ceramic particles is 0.1-1 um; the thickness of the inorganic ceramic particle coating is preferably 1 to 4 μm.
The preparation method of the surface modified PMMA/PVDF mixed coated lithium battery composite diaphragm comprises the following steps:
(1) mixing PVDF powder, PMMA powder, a coupling agent, an auxiliary agent and water to prepare PMMA and PVDF slurry, and then mixing PMMA and PVDF slurry modified by a silane coupling agent according to a certain proportion to prepare PMMA/PVDF coating slurry;
(2) sending the battery diaphragm into a coating device, and coating by using the PMMA/PVDF mixed slurry prepared in the step (1);
(3) and (3) drying and rolling the battery diaphragm coated in the step (2) to obtain a finished product of the surface modified PMMA/PVDF mixed coated lithium battery composite diaphragm.
In the step (1), the preferable process conditions are that the mixed slurry contains 1-9 parts by weight of PVDF powder, 1-9 parts by weight of PMMA powder and 0.5-3 parts by weight of coupling agent.
In the step (1), the auxiliary agent may be selected from the auxiliary agents commonly used in coating slurry preparation, such as: dispersants, binders, wetting agents, and the like.
In the step (2), the coating manner is various conventional coating manners, such as: dip coating, spray coating, scraper, coating wire rod, and micro-concave roller coating.
The invention has the beneficial effects that:
1. according to the invention, the surfaces of PMMA and PVDF are modified by adopting the coupling agent, and the coupling agent is grafted to the surfaces of PMMA and PVDF, so that the specific surface energy between PMMA and PVDF is improved, the problems of nonuniform mixing and easy sedimentation of PMMA and PVDF are solved, the coated film surface is flat, and the yield is high.
2. The PMMA/PVDF mixed coating not only effectively improves the mechanical property and the adhesive property of the diaphragm, but also increases the absorption of electrolyte and improves the ionic conductivity.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a surface scanning electron micrograph of a separator of example 1;
FIG. 2 is a surface scanning electron micrograph of a separator of comparative example 4;
FIG. 3 is a schematic diagram of PMMA, PVDF surface modification.
Detailed Description
The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Example 1:
(1) preparing PMMA/PVDF mixed slurry: firstly, adding 1.55 parts of dispersing agent and 0.44 part of wetting agent into deionized water for complete dissolution, then adding 4.42 parts of PVDF powder, fully stirring, and grinding for 1 h; adding 4.42 parts of PMMA powder into the ground PVDF slurry, fully stirring, adding 1.5 parts of silane coupling agent as a surface modifier, fully stirring, grinding for 0.5h, and finally adding 0.88 part of adhesive;
(2) the battery diaphragm is a ceramic diaphragm of a 7-micron polyethylene base film and a 2-micron inorganic ceramic particle coating, the battery diaphragm is sent into a coating device, the PMMA/PVDF mixed slurry prepared in the step (1) is used for coating, and the PMMA/PVDF mixed slurry is coated on one side of the battery diaphragm in a micro-concave roller coating mode;
(3) and (3) drying and rolling the battery diaphragm coated in the step (2) to obtain a finished product of the surface modified PMMA/PVDF mixed coated lithium battery composite diaphragm.
Example 2:
the present embodiment is different from embodiment 1 in that: when PMMA/PVDF mixed slurry is prepared, 5.30 parts of PMMA powder, 3.54 parts of PVDF powder and 1.8 parts of silane coupling agent are used.
Example 3:
the present embodiment is different from embodiment 1 in that: when PMMA/PVDF mixed slurry is prepared, 7.07 parts of PMMA powder, 1.77 parts of PVDF powder and 1 part of silane coupling agent are used.
Example 4:
the present embodiment is different from embodiment 1 in that: when PMMA/PVDF mixed slurry is prepared, 1.25 parts of PMMA powder, 7.59 parts of PVDF powder and 2.5 parts of silane coupling agent are used.
Comparative example 1:
comparative example 1 differs from example 1 in that: and 8.84 parts of PMMA powder. Coating is carried out by using PMMA paste.
Comparative example 2:
comparative example 2 differs from example 1 in that: PVDF slurry is prepared, and 8.84 parts of PVDF powder is used. The coating was performed using PVDF slurry.
Comparative example 3:
comparative example 3 is a ceramic separator of 7 μm polyethylene-based film +2 μm inorganic ceramic particle coating.
Comparative example 4:
comparative example 4 differs from example 1 in that: when PMMA/PVDF mixed slurry is prepared, no silane coupling agent is added.
The separators obtained in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance tests under the same conditions, and the results are shown in table 1.
TABLE 1 comparative test results of lithium battery separator
From the adhesion properties of table 1, the pure PMMA coated membrane of comparative example 1 has excellent adhesion properties, the pure PVDF coated membrane of comparative example 2 has insufficient adhesion properties, and the PMMA/PVDF mixed coated membranes of examples 1 to 4 have more excellent adhesion properties.
From the ionic conductivities of table 1, the PMMA/PVDF mixed coated membranes of examples 1-4 significantly increased the electrolyte absorption and ionic conductivity, and from experimental data validation, the PMMA/PVDF mixed coated membranes had an order of magnitude higher ionic conductivity than the ceramic membrane of comparative example 3 and the pure PVDF coated membrane of comparative example 2.
The surface scanning electron microscope photo of the diaphragm of the embodiment 1 is shown in fig. 1, and the surface scanning electron microscope photo of the diaphragm of the comparative example 4 is shown in fig. 2, and it can be seen from the figure that although the diaphragm is a PMMA/PVDF mixed coating diaphragm, the mere PMMA and PVDF mixed coating effect of the comparative example 4 is not ideal, the dispersibility of PMMA and PVDF is not good, the agglomeration phenomenon is serious, the film surface is uneven, and the yield is low; in the embodiment 1, the surfaces of PMMA and PVDF are modified by using the coupling agent, and the coupling agent is grafted to the surfaces of PMMA and PVDF (as shown in figure 3), so that the specific surface energy between PMMA and PVDF is improved, the dispersibility of PMMA and PVDF is good, the agglomeration phenomenon is avoided, the film surface is flat, and the yield is high.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (9)
1. The surface-modified PMMA/PVDF hybrid-coated lithium battery composite membrane comprises a battery membrane and a PMMA/PVDF hybrid coating coated on one side or two sides of the battery membrane, and is characterized in that: the PMMA/PVDF mixed coating comprises PMMA particles subjected to surface modification by a coupling agent and PVDF particles subjected to surface modification by the coupling agent;
the preparation method of the lithium battery composite diaphragm comprises the following steps:
(1) mixing PVDF powder, PMMA powder, a coupling agent, an auxiliary agent and water to prepare PMMA/PVDF mixed slurry;
(2) sending the battery diaphragm into a coating device, and coating by using the PMMA/PVDF mixed slurry prepared in the step (1);
(3) and (3) drying and rolling the battery diaphragm coated in the step (2) to obtain a finished product of the surface modified PMMA/PVDF mixed coated lithium battery composite diaphragm.
2. The surface modified PMMA/PVDF hybrid coated lithium battery composite separator as defined in claim 1, wherein: in the PMMA/PVDF mixed coating, the weight ratio of PMMA particles modified by the surface of the coupling agent to PVDF particles modified by the surface of the coupling agent is 1:9-9: 1.
3. The surface modified PMMA/PVDF hybrid coated lithium battery composite separator as defined in claim 1, wherein: the coupling agent is a silane coupling agent.
4. The surface modified PMMA/PVDF hybrid coated lithium battery composite separator as defined in claim 1, wherein: the thickness of the PMMA/PVDF mixed coating is 0.1-4 mu m.
5. The surface modified PMMA/PVDF hybrid coated lithium battery composite separator as defined in any one of claims 1 to 4, wherein: the battery diaphragm is a polyolefin-based diaphragm or a ceramic diaphragm coated with an inorganic ceramic particle coating on the polyolefin-based diaphragm.
6. The surface modified PMMA/PVDF hybrid coated lithium battery composite membrane of claim 5, wherein: the polyolefin base film is a polyethylene film, a polypropylene film or a polypropylene/polyethylene/polypropylene composite film with the thickness of 5-40 mu m and the porosity of 30-80%.
7. The surface modified PMMA/PVDF hybrid coated lithium battery composite membrane of claim 5, wherein: the inorganic ceramic particles are one or more of aluminum oxide, silicon dioxide, titanium dioxide, zirconium dioxide, magnesium oxide, zinc oxide and barium oxide, and the average particle size of the inorganic ceramic particles is 0.1-1 um; the thickness of the inorganic ceramic particle coating is 1-4 mu m.
8. The surface modified PMMA/PVDF hybrid coated lithium battery composite separator as defined in claim 1, wherein: in the step (1), the mixed slurry contains 1-9 parts by weight of PVDF powder, 1-9 parts by weight of PMMA powder and 0.5-3 parts by weight of coupling agent.
9. The surface modified PMMA/PVDF hybrid coated lithium battery composite separator as defined in claim 1, wherein: in the step (2), the coating mode is one of dip coating, spray coating, a scraper, a coating wire rod and micro-concave roller coating.
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| CN111129393A (en) * | 2019-11-18 | 2020-05-08 | 高芳 | Mixed coating lithium battery diaphragm and preparation method thereof |
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| CN115207566A (en) * | 2022-08-24 | 2022-10-18 | 宁德卓高新材料科技有限公司 | PMMA/PVDF composite diaphragm and preparation method and application thereof |
| CN116111286B (en) * | 2023-04-04 | 2023-08-18 | 宁德卓高新材料科技有限公司 | Modified PVDF (polyvinylidene fluoride) coated diaphragm and preparation method and application thereof |
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