CN110048057A - Surface modified PMMA/PVDF mixing coating composite diaphragm for lithium battery and preparation method thereof - Google Patents
Surface modified PMMA/PVDF mixing coating composite diaphragm for lithium battery and preparation method thereof Download PDFInfo
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- CN110048057A CN110048057A CN201910228370.3A CN201910228370A CN110048057A CN 110048057 A CN110048057 A CN 110048057A CN 201910228370 A CN201910228370 A CN 201910228370A CN 110048057 A CN110048057 A CN 110048057A
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- pvdf
- pmma
- coating
- diaphragm
- lithium battery
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Classifications
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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
-
- 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
-
- 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 kind of surface modified PMMA/PVDF mixing coating composite diaphragm for lithium batteries and preparation method thereof；The composite diaphragm for lithium battery includes battery diaphragm and the PMMA/PVDF mixed coating coated on battery diaphragm unilateral or bilateral, and the PMMA/PVDF mixed coating includes the modified PMMA particle in coupling agent surface and the PVDF particle that coupling agent surface is modified.The present invention is modified the surface PMMA and PVDF using coupling agent, solve the problems, such as that PMMA mixes uneven, easy sedimentation with PVDF, so that the film surface of coating is smooth, yields is high, and effectively improve the mechanical property and cementability of diaphragm, electrolyte absorption is increased, ionic conductivity is improved.
Description
Technical field
The invention belongs to lithium battery diaphragm Material Fields, and in particular to a kind of surface modified PMMA/PVDF mixing coating
Composite diaphragm for lithium battery and preparation method thereof.
Background technique
Lithium battery has many advantages, such as high-energy density, has extended cycle life as novel secondary cell, and application range is not
Disconnected extension, is widely used in portable electronic device, electric tool, energy storage and power vehicle, especially as new energy row
The fast development of industry, lithium battery are more and more applied in power vehicle.However, the lithium battery safety accident frequently occurred
Increasingly cause the extensive concern of people.Wherein, important component of the diaphragm as lithium battery can be effectively prevented positive and negative
Short circuit occurs for pole contact, has very important influence, therefore, the promotion and safety of lithium battery performance to the safety of lithium battery
Property require have higher requirement to the performance of diaphragm.
Polyalkene diaphragm is current the most widely used lithium battery diaphragm, still, existing polyalkene diaphragm in the market
There is a problem of adhesive property and close electrolyte property deficiency.In order to improve cementability and the electrolyte infiltration of polyalkene diaphragm
Property, current main solution is the single or double coating PVDF coating in polyalkene diaphragm, and this coating is in certain journey
The cementability of diaphragm can be improved on degree, while having good wellability with electrolyte.With the development of lithium battery, to its diaphragm
Cementability require it is higher and higher, simple PVDF coating cannot reach corresponding requirements, therefore it is excellent to seek next-generation adhesive property
High-end diaphragm just at the task of top priority.
Polymethyl methacrylate (PMMA), also known as acryl, acrylic or organic glass have high intensity, excellent
Stretch-proof and shock proof ability.And PMMA is mixed with PVDF, can both influence the crystallinity of PVDF, increase electrolyte absorb and
Ionic conductivity is improved, and the mechanical property and cementability of diaphragm can be improved.
But simple PMMA mixes coating with PVDF that the effect is unsatisfactory, wherein most important problem is, PMMA with
Effect is poor in PVDF mixed process, is easy sedimentation, and mix unevenly, film surface out-of-flatness, non-defective unit are caused in coating procedure
Rate is low.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of surface modified PMMA/PVDF mixing coating lithium battery is multiple
Close diaphragm and preparation method thereof, both can effectively solve PVDF adhesive property deficiency and crystallinity influence ionic conductivity and
PMMA electrolyte infiltrates the problems such as consistency is poor, and can solve the problem of PMMA mixes uneven, easy sedimentation with PVDF.
In order to achieve the above objectives, the invention provides the following technical scheme:
A kind of surface modified PMMA/PVDF mixing coating composite diaphragm for lithium battery, including battery diaphragm and it is coated on electricity
The PMMA/PVDF mixed coating of pond diaphragm unilateral or bilateral, the PMMA/PVDF mixed coating include that coupling agent surface is modified
The PVDF particle that PMMA particle and coupling agent surface are modified.
In the PMMA/PVDF mixed coating, what the modified PMMA particle in coupling agent surface was modified with coupling agent surface
Weight proportion between PVDF particle can be adjusted according to the demand of diaphragm applicable cases, and preferred weight ratio is 1:9-9:1.
The coupling agent can be various conventional coupling agents, and the coupling agent selects silane as a preferred technical solution,
Coupling agent, such as KH-550, KH-570, KH-580 etc..
The PMMA/PVDF mixed coating is preferably with a thickness of 0.1-4 μm.
The battery diaphragm is polyolefin base membrane or the ceramics that inorganic ceramic grain coating is coated in polyolefin base membrane
Diaphragm；That is, PMMA/PVDF mixed coating can be applied directly in polyolefin base membrane, it can also be coated in and include inorganic pottery
On the ceramic diaphragm of porcelain grain coating.
The polyolefin base membrane can be various conventional polyolefin basement membranes, as a preferred technical solution, the polyolefin
Basement membrane is 5-40 μm of thickness, the polyethylene film of porosity 30-80%, polypropylene screen or polypropylene, polyethylene/polypropylene composite materials
Film.
The inorganic ceramic particle can be various general inorganic ceramic particles, as a preferred technical solution, the nothing
Machine ceramic particle be one of aluminium oxide, silica, titanium dioxide, zirconium dioxide, magnesia, zinc oxide and barium monoxide or
Several, the average grain diameter of the inorganic ceramic particle is 0.1-1um；The thickness of the inorganic ceramic grain coating is preferably 1-4 μ
m。
The preparation method of above-mentioned surface modified PMMA/PVDF mixing coating composite diaphragm for lithium battery, comprising the following steps:
(1) PVDF powder, PMMA powder and coupling agent, auxiliary agent and water are hybridly prepared into PMMA, PVDF slurry respectively, so
Silane coupler modified PMMA, PVDF slurry is mixedly configured into PMMA/PVDF coating slurry by a certain percentage afterwards；
(2) battery diaphragm is sent into coating unit, is coated using the PMMA/PVDF mixed slurry that step (1) is prepared；
(3) the dry, winding by the battery diaphragm after step (2) coat obtains surface modified PMMA/PVDF mixing and applies
The composite diaphragm for lithium battery finished product covered.
In the step (1), preferred process conditions are to include PVDF powder, the 1-9 of 1-9 parts by weight in mixed slurry
The coupling agent of the PMMA powders of parts by weight, 0.5-3 parts by weight.
In the step (1), auxiliary agent can select common auxiliary agent in painting slurry preparation, such as: dispersing agent, bonding
Agent, wetting agent etc..
In the step (2), coating method is various conventional coating methods, such as: dip-coating, spraying, scraper, coating line
Stick, dimple roller coating apply.
The beneficial effects of the present invention are:
1, the present invention is modified the surface PMMA and PVDF using coupling agent, and coupling agent is grafted to PMMA and PVDF table
Face solves PMMA and mixes uneven, easy sedimentation ask with PVDF so as to improve the specific surface energy between PMMA and PVDF
Topic, so that the film surface of coating is smooth, yields is high.
2, PMMA/PVDF mixed coating of the invention had not only effectively improved the mechanical property and cementability of diaphragm, but also had increased
Electrolyte absorption, improves ionic conductivity.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is the surface scan electromicroscopic photograph of the diaphragm of embodiment 1；
Fig. 2 is the surface scan electromicroscopic photograph of the diaphragm of comparative example 4；
Fig. 3 is the modified schematic diagram in the surface PMMA, PVDF.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It better understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1:
(1) it prepares PMMA/PVDF mixed slurry: first 1.55 parts of dispersing agents and 0.44 part of wetting agent being added in deionized water
It is completely dissolved, after then 4.42 parts of PVDF powders of addition are sufficiently stirred, grinds 1h；4.42 parts of PMMA powders are added again ground
PVDF slurry in be sufficiently stirred, and 1.5 parts of silane coupling agents are added and are sufficiently stirred as surface modifier, then grind 0.5h,
It is eventually adding 0.88 part of bonding agent；
(2) battery diaphragm selects the ceramic diaphragm of+2 μm of inorganic ceramic grain coatings of 7 μm of polyethylene based films, by battery diaphragm
It is sent into coating unit, is coated using the PMMA/PVDF mixed slurry that step (1) is prepared, in such a way that dimple roller coating applies
Unilateral side coated on battery diaphragm；
(3) the dry, winding by the battery diaphragm after step (2) coat obtains surface modified PMMA/PVDF mixing and applies
The composite diaphragm for lithium battery finished product covered.
Embodiment 2:
The present embodiment difference from example 1 is that: prepare PMMA/PVDF mixed slurry when, PMMA powder is
5.30 parts, PVDF powder is 3.54 parts, and silane coupling agent is 1.8 parts.
Embodiment 3:
The present embodiment difference from example 1 is that: prepare PMMA/PVDF mixed slurry when, PMMA powder is
7.07 parts, PVDF powder is 1.77 parts, and silane coupling agent is 1 part.
Embodiment 4:
The present embodiment difference from example 1 is that: prepare PMMA/PVDF mixed slurry when, PMMA powder is
1.25 parts, PVDF powder is 7.59 parts, and silane coupling agent is 2.5 parts.
Comparative example 1:
Comparative example 1 difference from example 1 is that: prepare PMMA slurry, PMMA powder be 8.84 parts.Using PMMA
Slurry is coated.
Comparative example 2:
Comparative example 2 difference from example 1 is that: prepare PVDF slurry, PVDF powder be 8.84 parts.Using PVDF
Slurry is coated.
Comparative example 3:
Comparative example 3 is the ceramic diaphragm of+2 μm of inorganic ceramic grain coatings of 7 μm of polyethylene based films.
Comparative example 4:
Comparative example 4 difference from example 1 is that: prepare PMMA/PVDF mixed slurry when, do not add silane idol
Join agent.
The obtained diaphragm of embodiment 1-4 and comparative example 1-3 is tested for the property at identical conditions, as a result such as table 1
It is shown.
1 lithium battery diaphragm the performance test results comparative situation of table
From the point of view of adhesive property by table 1, the pure PMMA coating diaphragm of comparative example 1 has excellent adhesion energy, comparative example 2
Pure PVDF coating diaphragm adhesive property it is insufficient, and the adhesive property of the PMMA/PVDF of embodiment 1-4 mixing coating diaphragm is more
Add excellent.
From the point of view of ionic conductivity by table 1, the PMMA/PVDF mixing coating diaphragm of embodiment 1-4 significantly increases electrolysis
Liquid absorbs and ionic conductivity, from experimental data verifying as can be seen that the ionic conductivity ratio of PMMA/PVDF mixing coating diaphragm
The ceramic diaphragm of comparative example 3 and the pure PVDF of comparative example 2 coat the high an order of magnitude of diaphragm.
The surface scan electromicroscopic photograph of the diaphragm of embodiment 1 as shown in Figure 1, the diaphragm of comparative example 4 surface scan Electronic Speculum
Although photo as shown in Fig. 2, it can be seen from the figure that be all PMMA/PVDF mixing coating diaphragm, comparative example 4 is simple
PMMA mixes coating with PVDF, and the effect is unsatisfactory, PMMA and PVDF poor dispersion, and agglomeration leads to film surface than more serious
Out-of-flatness, yields are low；And embodiment 1 is modified the surface PMMA and PVDF using coupling agent, coupling agent is grafted to PMMA
With the surface PVDF (as shown in Figure 3), the specific surface energy between PMMA and PVDF, PMMA and PVDF good dispersion are improved, is not had
Agglomeration, film surface is smooth, and yields is high.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (10)
1. a kind of surface modified PMMA/composite diaphragm for lithium battery of PVDF mixing coating, including battery diaphragm and it is coated on battery
The PMMA/PVDF mixed coating of diaphragm unilateral or bilateral, it is characterised in that: the PMMA/PVDF mixed coating includes coupling agent
The PVDF particle that the modified PMMA particle in surface and coupling agent surface are modified.
2. surface modified PMMA according to claim 1/PVDF mixing coating composite diaphragm for lithium battery, feature exist
In: in the PMMA/PVDF mixed coating, the modified PMMA particle in the coupling agent surface PVDF particle modified with coupling agent surface
Between weight ratio be 1:9-9:1.
3. surface modified PMMA according to claim 1/PVDF mixing coating composite diaphragm for lithium battery, feature exist
In: the coupling agent is silane coupling agent.
4. surface modified PMMA according to claim 1/PVDF mixing coating composite diaphragm for lithium battery, feature exist
In: the PMMA/PVDF mixed coating with a thickness of 0.1-4 μm.
5. surface modified PMMA according to any one of claims 1 to 4/lithium battery of PVDF mixing coating it is compound every
Film, it is characterised in that: the battery diaphragm is polyolefin base membrane or inorganic ceramic grain coating is coated in polyolefin base membrane
Ceramic diaphragm.
6. surface modified PMMA according to claim 5/PVDF mixing coating composite diaphragm for lithium battery, feature exist
In: the polyolefin base membrane is 5-40 μm of thickness, the polyethylene film of porosity 30-80%, polypropylene screen or polypropylene/poly- second
Alkene/polypropylene composite film.
7. surface modified PMMA according to claim 5/PVDF mixing coating composite diaphragm for lithium battery, feature exist
In: the inorganic ceramic particle is aluminium oxide, silica, titanium dioxide, zirconium dioxide, magnesia, zinc oxide and barium monoxide
One or more of, the average grain diameter of the inorganic ceramic particle is 0.1-1um；The thickness of the inorganic ceramic grain coating
It is 1-4 μm.
8. the system of the modified PMMA of surface described in claim 1 to 7 any one/PVDF mixing coating composite diaphragm for lithium battery
Preparation Method, it is characterised in that: the following steps are included:
(1) PVDF powder, PMMA powder, coupling agent, auxiliary agent and water are hybridly prepared into PMMA/PVDF mixed slurry；
(2) battery diaphragm is sent into coating unit, is coated using the PMMA/PVDF mixed slurry that step (1) is prepared；
(3) the dry, winding by the battery diaphragm after step (2) coat obtains surface modified PMMA/PVDF mixing coating
Composite diaphragm for lithium battery finished product.
9. the preparation method of surface modified PMMA according to claim 8/PVDF mixing coating composite diaphragm for lithium battery,
It is characterized by: in the step (1), the PMMA powder of PVDF powder, 1-9 parts by weight in mixed slurry comprising 1-9 parts by weight
The coupling agent of body, 0.5-3 parts by weight.
10. the preparation side of surface modified PMMA according to claim 8/PVDF mixing coating composite diaphragm for lithium battery
Method, it is characterised in that: in the step (2), coating method is during dip-coating, spraying, scraper, coating bar and dimple roller coating apply
It is a kind of.
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| CN201910228370.3A CN110048057B (en) | 2019-03-25 | 2019-03-25 | Surface-modified PMMA/PVDF hybrid-coated lithium battery composite diaphragm and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110718659A (en) * | 2019-10-21 | 2020-01-21 | 重庆云天化纽米科技股份有限公司 | Boron nitride coated battery separator and method of making same |
| CN111129393A (en) * | 2019-11-18 | 2020-05-08 | 高芳 | Mixed coating lithium battery diaphragm and preparation method thereof |
| CN111211277A (en) * | 2020-02-19 | 2020-05-29 | 重庆云天化纽米科技股份有限公司 | Preparation method of PMMA gel coating diaphragm |
| CN111969160A (en) * | 2020-08-31 | 2020-11-20 | 佛山市金辉高科光电材料股份有限公司 | Composite lithium ion battery diaphragm and preparation method thereof, lithium ion battery and electronic product |
| CN113809477A (en) * | 2020-05-31 | 2021-12-17 | 重庆恩捷纽米科技股份有限公司 | Closed-pore characteristic battery diaphragm and preparation method and application thereof |
| CN114024088A (en) * | 2020-07-15 | 2022-02-08 | 重庆恩捷纽米科技股份有限公司 | Preparation method of PVDF (polyvinylidene fluoride) coating diaphragm |
| CN114221088A (en) * | 2021-11-30 | 2022-03-22 | 中材锂膜有限公司 | High-adhesion-strength PVDF (polyvinylidene fluoride) coated diaphragm and preparation method thereof |
| CN114335902A (en) * | 2021-12-23 | 2022-04-12 | 上海瑞浦青创新能源有限公司 | Composite diaphragm and preparation method and application thereof |
| 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 |
| CN116111286A (en) * | 2023-04-04 | 2023-05-12 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110718659A (en) * | 2019-10-21 | 2020-01-21 | 重庆云天化纽米科技股份有限公司 | Boron nitride coated battery separator and method of making same |
| CN111129393A (en) * | 2019-11-18 | 2020-05-08 | 高芳 | Mixed coating lithium battery diaphragm and preparation method thereof |
| CN111211277A (en) * | 2020-02-19 | 2020-05-29 | 重庆云天化纽米科技股份有限公司 | Preparation method of PMMA gel coating diaphragm |
| CN113809477A (en) * | 2020-05-31 | 2021-12-17 | 重庆恩捷纽米科技股份有限公司 | Closed-pore characteristic battery diaphragm and preparation method and application thereof |
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| CN114221088A (en) * | 2021-11-30 | 2022-03-22 | 中材锂膜有限公司 | High-adhesion-strength PVDF (polyvinylidene fluoride) coated diaphragm and preparation method thereof |
| CN114335902A (en) * | 2021-12-23 | 2022-04-12 | 上海瑞浦青创新能源有限公司 | Composite diaphragm and preparation method and application thereof |
| 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 |
| CN116111286A (en) * | 2023-04-04 | 2023-05-12 | 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 |
| 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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