CN105762319A - Composite lithium ion battery diaphragm with high cohesion and preparation method thereof - Google Patents
Composite lithium ion battery diaphragm with high cohesion and preparation method thereof Download PDFInfo
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- CN105762319A CN105762319A CN201610119300.0A CN201610119300A CN105762319A CN 105762319 A CN105762319 A CN 105762319A CN 201610119300 A CN201610119300 A CN 201610119300A CN 105762319 A CN105762319 A CN 105762319A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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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- 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)
- Cell Separators (AREA)
Abstract
The invention provides a composite lithium ion battery diaphragm with high cohesion and a preparation method thereof. The composite diaphragm comprises a polyolefin porous basic film, wherein the surface of polyolefin porous basic film is coated with an inorganic binding coating, and the inorganic binding coating is formed by combining the binder and inorganic particles by virtue of hydrogen bonds. According to the prepared composite diaphragm, the cohesion between a basic material and the inorganic particles is increased, so that the dropping of the inorganic particles is reduced; and the product quality is improved, and the risk of influencing the safety performance of the battery due to the dropping of the inorganic particles in the production process is reduced.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to lithium ion battery composite separation membrane of a kind of high cohesion and preparation method thereof.
Background technology
Lithium ion battery obtains general application with the high-energy-density performance advantage of its uniqueness in mobile communication, consumption electronic product (mobile phone, notebook computer etc.), and the high capacity lithium ion battery of current various countries research worker exploitation is as the electrical source of power popularization and application of electric automobile.
The structure of lithium ion battery includes the structural members such as positive pole, negative pole, barrier film, electrolyte and battery core, its septation is one of inside lithium ion cell critical component, it has the characteristic of electronic isolation ion conducting, negative electrode and the anode of lithium ion battery can be isolated, thus preventing the two poles of the earth in battery core from directly contacting and producing short circuit.The material of current barrier film is mainly polyolefin porous polymeric membrane, and this base polymer easily shrinks in high temperature environments, can cause battery positive and negative electrode bump contact and produce amount of heat rapidly and cause thermal runaway, so that burning or blast occur battery.
Through research and development for many years, inorganic ceramic coating barrier film is used widely in electrokinetic cell field with the high temperature resistant of its excellence and safety.Inorganic ceramic coating barrier film is at existing polyolefin porous separator mother metal one side or one layer of inorganic ceramic coating granule of dual coating.Yet with inorganic ceramic powder body material used, there is water-wetted surface, and the barrier film base material such as polyolefin porous separator mother metal such as polyethylene (PE), polypropylene (PP) is nonpolar hydrophobic surface, therefore surface compatability therebetween can be poor, it is easy to cause that ceramic powder coating procedure floating coat cohesive force is strong, surface checking and aging, porosity change etc. affect the situation generation of product quality.And coating cohesive force is not easily caused by force later stage barrier film dry linting in winding process, the ceramic particle come off from membrane surface is mixed in the middle of barrier film and pole piece, causes that battery core is breakdown in hot pressing test process septation, causes that producing yield rate reduces；Even if hot pressing test is passed through, it is mixed in the barrier film ceramic particle middle with pole piece and the internal micro-short circuit of barrier film, follow-up battery core self discharge probability can be caused high, even the security performance of battery such as internal short-circuit etc. is caused significant impact.
A kind of preparation method improving ceramic coating cohesiveness and a kind of ceramic-coated separator with diaphragm interface cohesive force has been it is an object of the invention to provide hence for the problems referred to above, the method can effectively solve the problems such as polyalkene diaphragm surface ceramic coat dry linting, stripping, is conducive to the security performance of Improving The Quality of Products and battery.
Summary of the invention
It is an object of the invention to provide lithium ion battery composite separation membrane of a kind of high cohesion and preparation method thereof, ceramic coating cohesiveness and the cohesive force with diaphragm interface thereof can have been improved, thus the security performance of Improving The Quality of Products and battery.
Technical scheme is as follows:
A kind of lithium ion battery composite separation membrane of high cohesion, described composite diaphragm includes polyolefin porous basement membrane, the surface-coated of described polyolefin porous basement membrane has inorganic bonding coat, and described inorganic bond coating is to be formed by hydrogen bonded by between binding agent and inorganic particle.
Further scheme, described binding agent is the water-based binder containing-CO-or-CN functional group；Described inorganic particle refers to the inorganic compound particle containing-OH functional group.
Further scheme, described water-based binder one or more monomer polymerizations in esters of acrylic acid, alkenyl carboxylate's class, thiazolinyl nitrile form.
Wherein esters of acrylic acid binding agent refers to structural formula monomer as shown in Equation 1:
Formula 1
In formula 1, R1Alkyl for H or carbon number 1-3；R2Alkyl for carbon number 1-4；R3Alkyl for H or carbon number 1-3.
Alkenyl carboxylate's class binding agent refers to structural formula monomer as shown in Equation 2:
R4-CH2COOR5Formula 2
In formula 2, R4H or the alkyl of carbon number 1-3, R can be independently be5The thiazolinyl of carbon number 2-4 can be independently be.
Thiazolinyl nitrile binding agent refers to structural formula monomer as shown in Equation 3:
R6-CN formula 3
In formula 3, R6The thiazolinyl of carbon number 2-5 can be independently be.
Alkyl concretely methyl, ethyl, propyl group, isopropyl, butyl in above-mentioned formula 1-3；Thiazolinyl concretely vinyl, acrylic, pi-allyl, isopropenyl, cyclobutenyl, pentenyl.
Specifically, aforesaid propylene esters of gallic acid is preferably acrylic acid methyl ester., ethyl acrylate, methyl methacrylate, ethyl methacrylate.
Specifically, above-mentioned alkenyl carboxylate's class is preferably vinylacetate.
Specifically, above-mentioned thiazolinyl nitrile is preferably acrylonitrile.
Further scheme, described inorganic compound particle at least one in boehmite, aluminium hydroxide, magnesium hydroxide particle.
Further scheme, particle diameter D50 < 2 μm of described inorganic particle, D100 < 10 μm.
Further scheme, the gross thickness of described composite diaphragm is 6-30 μm, and the thickness of described inorganic bond coating is 2-6 μm.
Further scheme, described inorganic bond coating is formed at the single or double of described polyolefin porous basement membrane.
The preparation method that another goal of the invention of the present invention is to provide above-mentioned lithium ion battery composite separation membrane, it specifically comprises the following steps that
(1) being added in planetary agitator tank by deionized water, then added in agitator tank by inorganic particle powder, controlling its solid content is 55%-65%；
(2) blender is opened after temperature is be stirred 50-60min in 25-35 DEG C of situation, under agitation binding agent is dividedly in some parts in blender, the molal quantity making-OH in the-CO-in the binding agent of addition or-CN and inorganic particle is suitable, continues stirring 180-200min and obtains mixed slurry；
(3) mixed slurry is proceeded in dispersed ultrafine machine and carry out disperseing to obtain inorganic bond coating paste；
(4) inorganic bond coating paste is coated uniformly on the single or double of polyolefin porous basement membrane, then drying, rolling, obtain lithium ion battery composite separation membrane.
Further scheme, at least scrapes agitator tank inwall once in described step (2) in the process of stirring.
The present invention adopts the inorganic material powders granule that crystal structure contains covalent bond hydroxyl-OH functional group to prepare into inorganic particulate coatings with the water-based binder containing-CO-or-CN functional group.Covalent bond-OH contained by crystal structure and-CO-contained by binding agent or-CN forms Hydrogen bonding forces, shown in its hydrogen bond action principle formula 4,5 specific as follows:
Formula 4
M-OH+R6-CN→M-OH···NC-R6Formula 5
So while there is stronger Hydrogen bonding forces with binding agent in inorganic particle so that composite diaphragm cohesive force prepared by the present invention is better than the oxide ceramic coating barrier film selecting the type such as aluminium oxide, silicon dioxide of existing pertinent literature report.
Therefore the composite diaphragm of the present invention is compared with existing lithium ion battery composite separation membrane, the method have the advantages that
1, the composite diaphragm that prepared by the present invention selects binding agent and the inorganic particle with ad hoc structure, improve the mode that intercouples between binding agent and inorganic particle, it is be combined with each other raising coating cohesive force by hydrogen bond, reduce that coating inorganic particles process floating coat cohesive force in actual production process is strong, surface checking and the problem that occurs inorganic particle to come off.
2, adopt inorganic particle in the battery energy Improving The Quality of Products of the lithium ion battery composite separation membrane of the present invention, reduction production process to come off and affect the risk of battery safety.
3, adopt the composite diaphragm prepared of the method to be remarkably reinforced because of its interfacial adhesion, solve composite diaphragm manufacture and battery core makes in winding process the phenomenons such as inorganic particle dry linting.
4, the inorganic particulate material that the composite diaphragm of the present invention is chosen containing particular functional group mates with the functional group of corresponding binding agent, the cohesive force between inorganic particle is improved, thus reducing granule dry linting and spallation problems that inorganic particle causes because cohesive force is not strong by the interaction force hydrogen bonded of functional group.
Detailed description of the invention
Illustrate the composite diaphragm of the present invention, its preparation method below in conjunction with embodiment and use the process data of lithium ion battery that it manufactures.
Embodiment 1:
(1) deionized water is added in planetary agitator tank, then by particle diameter D50 be 1 μm, D100 be that the aluminium-hydroxide powder of 8 μm adds in agitator tank, controlling its solid content is 60%；
(2) blender is opened after temperature is be stirred 60min in 25 DEG C of situations, under agitation binding agent methyl methacrylate is dividedly in some parts in blender, the mol ratio making the-CO-and-OH in inorganic particle in the binding agent of addition is 1:1, and scrape agitator tank inwall once, continue stirring 180min and obtain mixed slurry；
(3) mixed slurry is proceeded in dispersed ultrafine machine and carry out disperseing to obtain inorganic bond coating paste；
(4) inorganic bond coating paste is coated uniformly on the one side of polypropylene porous basement membrane, and coating layer thickness is 3 μm, then drying, rolling, obtain the lithium ion battery composite separation membrane that thickness is 15 μm.
Embodiment 2:
(1) deionized water is added in planetary agitator tank, then by particle diameter to be D50 be 1.6 μm, D100 be that the boehmite powder of 9 μm adds in agitator tank, controlling its solid content is 55%；
(2) blender is opened after temperature is be stirred 50min in 35 DEG C of situations, under agitation binding agent vinylacetate is dividedly in some parts in blender, making-the CO-in the binding agent of addition is 1:1 with the-OH mol ratio in inorganic particle, and scrape agitator tank inwall once, continue stirring 200min and obtain mixed slurry；
(3) mixed slurry is proceeded in dispersed ultrafine machine and carry out disperseing to obtain inorganic bond coating paste；
(4) inorganic bond coating paste is coated uniformly on one side 2 μ m-thick of polyethylene porous basement membrane, then drying, rolling, obtain the lithium ion battery composite separation membrane that thickness is 6 μm.
Embodiment 3:
(1) deionized water is added in planetary agitator tank, then by particle diameter D50 be 1.4 μm, D100 be that the magnesium hydroxide powder of 10 μm adds in agitator tank, controlling its solid content is 65%；
(2) blender is opened after temperature is be stirred 55min in 30 DEG C of situations, under agitation binding agent acrylonitrile is dividedly in some parts in blender, making-the CN in the binding agent of addition is 1:1 with the-OH mol ratio in inorganic particle, and scrape agitator tank inwall once, continue stirring 190min and obtain mixed slurry；
(3) mixed slurry is proceeded in dispersed ultrafine machine and carry out disperseing to obtain inorganic bond coating paste；
(4) inorganic bond coating paste is coated uniformly on the two-sided of polyethylene porous basement membrane, its thick 4 μm, then drying, rolling, obtain the lithium ion battery composite separation membrane that thickness is 20 μm.
Comparative example 1:
Polyvinyl acetate selected by binding agent, and ceramic particle selects traditional aluminium oxide Al without covalent bond-OH2O3, to prepare inorganic bond coating paste according to the preparation method of embodiment 1, and be coated uniformly on PE barrier film one side, its coating thickness is 3 μm, eventually passes baking, rolling obtains ceramic coating diaphragm for lithium ion battery.
Comparative example 2:
Selection inorganic particle is boehmite particles, the polymer P VDF that binding agent is without-CO-or-CN makes binding agent, inorganic bond coating paste is prepared according to the preparation method of embodiment 1, and it is coated uniformly on PE barrier film one side, its coating thickness is 3 μm, eventually passes baking, rolling obtains boehmite particles coating diaphragm for lithium ion battery.
Test case 1,
The coating cohesiveness size of test compound barrier film
The coating cohesiveness size of the composite diaphragm of embodiment 1-3 and comparative example 1,2 preparation is detected respectively by cohesiveness method of testing, its method of testing is: adopt the green gluing surface being attached to composite diaphragm at normal temperatures, then the pressure roller adopting 50N rolls 3 times, adopting high ferro strain gauge to carry out 180 ° with the speed of 5mm/min and peel off test, its test result is as shown in table 1:
Table 1 cohesiveness test result
From the cohesive force test result of table 1 it can be seen that adopt its coating cohesiveness of composite diaphragm prepared by the inventive method to be significantly greater than the cohesive force of comparative example 1,2, and the raising of its coating cohesiveness of composite diaphragm can effectively reduce inorganic particle and the impact of dry linting, stripping occurs in subsequent handling process.
Test case 2: contrast battery core assembling hot pressing short circuit ratio
Cathode and anode pole piece and the composite diaphragm by embodiment 1-3 and comparative example 1,2 preparation is adopted to form battery core assembly with the form of winding, battery core assembly with the power of 1000kgf, the temperature hot pressing of 80 DEG C above battery core, adopt 200V voltage, internal resistance 20M Ω Hi-pot tester test battery core internal short-circuit situation, as shown in table 2 below:
Wherein electrodes of lithium-ion batteries prepare as follows:
Adopt LiFePO4 (LFP) as active material of cathode, it is that 90%LFP active material adds in N-methyl-pyrrolidon (NMP) solvent by ratio, add 5% acetylene black and make conductive agent and 5% Kynoar (PVDF) makes binding agent, agitated, dispersion after formed cathode slurry, above-mentioned cathode slurry is coated uniformly in 20 μm of aluminum foil current collector, drying, cold pressing after formed cathode sheet.
Adopt graphite (C) as active material of positive electrode, the active material that ratio is 92% is added in deionized water solvent, add 3% white carbon black and make conductive agent and 1.5% hydroxymethyl cellulose (CMC) and 3.5% butadiene-styrene rubber (SBR) makes binding agent, agitated, dispersion after formed anode slurry, above-mentioned anode slurry is coated uniformly in 8 μm of copper foil current collector, drying, cold pressing after formed anode pole piece.
Table 2: the battery core short circuit result of composite diaphragm
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Short circuit ratio | 0.15% | 0.11% | 0.05% | 0.25% | 0.23% |
From upper table 2 test result it can be seen that the barrier film prepared far below comparative example 1,2 of composite diaphragm short circuit ratio prepared by the present invention.This is owing to the present invention adopts the inorganic ceramic granule containing covalent bond-OH to carry out hydrogen bonded with the binding agent containing-CO-or-CN so that the cohesiveness of ceramic coating is bigger；And the aluminium oxide without covalent bond-OH is less with the coating cohesiveness that the PVDF binding agent without-CO-or-CN is formed with the binding agent containing-CO-or-CN and the boehmite ceramic particle containing covalent bond-OH, cutting, in winding process, ceramic particle is easy to fall off is mixed in the middle of pole piece and barrier film and causes that barrier film is pierced through by barrier film ceramic particle under high pressure effect for composite diaphragm, thus breakdown under high voltages, disassemble the stain existence that can be seen that in battery core that membrane surface leaves ceramic particle.
In sum, the coating interface cohesive force of the composite diaphragm that prepared by the present invention, battery core short circuit ratio performance are all superior to the ceramic-coated separator that comparative example 1,2 is common.
Above example, only for illustrating the design of the present invention, is not intended to limit the present invention.Certainly; the present invention also can have other various embodiments; when without departing substantially from present invention spirit and essence thereof; those of ordinary skill in the art are when can make various corresponding change and deformation according to the present invention, but these change accordingly and deformation all should belong to the scope of the claims appended by the present invention.
Claims (9)
1. the lithium ion battery composite separation membrane of a high cohesion, described composite diaphragm includes polyolefin porous basement membrane, it is characterized in that: the surface-coated of described polyolefin porous basement membrane has inorganic bonding coat, and described inorganic bond coating is to be formed by hydrogen bonded by between binding agent and inorganic particle.
2. lithium ion battery composite separation membrane according to claim 1, it is characterised in that: described binding agent is the water-based binder containing-CO-or-CN functional group；Described inorganic particle refers to the inorganic compound particle containing-OH functional group.
3. lithium ion battery composite separation membrane according to claim 2, it is characterised in that: described water-based binder one or more monomer polymerizations in esters of acrylic acid, alkenyl carboxylate's class, thiazolinyl nitrile form.
4. lithium ion battery composite separation membrane according to claim 2, it is characterised in that: described inorganic compound particle at least one in boehmite, aluminium hydroxide, magnesium hydroxide particle.
5. lithium ion battery composite separation membrane according to claim 1, it is characterised in that: particle diameter D50 < 2 μm of described inorganic particle, D100 < 10 μm.
6. lithium ion battery composite separation membrane according to claim 1, it is characterised in that: the gross thickness of described composite diaphragm is 6-30 μm, and the thickness of described inorganic bond coating is 2-6 μm.
7. lithium ion battery composite separation membrane according to claim 1, it is characterised in that: described inorganic bond coating is formed at the single or double of described polyolefin porous basement membrane.
8. the preparation method of a lithium ion battery composite separation membrane as claimed in claim 1, it is characterised in that: step is as follows:
(1) being added in planetary agitator tank by deionized water, then added in agitator tank by inorganic particle powder, controlling its solid content is 55%-65%；
(2) blender is opened after temperature is be stirred 50-60min in 25-35 DEG C of situation, under agitation binding agent is dividedly in some parts in blender, make-OH the molal quantity in the-CO-in the binding agent of addition or-CN and inorganic particle suitable, continue stirring 180-200min and obtain mixed slurry；
(3) mixed slurry is proceeded in dispersed ultrafine machine and carry out disperseing to obtain inorganic bond coating paste；
(4) inorganic bond coating paste is coated uniformly on the single or double of polyolefin porous basement membrane, then drying, rolling, obtain lithium ion battery composite separation membrane.
9. preparation method according to claim 8, it is characterised in that: described step (2) at least scrapes agitator tank inwall once in the process of stirring.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106654124A (en) * | 2017-01-20 | 2017-05-10 | 东莞市卓高电子科技有限公司 | Method for preparing heat-resistant lithium battery separator |
| CN106684293A (en) * | 2016-08-29 | 2017-05-17 | 东莞市卓高电子科技有限公司 | Production process of lithium battery separator |
| CN107871620A (en) * | 2016-09-27 | 2018-04-03 | 宁德新能源科技有限公司 | Barrier film and energy storage device |
| 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 |
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