CN104091910B - A kind of preparation method of ceramic modified lithium ion battery separator - Google Patents

A kind of preparation method of ceramic modified lithium ion battery separator Download PDF

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Publication number
CN104091910B
CN104091910B CN201410288028.XA CN201410288028A CN104091910B CN 104091910 B CN104091910 B CN 104091910B CN 201410288028 A CN201410288028 A CN 201410288028A CN 104091910 B CN104091910 B CN 104091910B
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ceramic
lithium ion
ion battery
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preparation
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CN104091910A (en
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王丹
赵中令
于力娜
张克金
张斌
崔龙
曹婷婷
魏传盟
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FAW Group Corp
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FAW Group Corp
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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
    • 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
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Cell Separators (AREA)

Abstract

The present invention relates to a kind of preparation method of ceramic modified lithium ion battery separator, it is characterized in that concrete preparation process is as follows: A) adopt slurry coated polymer porous septum; B) adopt active material to process ceramic particle; C) by B) pottery that obtains of step is distributed on the polyalcohol stephanoporate barrier film after A step slurry applies; D) by C) diaphragm hot-pressing that obtains of step obtains product. It has fundamentally solved ceramic composition in configuration liquid ceramics slurry process and has disperseed inhomogeneous problem, has avoided employing surfactant to promote that pottery is dispersed, cost-saving; Strong dimensional stability and the mechanical property that improves barrier film, can be applied to lithium ion battery, fuel cell, lead-acid battery, ultracapacitor etc. simultaneously.

Description

A kind of preparation method of ceramic modified lithium ion battery separator
Technical field
The preparation method who the present invention relates to a kind of ceramic modified lithium ion battery separator, particularly one can be used for powerThe preparation method of the barrier film of battery.
Background technology
Research shows, battery diaphragm plays a key effect to the security of electrokinetic cell, and on the one hand, it is exhausted that barrier film plays electronicsThe effect of edge, avoids battery generation internal short-circuit; On the other hand, barrier film, for ion transport provides passage, ensures electrochemical reactionCarry out smoothly.
Lithium ion battery separator mostly is organic polymer class barrier film at present, and the most significant shortcoming of this class barrier film is exactly to be subject to, can there is larger thermal deformation, thereby make be in contact with one another and internal short-circuit occurs by both positive and negative polarity in when heat, so cause thermal runaway orThe possibility of person's blast increases greatly. This has limited the large-scale application of lithium-ion-power cell on electric automobile, and then limitMake the development of electric motor car.
Therefore, people adopt inorganic ceramic to carry out ceramic modification to lithium ion battery separator more, thereby raising barrier filmThermal stability.
At present, most ceramic modified membrane process are all the coatings of liquid slurry, then drying obtains ceramic modified barrier film.Usually, as described below: (1) pretreatment barrier film, comprises the means such as corona, ultraviolet; (2) preparation ceramic size; (3) adopt necessarilySlurry is applied over pretreatment membrane surface afterwards by means; (4) post processings such as oven dry, setting, cutting, coiling. Wherein, locate in advanceThe effect of reason is to increase the surface energy of membrane surface, thereby improves the adhesion between ceramic composition and barrier film; Ceramic size is manyFor the suspension system that contains multiple component, comprise ceramic composition, surfactant, binding agent, solvent and other auxiliary agents etc.,Wherein the effect of surfactant is strengthen inorganic ceramic component dispersed; Coating is rear, baking desolventizing, then through formalizing, cuttingCut, reel and obtain ceramic modified barrier film.
Generally speaking, because granular ceramic composition particle diameter is less, very easily reunite, in liquid slurry, ceramic composition is equalEven dispersion is more difficult, and researcher adopts surfactant to promote dispersed in slurry of ceramic composition more,As patent application CN101281961A has adopted a large amount of molecules surfactants as PVP, polyethyleneAlcohol etc. promote the dispersion of ceramic composition, and patent application CN101789499A adopts a large amount of little molecule coupling agent cetylsSodium sulfonate, neopelex etc. promote the dispersion of ceramic composition.
No matter adopt which kind of surfactant, all mean the difficulty of dispersion steps and consuming time, and this dispersion liquid is notStable, the resting period is also shorter, and this has all limited the application of said method.
Summary of the invention
In order to overcome the above problems, the object of the present invention is to provide a kind of preparation of ceramic modified lithium ion battery separatorMethod, it directly adopts solid powder as ceramic composition, adopts gas medium to disperse ceramic composition, has effectively avoided particleReunite, obtained ceramic modified lithium ion battery separator.
Technical scheme of the present invention is achieved in that a kind of preparation method of ceramic modified lithium ion battery separator, itsBe characterised in that concrete steps are as follows:
A) adopt slurry coated polymer porous septum;
B) adopt active material to process ceramic particle;
C) by B) pottery that obtains of step is distributed on the polyalcohol stephanoporate barrier film after A step slurry applies;
D) by C) diaphragm hot-pressing that obtains of step obtains product.
Wherein steps A) described slurry, be hydrophily stickiness slurry, in its component, contain the group that can form hydrogen bond, toolBody ground, slurry is mainly by carboxymethyl cellulose (CMC), polyethylene glycol (PEO), Kynoar (PVDF), polyvinyl alcohol(PVA), polyacrylic acid (PA), polymethylacrylic acid (PMA), vinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP), poly-methylHydroxy-ethyl acrylate, polyacrylamide, one or more in Hydrin etc. are dissolved in water, acetone, ethanol, isobutylAlcohol, propane diols, 1-METHYLPYRROLIDONE, DMF, DMA, dimethyl sulfoxide (DMSO), dioxy sixRing, benzinum, carrene, chloroform, carbon tetrachloride, benzene, toluene, makes in one or more solvents in dimethylbenzene;Described barrier film is high-molecular porous film, and particularly, its composition of macromolecule includes but not limited to polyethylene, and polypropylene is poly-to benzene twoFormic acid glycol ester, polyimides, polyacrylonitrile, Kynoar, vinylidene fluoride-hexafluoropropylene copolymer, glass fibre, fibreOne or more in dimension element, thickness is 10 ~ 90 μ m, porosity is 30 ~ 60%; Described coating, preferentially adopts hot slurry to be coated withCover, coating method can make to flood-lift, and can be also to adopt scraper to apply, and can also adopt bird type spreader or line rodApply.
In order to ensure the strong interaction between this step slurry and basilar partition, can adopt certain means pretreatment everyFilm, as sided corona treatment, Low Temperature Plasma Treating etc., but, recommendation dopamine pretreatment herein.
Wherein step B) described pottery, include but not limited to aluminium oxide, silica, titanium dioxide, magnesia, oxidationZinc, zeolite, doubly one or more in octahedra siloxanes etc., for the uniformity that ensures to apply, particle diameter and distribution require D90For certain value between 50nm ~ 2000nm, i.e. certain between 50 ~ 2000nm of more than 90% particle size distributionValue; Described active material is generally that the silicon that amino, hydroxyl, sulfydryl or epoxy radicals, the other end contain alkoxyl is contained in one endAlkane coupling agent, particularly, is and contains and one or more of the silane coupler of structure (1) same structure:
Amino, hydroxyl, sulfydryl and the epoxy radicals containing can with binding agent in strong polar compound form strong hydrogenKey effect, or form chemical bond (hydroxyl in epoxy and binding agent or amino open loop); The Si-OR containing can and potteryComponent forms stable chemical bond, thereby, improve the adhesion between ceramic composition and barrier film.
In production, consider supply chain situation, can adopt as KH-540, KH-550, KH-560, KH792, KH970,One or more of DL602 etc., its molecular formula is as follows:
Step B) in processing, be generally in high-speed mixer, add ceramic particle and content is pottery simultaneouslyThe above-mentioned silane coupler of amount 0.5% ~ 5%, after high-speed mixing 0.5 ~ 24h, through hyperthermia drying, for subsequent use. Dry the temperature adopting hereinDegree, can adopt the heat resisting temperature higher than barrier film base material, and general ceramic modified barrier film is while drying, and temperature can not be higher than base materialHeat resisting temperature, adopt higher temperature to dry, can impel the fracture of Si-R key in silane coupler, promote coupling agent and potteryThe combination of porcelain particle, and then the adhesion of increase ceramic particle and barrier film.
Step C) described uniform, its mode is, at A) the stickiness membrane surface slurry that obtains of step still in the time of hygrometric state, willParticle is suspended in gas medium and is applied over its surface, and due to the stickiness of hygrometric state membrane surface, particle can effectively be adsorbed.
The suspension of particle in gas medium, can adopt fluid bed---rely on advertising of air-flow and make it to be suspended to skyIn gas medium, can also adopt sieve---when vibration, by under particle sieve, natural subsidence is to stickiness surface, and preferential employing sprayedRifle, drives particle precipitation to hygrometric state membrane surface with compressed air, and, can also control coated weight and coating thickness. HereinAdopt gas medium to disperse ceramic composition, can effectively avoid ceramic reunion, strengthen modification evenness.
Step D) described hot pressing, be hot pair roller type hot pressing, usually, roller temperature is 70 DEG C ~ 170 DEG C, roller spacing is 9 ~ 60 μM, it should be noted that before hot pressing, need to adopt certain means, as slit, and brush etc., to remove the unnecessary particle in surface,Thickness remains on certain scope, and (usually, higher than target thickness 5 ~ 10 μ m), this is conducive to make uniformly on the one handBarrier film, on the other hand, avoids the too much mutual squeeze and destroy barrier film of particle.
Good effect of the present invention adopts solid ceramic particle to replace liquid ceramics slurry, and adopts gas medium to dispersePottery honor, has effectively avoided liquid slurry to disperse inhomogeneous and unsettled shortcoming, is the ceramic modified lithium ion battery of preparationThe effective ways of barrier film. In addition, the method can adopt higher temperature to process ceramic particle, has avoided the high temperature place of barrier filmReason, is conducive to the stable of base material.
The method is rarely seen report also, can wash patent barrier open, and exploitation has the ceramic modified barrier film of independent intellectual property rightProduction technology and production line.
Brief description of the drawings
Fig. 1 is that the device that embodiment 1 adopts fluidized-bed process of the present invention to prepare ceramic modified lithium ion battery separator showsIntention.
Fig. 2 is that embodiment 2 adopts spray gun technique of the present invention to prepare the device signal of ceramic modified lithium ion battery separatorFigure.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention will be further described:
Embodiment 1
As shown in Figure 1, taking CMC as binding agent, water is solvent, and solution is heated to after 80 DEG C, adopts dipping-pulling method,Coated thickness and be the PE barrier film (PE barrier film adopts poly-dopamine processing in advance) of 10 μ m, obtain that stickiness slurry applies everyFilm 1; Meanwhile, adopt silane coupler KH560 to process the SiO 2-ceramic that D90 is 400nm, consumption is SiO 2-ceramic3%(mass fraction), adopt Henschel homogenizer, after high-speed mixing 1h, at 180 DEG C, vacuum bakeout 2h, obtains active matterMatter is processed pottery 4. Keeping the temperature of fluid bed chamber 3 by heater strip 5 is 80 DEG C, adopts roller 2 and roller 3, and traction barrier film advances,Due to 1 stickiness, ceramic particle can be deposited in its surface, adopts hairbrush to remove unnecessary particle again through roller 6 hot pressing, then through dryingDo and obtain ceramic modified barrier film.
Embodiment 2
As shown in Figure 2, vinylidene fluoride-hexafluoropropylene copolymer/DMF solution is heated to after 80 DEG C,Be placed in barrel 10, barrier film 9, by after barrel, hangs up one deck wet film on its surface, and after guide roller 11, spray gun array 16 willThe ceramic particle 15 of atomization is applied over wet film surface, and after twin rollers 14 hot pressing, more drying obtains ceramic modified barrier film. ThisPlace, the base material barrier film of employing is that thickness is the PE membrane surface of 16 μ m, and silane coupler adopts KH540, and pottery adopts aluminium oxide,Particle diameter D90 is 900nm, the 2%(mass fraction that KH540 amount is aluminium oxide ceramics), processing mode is to adopt Henschel high-speed stirredMachine, after high-speed mixing 2h, vacuum bakeout 2h at 180 DEG C, obtains active material and processes pottery. The modification herein obtaining everyFilm, a side is PVDF-HFP, opposite side is PVDF-HFP/ pottery, when heat endurance is improved, has saved ceramic useAmount is considerable advantage of the present invention.
Embodiment 3
Taking polyvinyl alcohol as binding agent, water is solvent, and solution is heated to after 80 DEG C, and it is 16 μ m's that one side is coated thicknessPE membrane surface (in advance through poly-dopamine processing), obtains the barrier film that stickiness slurry applies; Meanwhile, adopt silane couplerKH550 processes the zirconia ceramics that D90 is 500nm, the 2%(mass fraction that consumption is zirconia ceramics), adopt Henschel at a high speedMixer, after high-speed mixing 4h (zirconia ceramics density is larger, and incorporation time is longer), at 180 DEG C, vacuum bakeout 2h, obtainsActive material is processed pottery. Then adopt spray gun, with compressed air by the modified ceramic particle atomizing obtaining be sprayed at hygrometric state everyFilm surface, controlling coating thickness is 5 μ m, then through twin rollers hot pressing, more drying obtains ceramic modified barrier film.
Embodiment 4
Taking polyethylene glycol as binding agent, water is solvent, and solution is heated to after 80 DEG C, and it is 20 μ m's that one side is coated thicknessPP membrane surface (in advance through poly-dopamine processing), obtains the barrier film that stickiness slurry applies; Meanwhile, adopt silane couplerKH970 processes the barium titanate ceramics that D90 is 400nm, the 3%(mass fraction that consumption is barium titanate ceramics), adopt Henschel at a high speedMixer, after high-speed mixing 1h, vacuum bakeout 2h at 180 DEG C, obtains active material and processes pottery. Then adopt spray gun, withThe modified ceramic particle atomizing obtaining is sprayed at hygrometric state membrane surface by compressed air, and controlling coating thickness is 5 μ m, then through rightThe hot pressing of roller machine, more drying obtains ceramic modified barrier film.
Embodiment 5
Taking polyacrylamide as binding agent, water is solvent, and solution is heated to after 80 DEG C, and it is 16 μ m that one side is coated thicknessPE membrane surface (in advance through poly-dopamine processing), obtain the barrier film that stickiness slurry applies; Meanwhile, adopt silane couplerKH550 processes the zeolite granular that D90 is 100nm, the 5%(mass fraction that consumption is zeolite), adopt Henschel homogenizer,After high-speed mixing 4h, vacuum bakeout 4h at 180 DEG C, obtains active material and processes pottery. Then adopt spray gun, with compressed airThe modified ceramic particle atomizing obtaining is sprayed to hygrometric state membrane surface, and controlling coating thickness is 5 μ m, then through twin rollers heatPress, more drying obtains ceramic modified barrier film.

Claims (3)

1. a preparation method for ceramic modified lithium ion battery separator, is characterized in that concrete preparation process is as follows:
A) adopt hydrophily stickiness slurry coated polymer porous septum, the reaction cement in stickiness slurry contains can form hydrogenThe group of key;
B) adopt silane coupler to process ceramic particle;
C) by the stickiness membrane surface slurry obtaining in steps A still when the hygrometric state, by step B) ceramic particle handled is outstandingFloat on and in gas medium, be applied over its surface;
D) by C) diaphragm hot-pressing that obtains of step obtains product.
2. the preparation method of a kind of ceramic modified lithium ion battery separator according to claim 1, described in it is characterized in thatStep B) in active material for thering are one or more of silane coupler of structure (1):
3. the preparation method of a kind of ceramic modified lithium ion battery separator according to claim 1, described in it is characterized in thatStep D) in hot pressing, be hot pair roller type hot pressing.
CN201410288028.XA 2014-06-25 2014-06-25 A kind of preparation method of ceramic modified lithium ion battery separator Active CN104091910B (en)

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CN105070868B (en) * 2015-08-26 2017-12-08 厦门大学 A kind of dopamine modified ceramic composite diaphragm and its application
JP6824558B2 (en) * 2017-01-06 2021-02-03 エルジー・ケム・リミテッド Separation membrane for batteries to which a functional binder is applied and electrochemical elements to which this is applied
CN107611315A (en) * 2017-08-10 2018-01-19 无锡沄沨科技有限公司 A kind of PDVF painting methods of battery diaphragm
CN107492620A (en) * 2017-08-16 2017-12-19 广州鹏辉能源科技股份有限公司 A kind of high-temperature-reslithium lithium battery barrier film and preparation method thereof
CN110364661B (en) * 2018-04-11 2022-11-25 宁德新能源科技有限公司 Isolating membrane and energy storage device
CN109065801A (en) * 2018-07-09 2018-12-21 中国电力科学研究院有限公司 The preparation method and anodic aluminium oxide membrane of polymolecularity anodic aluminium oxide membrane slurry
CN109148798B (en) * 2018-08-08 2021-06-22 欣旺达电子股份有限公司 Lithium ion battery, coating diaphragm and preparation method thereof
CN109994694A (en) * 2019-02-25 2019-07-09 刘�英 A kind of preparation method of stable structure type lithium ion battery separator
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CN111029514B (en) * 2019-11-14 2021-09-28 珠海冠宇电池股份有限公司 Diaphragm and high-voltage battery comprising same
CN112909430A (en) * 2019-12-03 2021-06-04 恒大新能源技术(深圳)有限公司 Lithium ion battery diaphragm and preparation method thereof and lithium ion battery
CN113964450A (en) * 2020-07-17 2022-01-21 深圳市星源材质科技股份有限公司 Battery diaphragm coating liquid and preparation method thereof, battery diaphragm and battery
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