CN102394282B - Lithium ion secondary battery porous multilayer diaphragm and manufacture method thereof - Google Patents
Lithium ion secondary battery porous multilayer diaphragm and manufacture method thereof Download PDFInfo
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- CN102394282B CN102394282B CN201110382570.8A CN201110382570A CN102394282B CN 102394282 B CN102394282 B CN 102394282B CN 201110382570 A CN201110382570 A CN 201110382570A CN 102394282 B CN102394282 B CN 102394282B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 77
- 239000011248 coating agent Substances 0.000 claims abstract description 76
- 239000012528 membrane Substances 0.000 claims abstract description 39
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims description 36
- 230000004888 barrier function Effects 0.000 claims description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 24
- -1 polyethylene Polymers 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 21
- 239000004698 Polyethylene Substances 0.000 claims description 20
- 229920000573 polyethylene Polymers 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 7
- 230000002045 lasting effect Effects 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 18
- 229920000098 polyolefin Polymers 0.000 abstract description 16
- 239000010410 layer Substances 0.000 abstract description 10
- 239000011247 coating layer Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 description 14
- 230000001276 controlling effect Effects 0.000 description 12
- 229920006015 heat resistant resin Polymers 0.000 description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 9
- 229910052744 lithium Inorganic materials 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- 239000012530 fluid Substances 0.000 description 7
- 239000012982 microporous membrane Substances 0.000 description 7
- 238000011056 performance test Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920001230 polyarylate Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000306 polymethylpentene Polymers 0.000 description 2
- 239000011116 polymethylpentene Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012811 non-conductive material Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- 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
- H01M50/414—Synthetic resins, e.g. thermoplastics or thermosetting resins
-
- 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
-
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
-
- 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
- H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
- H01M50/491—Porosity
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/18—Homopolymers or copolymers of nitriles
- C08J2333/20—Homopolymers or copolymers of acrylonitrile
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
- H01M50/457—Separators, membranes or diaphragms characterised by the material having a layered structure comprising three or more layers
-
- 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 relates to the technical field of lithium ion battery and specifically relates to a lithium ion secondary battery porous multilayer diaphragm and a manufacture method thereof. The porous multilayer diaphragm comprises a polyolefin porous membrane and at least one layer of heatproof coating layer coated on the polyolefin porous membrane; the heatproof coating layer comprises heatproof resin and inorganic insulating particles in a mass ratio of 1:0.5-5. The porous multilayer diaphragm prepared by steps of preparing coating liquid, coating, stretching and fixing has excellent heat resistance; the heatproof coating is also a film with micropore structure and enough high amount of porosity and heat resistance temperature; even a microporous base film is fused and ruptured, the coating can still maintain integrity thereof and obstruct direct contact of cell electrodes, so as to guarantee cell safety; the heatproof coating layer communicates with micropores of the microporous film of the matrix film layer to guarantee permeation performance of lithium ions.
Description
Technical field
The present invention relates to technical field of lithium ion, be specifically related to a kind of lithium ion secondary battery porous multilayer diaphragm and manufacture method thereof.
Background technology
Chargeable lithium ion secondary cell have high working voltage, high-energy-density, long circulation life, memory-less effect, pollution-free characteristic and can fast charging and discharging etc. advantage, be widely used among daily electronics, electrical equipment and digital product, there is the wide market space and good development prospect.Along with the day by day raising of the mankind to portable cell quality demand, lithium rechargeable battery becomes the focus of novel power supply technical research in recent years.Seek lithium rechargeable battery more high-energy-density be the important directions of current research, the thing followed is the technical problem that how to ensure lithium battery safety.
Membrane for polymer is one of key components of lithium rechargeable battery, is the key that ensures lithium battery security performance, and the quality of its quality has a great impact the fail safe of the amount of capacity of lithium battery, useful life and battery.Membrane for polymer as lithium ion secondary battery membrane must meet certain requirement: first, barrier film itself must be electrically non-conductive material, and the both positive and negative polarity of battery is separated, and prevents two electrode contacts and short circuit; Secondly, barrier film must be porous material, allows the negative ions in electrolyte to pass through, the good ion guide general character between both positive and negative polarity in maintenance lithium ion battery charge and discharge process; The 3rd, barrier film must have the good performance of closing, when outside is owing to being short-circuited or when incorrect link makes inside battery produce very large electric current, when inside battery is elevated to uniform temperature, barrier film causes microcellular structure to be closed generation heat fusing, thereby cut-out electric current, quits work battery, guarantees cell safety; When finally, barrier film must have enough chemical stabilities, electrolyte resistance corrosion, can by electrolyte, be infiltrated and have enough mechanical strengths etc.
Along with the development of new-energy automobile, the design of lithium ion battery group makes the safety of lithium ion battery be subject to serious challenge, so lithium ion battery producer has proposed more and more higher requirement to lithium ion battery separator.Lithium ion battery separator must have suitable closed pore temperature, can cut off in time electric current, guarantees cell safety; Simultaneously barrier film must possess high heat resisting temperature, and temperature raises and causes barrier film fusing, breaks when preventing battery short circuit, causes battery to be short-circuited and explosion caused.
The suitable closed pore temperature that generally believes lithium battery diaphragm is 120-140 ℃, and closed pore temperature is too high or too low to be all not suitable for as lithium battery diaphragm.Polyethylene diaphragm closed pore temperature prepared by the wet method of take is 130-140 ℃, is comparatively ideal closed pore temperature, but the poor heat resistance of polyethylene barrier film, broken film temperature is lower than 150 ℃, and during battery short circuit, its fail safe can not get good guarantee.Although current, have and propose by regulating poly molecular weight, crystal structure and doping or laminated polyacrylic technology, the thermal endurance of barrier film prepared by these systems is still not enough.
There is in recent years scholar to propose the technology at the micro-porous septum surface-coated of polyethylene or laminated heat-resisting organic polymer resin composite membrane.Chinese invention patent CN101689624A discloses a kind ofly take polyethylene film as base material, at its surface coverage one deck, by fully aromatic polyamide with at the composite membrane of the more than 200 ℃ heat-resisting high-molecular organic material of the metal hydroxides of the temperature generation dehydration below 400 ℃, object is to provide a kind of thermal endurance, closes function, the barrier film of anti-flammability and treatability excellence.Described coating is laminated the forming of porous layer heat resistant polymer being formed by wet type freezing method, need to solidify, wash operations such as removing solidification liquid and drying water through solidification liquid, complex procedures, and the consistency of membrane thicknesses is poor.
Chinese invention patent CN101281961 discloses the coating composition that a kind of lithium ion secondary battery membrane is used, and specifically, is on polyethylene film, to apply the coating that contains electric insulation oxide particle and binding agent.The preparation of coating is to make coating fluid coating with in polyethylene based film, then convection drying moulding after containing binding agent, electric insulation oxide particle and stirring solvent.Because this painting method is ambient spray, described barrier film is difficult to guarantee the adhesive force between effective dispersion of inorganic particle and itself and binding agent, and coating pore structure is few.
Summary of the invention
In order to overcome above-mentioned defect, the object of the present invention is to provide a kind of lithium ion secondary battery porous multilayer diaphragm.
Another object of the present invention is to provide a kind of preparation method of lithium ion secondary battery porous multilayer diaphragm.
For achieving the above object, the technical solution adopted in the present invention is as follows:
A kind of lithium ion secondary battery porous multilayer diaphragm, it comprise polyolefin porous membrane and at least one deck be coated on the heat-resisting coating layer on polyolefin porous membrane, wherein heat-resisting coating layer is comprised of heat-resistant resin and inorganic insulation particle, and the weight ratio of heat-resistant resin and inorganic insulation particle is 1: 0.5-5.If the weight ratio of heat-resistant resin and inorganic insulation particle is less than 1: 0.5, the inorganic porous insulating particle adding is effect improved not obvious to barrier film thermal endurance effect and heat-shrinkable; If weight ratio is greater than 1: 5, resin content is too small, bonding not firm to inorganic non-conductive particle, easily occurs that inorganic ions comes off.
Heat-resistant resin described in the present invention is one or more mixing of Kynoar, Merlon, polyester, polyarylate, polyamide, polyacrylonitrile and poly(4-methyl-1-pentene) etc.
One or more mixing in oxide, carbide and the nitride of oxide, hydroxide or silicon that inorganic insulation particle of the present invention is aluminium, magnesium.
A manufacture method that contains the lithium ion secondary battery porous multilayer diaphragm of heat stable resin coating, it comprises that step is as follows:
A. prepare coating fluid: first heat-resistant resin being dissolved, is 1 by the weight ratio of heat stable resin and inorganic insulation particle: 0.2-10 adds inorganic insulation particle, is uniformly mixed the homogeneous coating fluid that is prepared into heat stable resin and inorganic insulation particle;
B. coating: above-mentioned coating fluid is coated on the surface in the hot many micropore basal membranes of polyolefin, forms thermal endurance coating, containing many micropore basal membranes of polyolefin solvent flashing of coat, obtain the microporous membrane containing micro porous coating after solvent evaporates;
C. stretch: the above-mentioned microporous membrane containing micro porous coating is vertical or horizontally carried out to simple tension or biaxial tension along it, expand coating micropore;
D. thermal finalization: the microporous membrane after above-mentioned stretching is carried out to thermal finalization, finally obtain the lithium ion secondary battery porous multilayer diaphragm containing heat stable resin coating.
In the manufacture method of the lithium ion secondary battery porous multilayer diaphragm containing heat stable resin coating of the present invention, described heat-resistant resin is one or more mixing of Kynoar, Merlon, polyester, polyarylate, polyamide, polyacrylonitrile and poly(4-methyl-1-pentene) etc.
In the manufacture method of the lithium ion secondary battery porous multilayer diaphragm containing heat stable resin coating of the present invention, described inorganic porous insulating particle is oxide, the hydroxide of aluminium, magnesium, and one or more mixing in the oxide of silicon, carbide and nitride.
In step a of the present invention, dissolving heat stable resin solvent used is one or more mixing in 1-METHYLPYRROLIDONE, N,N-DMAA, DMF, dimethyl sulfoxide (DMSO).
In a step of the present invention, heat-resistant resin fusing point is greater than 180 ℃; The specific area of inorganic insulation particle is 5-200m
2/ g; The consumption of heat-resistant resin accounts for the 5-50% of heat-resistant resin and solvent total weight.
In b step of the present invention, the microporous temperature of polyolefin is 50-100 ℃, and solvent evaporates temperature is 30-110 ℃, and the volatilization time is 10-300S.
In c step of the present invention, stretching can be the biaxial tension of vertical and horizontal, can be also vertical or horizontal simple tension.The total multiplying power stretching is 1.1-5 times, is preferably 1.5-3 doubly, and total multiplying power that stretches is less than 1.1, coating aperture reaming DeGrain; Stretching ratio is greater than 5, and coating easily departs from the many micropore basal membranes of polyolefin, and easy rupture of membranes.Draft temperature is 80-150 ℃, is preferably 90-120 ℃.
In d step of the present invention, the temperature of thermal finalization is 100-160 ℃, and heat-setting time is 10s-120s.
The granular size of the inorganic insulation particle in a step of the present invention is 10-1000nm.
In order to guarantee that lithium ion secondary battery porous multilayer diaphragm has enough mechanical performances and makes battery have sufficiently high energy density, when the thickness of the many micropore basal membranes of polyolefin is less than 10 μ m, every lepthymenia, the mechanical performance of barrier film is not enough, easy rupture of membranes, barrier film poor stability; When the thickness of the many micropore basal membranes of polyolefin is greater than 25 μ m, the thickness of the composite diaphragm obtaining after coating is excessive, causes the energy density of lithium ion battery to reduce, and is unfavorable for the application of dynamic lithium battery.The thickness of the many micropore basal membranes of polyolefin of the present invention is 12-25 μ m, and the thickness of every layer of refractory coating is 2-6 μ m; Finally obtain can adjusting according to demand containing the thickness of the lithium ion secondary battery porous multilayer diaphragm of heat stable resin coating, preferably its thickness is 18-40 μ m.
Lithium ion secondary battery porous multilayer diaphragm of the present invention, can be in single layer coating thermal endurance coating of the many micropore basal membranes of polyolefin, also can be according to performance need the identical or different coating thermal endurance coating of coated with multiple layer; Can carry out single or double to the many micropore basal membranes of polyolefin and apply thermal endurance coating, wherein its heat resistance of the porous multilayer diaphragm of dual coating gained is better.
Compared to existing technology, beneficial effect of the present invention is: the porous multilayer diaphragm coating that the present invention makes has good heat resistance, refractory coating is similarly the rete with multi-cellular structure, rete has sufficiently high porosity and heat resisting temperature, even the in the situation that of many micropore basal membranes of polyolefin generation melting rupture of membranes, coating still can keep its integrality, intercepts the direct contact of battery electrode, thereby ensures the fail safe of battery; The micropore of the microporous membrane of thermal endurance coating and matrix rete connects mutually, ensures the through performance of lithium ion.Porous multilayer diaphragm of the present invention expands the aperture of many micro porous coatings by follow-up biaxial tension, improve the ability that sees through of its porosity and lithium ion.Porosity by the prepared porous multilayer diaphragm of preparation method of the present invention is 30-80%, and gas permeability is 200-700s/100ml, and pore size is 0.01-0.2 μ m, and closed pore temperature is 130-140 ℃, and broken film temperature is greater than 190 ℃.
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment
A manufacture method that contains the lithium ion secondary battery porous multilayer diaphragm of heat stable resin coating, it comprises that step is as follows:
A. prepare coating fluid: first heat-resistant resin being dissolved, is 1 by the weight ratio of heat stable resin and inorganic insulation particle: 0.2-10 adds inorganic insulation particle, is uniformly mixed the homogeneous coating fluid that is prepared into heat stable resin and inorganic insulation particle;
B. coating: above-mentioned coating fluid is coated on the surface in the hot many micropore basal membranes of polyolefin, forms thermal endurance coating, containing many micropore basal membranes of polyolefin solvent flashing of coat, obtain the microporous membrane containing micro porous coating after solvent evaporates;
C. stretch: the above-mentioned microporous membrane containing micro porous coating is vertical or horizontally carried out to simple tension or biaxial tension along it, expand coating micropore;
D. thermal finalization: the microporous membrane after above-mentioned stretching is carried out to thermal finalization, finally obtain the lithium ion secondary battery porous multilayer diaphragm containing heat stable resin coating.
It is below the preferred embodiment of the invention.
Embodiment 1
10g PETG (PET, fusing point 256-265 ℃) is joined in the beaker of DMF (DMF) solvent that fills 100g, be heated to 80 ℃, and slowly stir with blender, until resin dissolves.By 10g magnesium oxide (MgO, average grain is 500nm) evenly join in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, with the coating speed of 5 centimetres/s, be coated on the many micropore basal membranes of polyethylene, the temperature of controlling solvent evaporates is 80 ℃, and the time of controlling solvent evaporates by blowing mode is 60S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing heat stable resin and magnesian many micropores refractory layer; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.3 times, and Width stretches 1.3 times, and the micropore size of refractory coating is expanded; Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 26 μ m.The performance test data of barrier film is in Table 1.
Embodiment 2
10g polyacrylonitrile is joined in the beaker of DMF (DMF) solvent that fills 100g, be heated to 80 ℃, and slowly stir with blender, until resin dissolves.By 10g aluminium oxide (Al
2o
3average grain is 500nm) evenly join in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, with the coating speed of 5 centimetres/s, be coated on the many micropore basal membranes of polyethylene, the temperature of controlling solvent evaporates is 80 ℃, and the time of controlling solvent evaporates by blowing mode is 100S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing many micropores refractory layer of heat stable resin and aluminium oxide; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.3 times, and Width stretches 1.3 times, and the micropore size of refractory coating is expanded.Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 29 μ m.The performance test data of barrier film is in Table 1.
Embodiment 3
10g Kynoar is joined in the beaker of the 1-METHYLPYRROLIDONE solvent that fills 100g, be heated to 80 ℃, and slowly stir with blender, until resin dissolves.By 20g silicon dioxide (SiO
2average grain is 500nm) evenly join in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, with the coating speed of 5 centimetres/s, be coated on the many micropore basal membranes of polyethylene, the temperature of controlling solvent evaporates is 80 ℃, and the time of controlling solvent evaporates by blowing mode is 60S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing many micropores refractory layer of heat stable resin and aluminium oxide; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.3 times, and Width stretches 1.3 times, and the micropore size of refractory coating is expanded.Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 30 μ m.The performance test data of barrier film is in Table 1.
Embodiment 4
10g Merlon is joined in the beaker of DMF (DMF) solvent containing 100g, be heated to 80 ℃, and slowly stir with blender, to resin dissolves.By 20g aluminium hydroxide (Al (OH)
3average grain is 500nm) evenly join in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, with the coating speed of 5 centimetres/s, be coated on the many micropore basal membranes of polyethylene, the temperature of controlling solvent evaporates is 100 ℃, and the time of controlling solvent evaporates by blowing mode is 10S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing many micropores refractory layer of heat stable resin and aluminium oxide; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.3 times, and Width stretches 1.3 times, and the micropore size of refractory coating is expanded.Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 26 μ m.The performance test data of barrier film is in Table 1.
Embodiment 5
10g Merlon is joined in the beaker of DMF (DMF) solvent containing 100g, be heated to 80 ℃, and slowly stir with blender, to resin dissolves.By 20g aluminium hydroxide (Al (OH)
3average grain is 500nm) evenly join in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, with the coating speed of 5 centimetres/s, be coated on the many micropore basal membranes of polyethylene, the temperature of controlling solvent evaporates is 80 ℃, and the time of controlling solvent evaporates by blowing mode is 60S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing many micropores refractory layer of heat stable resin and aluminium oxide; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.4 times, and Width stretches 1.4 times, and the micropore size of refractory coating is expanded.Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 27 μ m.The performance test data of barrier film is in Table 1.
Embodiment 6
20g Merlon is joined in the beaker of DMF (DMF) solvent containing 100g, be heated to 80 ℃, and slowly stir with blender, to resin dissolves.By 20g aluminium hydroxide (Al (OH)
3average grain is 500nm) evenly join in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, with the coating speed of 5 centimetres/s, be coated on the many micropore basal membranes of polyethylene, the temperature of controlling solvent evaporates is 80 ℃, and the time of controlling solvent evaporates by blowing mode is 60S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing many micropores refractory layer of heat stable resin and aluminium oxide; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.5 times, and Width stretches 1.5 times, and the micropore size of refractory coating is expanded.Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 28 μ m.The performance test data of barrier film is in Table 1.
Table 1:
Above-described embodiment is only the preferred embodiments of the present invention, can not limit protection scope of the present invention with this, and the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (1)
1. the manufacture method containing the lithium ion secondary battery porous multilayer diaphragm of heat stable resin coating, it is characterized in that: 10g polyacrylonitrile is joined in the beaker of the DMF solvent that fills 100g, be heated to 80 ℃, and slowly stirring with blender, until resin dissolves; The aluminium oxide that is 500nm by 10g average grain evenly joins in above-mentioned solution, stir, and the lasting 60min that stirs, obtain uniform suspension, in whipping process, beaker mouth should seal, reduce the volatilization of solvent, by thickness, be that the many micropore basal membranes of polyethylene that 20 μ m, porosity are 50% are heated to 100 ℃ afterwards, and by above-mentioned suspension by the mode of blade coating, coating speed with 5 centimetres/s is coated on the many micropore basal membranes of polyethylene, and the temperature of controlling solvent evaporates is 80 ℃, and the time of controlling solvent evaporates by blowing mode is 100S; Again the one side of uncoated suspension is carried out to above-mentioned coating step subsequently, obtain two sides and be all attached with equably the barrier film containing many micropores refractory layer of heat stable resin and aluminium oxide; The barrier film of above-mentioned preparation is carried out to low power stretch processing, and draft temperature is 110 ℃, and length direction stretches 1.3 times, and Width stretches 1.3 times, and the micropore size of refractory coating is expanded; Through thermal finalization at 120 ℃ 60 seconds, obtain the porous multilayer composite diaphragm that thickness is 29 μ m.
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| CN201110382570.8A CN102394282B (en) | 2011-11-25 | 2011-11-25 | Lithium ion secondary battery porous multilayer diaphragm and manufacture method thereof |
| PCT/CN2012/080782 WO2013075524A1 (en) | 2011-11-25 | 2012-08-30 | Porous multi-layer separating film for lithium ion secondary battery and method for manufacturing same |
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| JP2013222582A (en) | 2012-04-16 | 2013-10-28 | Sony Corp | Secondary battery, battery pack, electric vehicle, power storage system, power tool, and electronic equipment |
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| CN102942831B (en) * | 2012-11-21 | 2014-10-29 | 佛山市金辉高科光电材料有限公司 | Coating composite for lithium ion secondary battery membrane and method for manufacturing membrane |
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