CN108390000A - A kind of preparation method of high-performance Low ESR composite diaphragm - Google Patents
A kind of preparation method of high-performance Low ESR composite diaphragm Download PDFInfo
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- CN108390000A CN108390000A CN201810135745.7A CN201810135745A CN108390000A CN 108390000 A CN108390000 A CN 108390000A CN 201810135745 A CN201810135745 A CN 201810135745A CN 108390000 A CN108390000 A CN 108390000A
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- Prior art keywords
- preparation
- coating
- diaphragm
- lithium battery
- coating material
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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
- 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
- H01M50/431—Inorganic 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 present invention provides a kind of preparation methods of high-performance Low ESR composite diaphragm.The present invention passes through with graphene, graphite, carbon nanotube, acetylene black, Al2O3In one or more be raw material, be coated with one layer of slurry in membrane surface, so as to improve the thermal stability of polyolefin lithium battery diaphragm, thermal coefficient and realize high current charge-discharge, improve the wellability of electrolyte；In addition interface impedance is substantially reduced to reduce the impedance of lithium battery；And then improve the cyclical stability and cycle life of lithium battery；To prepare the low-impedance lithium battery diaphragm more stablized, in lithium battery, improving service life and the performance of battery.
Description
Technical field
A kind of low-impedance composite battery separator film material of high-performance, more particularly to diaphragm for lithium ion battery are invented in this research
Material and its forming method, belong to technical field of lithium-ion battery.
Background technology
In the structure of lithium battery, diaphragm is one of the interior layer assembly of key；The performance of diaphragm determines the interface of battery
Structure and internal resistance etc. directly affect the characteristics such as capacity, cycle, the security performance of battery.Diaphragm material is difficult to realize quotient at present
Industry be because of its service life reason, therefore, exploitation high security and inexpensive battery diaphragm be future studies main target it
One.With the high speed development of lithium ion battery industry, lithium ion battery separator material becomes hot research problem instantly；Lithium from
The improved technology of sub- battery diaphragm has also obtained the attention and concern of bigger.Lithium ion battery separator plays crucial make in battery
With the anode and cathode of its main function isolation battery prevent short circuit, while lithium ion being allowed quickly to be passed in positive and negative interpolar
It is defeated.Currently, the lithium battery diaphragm of commercialization is based on polyolefin (PP, PE) single thin film or plural layers.Although it has
Electrochemical stability is good, and intensity is high, it is at low cost the advantages that, but porous polyolefin at relatively high temperatures under conditions of have and shrink
The self-closing in gap acts on, and causes impedance obviously to rise, is restricted by the electric current of battery, can prevent to a certain extent by
It is a kind of relatively reliable lithium battery material in explode caused by overheat phenomena such as；In addition the fusing point one of polyolefin-based separator
As at 170 DEG C hereinafter, being easily deformed under high temperature.When battery temperature increases under the effect of external or internal factor, diaphragm can be sent out
Raw deformation retract, it is likely that cause battery short circuit, cause the generation of explosion accident.The especially power battery of high power discharge, makes
Higher with internal temperature of battery in the process, this requires diaphragms to have better thermal safety energy.It is swift and violent with battery industry
Development, graphene, carbon nanotube, inorganic ceramic material (Al2O3、SiO2), graphite become research hotspot instantly, past
The method that many improved polyalkene lithium battery diaphragms are reported in 10 years, such as Al2O3Or SiO2Coating polyolefin lithium battery is ground
Study carefully；Currently, there has been no graphene coated Al2O3The slurry of powder/carbon nano tube/graphene/graphite is coated with polyolefin lithium battery
Any report of diaphragm, our achievement in research have confirmed that the ornamental of its feasibility and development.
For drawbacks described above, Chinese patent CN105336901A discloses the preparation side that diaphragm is coated between a kind of high-performance hole
Method is coated with a thin layer of heat-resisting material between membrane surface and hole, improves the heat resistance of diaphragm by the method for dip-coating
And the wellability of electrolyte；It coats the high temperature resistance of metacneme and thermal coefficient increases and interface impedance substantially reduces；
To greatly improve the service life of lithium battery.In addition Chinese patent CN1969407A, CN102306726A and United States Patent (USP)
US2013/0183570 A1 propositions use PVDF-HFP as adhesive and Al2O3、BaTiO3Equal inorganic fillers are made into slurry coating
On polyalkene diaphragm, substantially increases the heat resistance of diaphragm and absorb the ability for keeping electrolyte.In addition Chinese patent
CN101689624A discloses three primary cell of diaphragm for non-water system secondary battery, non-fabrication method and non-water system；And patent
CN1969407A discloses organic/inorganic composite porous film and the research using its electrochemical appliance.Its purpose is all
Its security performance and service life are improved in order to solve the thermal stability of diaphragm and reduce interface impedance.
Invention content
The present invention is coated with one layer of slurry by way of dip-coating, in membrane surface, so as to improve the heat resistance of diaphragm
With the wellability of electrolyte；And reduce the impedance of lithium battery by reducing the interface impedance of diaphragm.
In order to achieve the above purpose, the present invention provides a kind of preparation methods of high-performance Low ESR composite diaphragm.It should
Composite diaphragm is by basement membrane and is coated on the coating material of membrane surface and forms, it is characterised in that table of the coating material in composite diaphragm
There are microcellular structure in face and inside, and it is little that gas permeability compares variation with basement membrane.The present invention provides a kind of composite diaphragm material,
The performance of lithium battery can be improved；And then promote the progress of battery industry.It can solve problems with：
1. by reducing interface impedance to reduce the impedance of lithium battery；Improve stability and the service life of lithium battery.
2. by improving the thermal coefficient of polyolefin lithium battery diaphragm and realizing high current charge-discharge, and then improving lithium battery
Cyclical stability and cycle life.
It is as follows：
(1) coating material is dissolved in organic solvent at a certain temperature, slurry, the mass fraction of coating material is made
For 5%-70%；
(2) slurry in step (1) is coated on by way of dip-coating on basement membrane, then by naturally dry or drying,
Obtain finished film.
Above-mentioned coating material includes graphene, graphite, carbon nanotube, acetylene black, Al2O3In one or more.
Above-mentioned organic solvent is N,N-dimethylformamide, N- dimethyl pyrrolidines copper, butadiene-styrene rubber, sodium alginate, CMC
With the one or more in acetone.
The mass fraction of above-mentioned coating material is 5%-70%.Coating material mass fraction is control composite diaphragm performance
Key parameter.Under the premise of certain porosity and aperture basement membrane, the concentration of coating material is bigger, and coating is thicker, diaphragm
Heat resistance is better, but the blocking of device to hole is more serious, and gas permeability declines, and impedance reduces；The concentration of coating material is smaller, and coating is got over
Thin, the influence to gas permeability is smaller, and heat resistance improves limited, impedance raising.When the mass fraction of coating material is 5%, always
Coating quality score is improved, impedance can be reduced constantly, but be promoted to after 70%, and raised trend is presented in impedance.But because
This, for a certain basement membrane, composite diaphragm will have relatively good performance, it is desirable that slurry will have suitable concentration.
The solution temperature of above-mentioned coating material in organic solvent is at 5 DEG C -100 DEG C.
Preferably, the solution temperature of above-mentioned coating material in organic solvent is at 45 DEG C -90 DEG C.Because of solution temperature mistake
Height, the easy decomposition of coating material, manufactured slurry are evenly distributed, and coating effect is more preferable；Otherwise, on the contrary.
Above-mentioned basement membrane can be graphene, graphite, carbon nanotube, acetylene black, Al2O3In one or more.Basement membrane
Thickness range at 4 μm -80 μm, porosity ranges 30%-85%, average pore size is at 0.02 μm -10 μm.
The speed of above-mentioned dip-coating is 0.3m/min-15m/min, and hot blast temperature is 50 DEG C -100 DEG C.Wherein dip-coating speed pair
In membrane properties also there is large effect, the speed of dip-coating to influence production efficiency slowly excessively, the excessive velocities of dip-coating are difficult then to reach
To expected coating effect.
Advantages of the present invention：
(1) by the way that in polyalkene diaphragm surface Coating material, interface impedance can be significantly reduced, to reduce lithium electricity
The impedance in pond；
(2) by the way that in polyalkene diaphragm surface Coating material, the wellability of electrolyte can be improved.
(3) by the way that in polyalkene diaphragm surface Coating material, the heat resistance of diaphragm can be improved.
Description of the drawings
Fig. 1 CMC and sodium alginate binder admixed graphite are prepared into slurry coating polyolefin lithium battery diaphragm PP/PE/PP
Lithium battery stable circulation performance.
Admixed graphite is prepared into slurry coating polyolefin lithium battery diaphragm PP/ respectively for Fig. 2 CMC and sodium alginate binder
The EIS of the lithium battery of PE/PP is tested.
The lithium electricity of Fig. 3 sodium alginates and CMC binder mixing and doping graphite coating polyolefin lithium battery diaphragm PP/PE/PP
The stable circulation performance in pond.
The lithium electricity of Fig. 4 sodium alginates and CMC binder mixing and doping graphite coating polyolefin lithium battery diaphragm PP/PE/PP
The EIS in pond is tested.
The friendship of the lithium battery of the graphene coating polyolefin lithium battery diaphragm PP/PE/PP of charge and discharge under Fig. 5 0.5C multiplying powers
Flow impedance (EIS) is tested.
The friendship of the lithium battery of the graphene coating polyolefin lithium battery diaphragm PP/PE/PP of charge and discharge under the big multiplying powers of Fig. 6 20C
Flow impedance (EIS) is tested.
Specific implementation mode
To further illustrate present disclosure below in conjunction with specific embodiment and attached drawing, but the protection of the present invention
Range is not limited only to the content of embodiment description, but also concerning the material of coating.
Embodiment 1
The coating material that mass fraction is 5% is added in measuring cup simultaneously with organic solvent (sodium alginate or CMC, SBR)
Suitable deionized water is added to be uniformly mixed, is dissolved at 60 DEG C, in stirring 1h, mixing speed 90r/ on magnetic stirring apparatus
Min is coated in a manner of dip-coating on PE diaphragms after stirring, and the porosity of PE diaphragms is 43%, average pore size 42nm, thickness
25 μm of degree.Coating speed is 5m/min, then puts 40 DEG C of drying in air dry oven into, is taken out after 1h, obtain composite diaphragm, used
Sheet-punching machine is cut into the round pole piece of certain diameter, is put into 50 DEG C of drying in vacuum drying chamber, spare.
Embodiment 2
The coating material that mass fraction is 30% is added in measuring cup simultaneously with organic solvent (sodium alginate or CMC, SBR)
Suitable deionized water is added and is uniformly mixed and is dissolved at 60 DEG C, in stirring 1h, mixing speed 90r/ on magnetic stirring apparatus
Min is coated in a manner of dip-coating on PE diaphragms after stirring, and the porosity of PE diaphragms is 43%, average pore size 42nm, thickness
25 μm of degree.Coating speed is 5m/min, then puts 40 DEG C of drying in air dry oven into, is taken out after 1h, obtain composite diaphragm, used
Sheet-punching machine is cut into the round pole piece of certain diameter, is put into 50 DEG C of drying in vacuum drying chamber, spare.
Embodiment 3
The coating material that mass fraction is 70% is added in measuring cup simultaneously with organic solvent (sodium alginate or CMC, SBR)
Suitable deionized water is added and is uniformly mixed and is dissolved at 60 DEG C, in stirring 1h, mixing speed 90r/ on magnetic stirring apparatus
Min is coated in a manner of dip-coating on PE diaphragms after stirring, and the porosity of PE diaphragms is 43%, average pore size 42nm, thickness
25 μm of degree.Coating speed is 5m/min, then puts 40 DEG C of drying in air dry oven into, is taken out after 1h, obtain composite diaphragm, used
Sheet-punching machine is cut into the round pole piece of certain diameter, is put into 50 DEG C of drying in vacuum drying chamber, spare.
Embodiment 4
The coating material that mass fraction is 70% is added in measuring cup simultaneously with organic solvent (sodium alginate or CMC, SBR)
Suitable deionized water is added and is uniformly mixed and is dissolved at 60 DEG C, in stirring 1h, mixing speed 90r/ on magnetic stirring apparatus
Min is coated in a manner of dip-coating on PP diaphragms after stirring, and the porosity of PP diaphragms is 40%, average pore size 28nm, thickness
25 μm of degree.Coating speed is 5m/min, then puts 40 DEG C of drying in air dry oven into, is taken out after 1h, obtain composite diaphragm, used
Sheet-punching machine is cut into the round pole piece of certain diameter, is put into 50 DEG C of drying in vacuum drying chamber, spare.
Embodiment 5
The coating material that mass fraction is 70% is added in measuring cup simultaneously with organic solvent (sodium alginate or CMC, SBR)
Suitable deionized water is added and is uniformly mixed and is dissolved at 60 DEG C, in stirring 1h, mixing speed 90r/ on magnetic stirring apparatus
Min is coated in a manner of dip-coating on PP/PE/PP diaphragms after stirring, and the porosity of PP/PE/PP diaphragms is 42%, is put down
Equal aperture 32nm, 25 μm of thickness.Coating speed is 5m/min, then puts 40 DEG C of drying in air dry oven into, takes out, obtain after 1h
To composite diaphragm, it is cut into the round pole piece of certain diameter with sheet-punching machine, is put into 50 DEG C of drying in vacuum drying chamber, it is spare.
By Fig. 1-6 it is found that can significantly reduce the impedance of lithium battery using graphite or graphene as coating material, up to 10
It is more again, and improve the stability of lithium battery.
Claims (7)
1. a kind of preparation method of high-performance Low ESR composite diaphragm, it is characterised in that：
(1) coating material is dissolved at a certain temperature and uniformly mixed slurry is made in a binder, the quality of coating material
Score is 5%-70%；
(2) slurry in step (1) is applied to by way of dip-coating on basement membrane, then by naturally dry or drying, is obtained
Finished film.
2. preparation method according to claim 1, which is characterized in that coating material is graphene, graphite, carbon nanotube, second
Acetylene black, Al2O3In one or more.
3. preparation method according to claim 1, which is characterized in that the organic solvent is n,N-Dimethylformamide, N-
One or more in dimethyl pyrrolidine copper, butadiene-styrene rubber, sodium alginate, CMC and acetone.
4. preparation method according to claim 1, which is characterized in that the temperature that the coating material dissolves in organic solvent
Degree is at 5 DEG C -110 DEG C.
5. preparation method according to claim 4, which is characterized in that the dissolving temperature of the coating material in organic solvent
Degree is at 45 DEG C -90 DEG C.
6. according to preparation method described in claim 1-5, which is characterized in that the thickness range of the basement membrane is 4 μm -80 μm, hole
Gap rate ranging from 30%-85%, average pore size is at 0.02 μm -10 μm.
7. according to preparation method described in claim 1-5, which is characterized in that the speed of the dip-coating is 0.3m/min-15m/
Min, hot blast temperature are 50 DEG C -100 DEG C.
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| CN201810135745.7A CN108390000A (en) | 2018-02-09 | 2018-02-09 | A kind of preparation method of high-performance Low ESR composite diaphragm |
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| CN201810135745.7A CN108390000A (en) | 2018-02-09 | 2018-02-09 | A kind of preparation method of high-performance Low ESR composite diaphragm |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109786623A (en) * | 2018-12-29 | 2019-05-21 | 深圳中兴新材技术股份有限公司 | Improve the method and polymer coating diaphragm of polymer coating diaphragm ionic conductivity |
| CN110148697A (en) * | 2019-05-22 | 2019-08-20 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of polyolefin lithium battery diaphragm coating paste and its application |
| CN112688022A (en) * | 2020-12-28 | 2021-04-20 | 安普瑞斯（无锡）有限公司 | Quick charge-discharge lithium ion battery and preparation method thereof |
| CN112952293A (en) * | 2021-01-29 | 2021-06-11 | 枣阳市格芯电子科技有限公司 | Explosion-proof low-internal-resistance lithium ion battery and preparation method thereof |
| US20210288383A1 (en) * | 2020-03-10 | 2021-09-16 | Samsung Sdi Co., Ltd. | Coating composition for separator, method for preparing separator using the same, and separator and lithium battery employing the separator |
| CN113629358A (en) * | 2021-07-09 | 2021-11-09 | 惠州锂威新能源科技有限公司 | Composite diaphragm, preparation method thereof and lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109786623A (en) * | 2018-12-29 | 2019-05-21 | 深圳中兴新材技术股份有限公司 | Improve the method and polymer coating diaphragm of polymer coating diaphragm ionic conductivity |
| CN110148697A (en) * | 2019-05-22 | 2019-08-20 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of polyolefin lithium battery diaphragm coating paste and its application |
| US20210288383A1 (en) * | 2020-03-10 | 2021-09-16 | Samsung Sdi Co., Ltd. | Coating composition for separator, method for preparing separator using the same, and separator and lithium battery employing the separator |
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Inventor after: Liu Jianhong Inventor after: Ouyang Xiaoping Inventor after: Huang Jiayuan Inventor after: Xiong Wei Inventor after: Zhang Qianling Inventor after: He Chuanxin Inventor after: Liu Jinxin Inventor after: Zhang Xiaoyong Inventor after: Wu Qi Inventor after: Sun Xueliang Inventor before: Liu Jianhong |
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Application publication date: 20180810 |