CN110176568A - A kind of preparation method of high-performance coating diaphragm - Google Patents
A kind of preparation method of high-performance coating diaphragm Download PDFInfo
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- CN110176568A CN110176568A CN201910414100.1A CN201910414100A CN110176568A CN 110176568 A CN110176568 A CN 110176568A CN 201910414100 A CN201910414100 A CN 201910414100A CN 110176568 A CN110176568 A CN 110176568A
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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
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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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- 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
- 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
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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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Abstract
A kind of preparation method of high-performance coating diaphragm, the coating including basement membrane and its surface.Its floating coat is made of coating material one, coating material two and binder.Coating material one includes aluminium nitride, aluminum oxide, boron nitride, magnesium hydroxide, calcium hydroxide, one or more of silica；Coating material two includes fluorographite, graphite oxide, fluorinated graphite, fluorinated graphene, graphene oxide, one or more of Fluorinated graphene oxide.Coating material one of the present invention can effectively improve the thermal stability of diaphragm, thermal conductivity；Coating material two has biggish specific surface area, can be obviously improved the liquid-keeping property of diaphragm, this top layer material two resistance to oxidation current potential also with higher can effectively promote the oxidative resistance of diaphragm.Diaphragm prepared by the present invention has high-termal conductivity, high thermal stability and high liquid retention, can effectively improve the heating problem of lithium battery, is obviously improved the high rate performance of lithium battery, cycle performance etc..
Description
Technical field
The present invention relates to battery material fields, more particularly to a kind of preparation method of high-performance coating diaphragm.
Background technique
With the continuous development of battery technology, demand of the people to new-energy automobile is also increasing, and the safety of battery is asked
Topic is also increasingly taken seriously.Its septation plays an important role in cell safety.Diaphragm as one of big material of battery four,
Separation positive and negative anodes are played in the battery, the ion in electrolyte is allowed to pass through, while the closed pore in inside battery overheat, prevent to fill
The effect continued put.
Conventional membrane mainly uses polyethylene, polypropylene and polyethylene polypropylene composite membrane.It is resistance to high mechanical strength
The advantages that corrosive nature is good.But the heat distortion temperature of polypropylene and polyethylene is lower, once internal temperature of battery is excessively high,
Diaphragm is shunk, and be will lead to battery positive/negative plate contact, is generated huge security risk.It is now widely used ceramics every
Film is that aluminum oxide is coated in membrane surface, and the introducing of aluminum oxide can effectively improve the problem of diaphragm is heat-shrinked,
Simultaneously because aluminum oxide particle is small, moreover it is possible to promote the liquid-keeping property of diaphragm.But since aluminum oxide particle is smaller, hold
Easily reunite, leading to it is not to be uniformly coated in membrane surface, the hole of diaphragm can be blocked when it is packed together,
So that diaphragm porosity declines, ion percent of pass is reduced, and seriously affects the performance of diaphragm.
Summary of the invention
The purpose of the present invention is to solve proposing in above-mentioned background problems, a kind of high-performance coating diaphragm is provided
Preparation method, its good heat conductivity, thermal stability is high, and liquid-keeping property is strong, and resistance to oxidation current potential is high, even pore distribution.
The object of the present invention is achieved like this: a kind of preparation method of high-performance coating diaphragm, comprising the following steps:
Step 1: coating material one, coating material two and binder are stirred evenly in a solvent, are configured to aaerosol solution；
Step 2: aaerosol solution is uniformly coated on membrane surface and drying, obtains coated separator.
Coating material one in the step 1 includes aluminium nitride, aluminum oxide, boron nitride, magnesium hydroxide, hydroxide
Calcium, one or more of silica.
The particle size of coating material one in the step 1 is 1nm-5 μm.
Coating material two in the step 1 includes fluorographite, graphite oxide, fluorinated graphite, fluorographite
Alkene, graphene oxide, one or more of Fluorinated graphene oxide.
The specific surface area of coating material two in the step 1 is 0.1-1000m2/g。
Fluorination/oxidation of coating material two in the step 1 is compared for 0.01-1.25.
Binder in the step 1 includes Kynoar, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, polyacrylic acid, and poly- third
Alkene is fine, phenolic resin, one or more of epoxy resin.
Solvent in the step 1 includes water, ethyl alcohol, isopropanol, poly-methyl pyrrole alkanone, ethylene glycol, glycerol, positive fourth
One or more of alcohol.
The solid content of suspension in the step 1 is 10-99%.
Suspension coating material one in the step 1: coating material two: binder: the mass ratio of solvent is 10-
90:10-90:1-10:10-90。
Basement membrane in the step 2 is polyethylene film, polypropylene screen, polyethylene and polypropylene composite film, non-woven membrane,
One or more of cellulose membrane.
Basement membrane thickness in the step 2 is 5-100 μm.
Coating in the step 2 with a thickness of 1-20 μm.
Coating in the step 2 is single or double coating.
Compared with the prior art, the invention has the following advantages that
1. coated separator made from the preparation method has thermal conductivity more better than aluminum oxide diaphragm and thermal stability；
2. coated separator made from the preparation method has liquid-keeping property more better than aluminum oxide diaphragm；
3. coated separator made from the preparation method has higher resistance to oxidation current potential；
4. the particle of coating material one can be preferably dispersed on the lamella of coating material two due to the introducing of coating material two
Face so that coating is more uniform, prepared coated separator distribution of pores it is more uniform, prepared battery performance is more preferable.
Detailed description of the invention
Fig. 1 is the aluminium nitride/fluorographite coated separator for preparing of the embodiment of the present invention 1 in 0.1C ~ 10C under different sections
High rate performance test result figure.
Fig. 2 is that comparative example 1 is commercialized high rate performance test result figure of the polypropylene screen in 0.1C ~ 10C under different sections.
Fig. 3 is that high rate performance of the aluminum oxide coating diaphragm of the preparation of comparative example 2 in 0.1C ~ 5C under different sections is surveyed
Test result figure.
Fig. 4 is above-mentioned difference diaphragm room temperature 1C circulation figure.
Fig. 5 is aluminium nitride/fluorographite coated separator prepared by above-described embodiment 1 and three oxidations two prepared by comparative example 2
55 DEG C of 1C of aluminized coating diaphragm recycle figure.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, clear, complete description is carried out to technical solution of the present invention.
Embodiment 1
(1) preparation of diaphragm
By 3.7kg aluminium nitride (Dmax≤ 500nm), 0.2kg fluorographite (F:C/=1.2, specific surface area >=100m2/ g),
0.3kgPVDF, 6kg poly-methyl pyrrole alkanone are added in blender and stir for 24 hours, and being configured to solid content is 41.7% stable homogeneous
Aaerosol solution.The suspension prepared is uniformly coated on above the polypropylene basement membrane with a thickness of 12 μm by coating machine, so
Oven dried is crossed afterwards, and obtaining coating layer thickness is 4 μm, the single side coated separator that overall thickness is 16 μm.
(2) quantitative measurement
To verify invention effect, quantitative measurement is carried out to the present invention, quantitative measurement project includes: porosity, is breathed freely
Degree is heat-shrinked, dielectric constant, imbibition rate, conductivity, peel strength etc..
(3) electrochemical property test
To verify invention effect, the present invention is prepared into 2714897 type aluminum hull battery cores and carries out electrochemical property test.Chemical property
Test item includes high rate performance, cycle performance, battery temperature rise etc..Specific 2714897 aluminum hull battery core is produced as follows:
Anode: with LiNi1/3Co1/3Mn1/3O2For active material, SP is conductive agent, and PVDF is binder, N-Methyl pyrrolidone
For solvent, according to LiNi1/3Co1/3Mn1/3O2: the mass ratio of SP:PVDF=90:5:5 is homogenized, coating.
Cathode: using artificial graphite as active material, SP is conductive agent, and CMC is thickener, and SBR is binder, and water is molten
Agent, according to artificial graphite: the mass ratio of SP:CMC:SBR=90:5:2:3 is homogenized, coating.
Roll-in is carried out to prepared positive/negative plate, is wound, assembly, diaphragm used is prepared by the above method.Electrolyte
For 1mol/L LiPF6/ EC+DMC(1:1, w/w).The range of the charging/discharging voltage of electrochemical property test is 2.8V-4.2V, times
The range of rate test is 0.1C-10C；Loop test includes room temperature 1C circulation and 55 DEG C of high temperature circulations.
Embodiment 2
By 4.0kg aluminium nitride (Dmax≤ 1 μm), 0.5kg fluorinated graphene (F:C/=1.2, specific surface area >=100m2/ g),
0.5kgPVDF, 6kg poly-methyl pyrrole alkanone are added in blender and stir for 24 hours, and being configured to solid content is 45.5% stable homogeneous
Aaerosol solution.The suspension prepared is uniformly coated on above the polypropylene basement membrane with a thickness of 16 μm by coating machine, so
Oven dried is crossed afterwards, and obtaining coating layer thickness is 6 μm, the single side coated separator that overall thickness is 22 μm.
Embodiment 3
By 4.0kg aluminium nitride (Dmax≤ 10 μm), 0.5kg fluorographite (F:C/=1.25, specific surface area >=200m2/ g),
0.5kgCMC, 0.5kg butadiene-styrene rubber, 6kg deionized water are added in blender and stir for 24 hours, and being configured to solid content is 45.7% uniform
Stable aaerosol solution.The suspension prepared is uniformly coated in the polyethylene based film with a thickness of 12 μm by coating machine
Then oven dried is crossed in face, obtaining coating layer thickness is 6 μm, the single side coated separator that overall thickness is 18 μm.
Embodiment 4
By 3.6kg aluminium nitride (Dmax≤ 1 μm), 0.3kg fluorinated graphene (F:C/=1, specific surface area >=70m2/ g),
0.5kgCMC, 0.5kg butadiene-styrene rubber, 8kg deionized water are added in blender and stir 12h, and being configured to solid content is 35.4% uniform
Stable aaerosol solution.The suspension prepared is uniformly coated in the polyethylene based film with a thickness of 9 μm by coating machine
Then oven dried is crossed in face, obtaining coating layer thickness is 3 μm, the coated on both sides diaphragm that overall thickness is 15 μm.
Embodiment 5
By 4.0kg aluminum oxide (Dmax≤ 10 μm), 0.3kg fluorographite (F:C/=1.1, specific surface area >=90m2/ g),
0.5kgCMC, 0.5kg butadiene-styrene rubber, 8kg deionized water are added in blender and stir 15h, and being configured to solid content is 38.2% uniform
Stable aaerosol solution.The suspension prepared is uniformly coated on the non-woven fabrics basement membrane with a thickness of 12 μm by coating machine
Then oven dried is crossed in face, obtaining coating layer thickness is 3 μm, the coated on both sides diaphragm that overall thickness is 18 μm.
Embodiment 6
By 4.0kg boron nitride (Dmax≤ 800nm), 0.5kg graphite oxide (O:C/=1.2, specific surface area >=120m2/ g),
0.5kgCMC, 0.5kg butadiene-styrene rubber, 8kg deionized water are added in blender and stir 12h, and being configured to solid content is 42% uniform steady
Fixed aaerosol solution.The suspension prepared is uniformly coated on the non-woven fabrics basement membrane with a thickness of 15 μm by coating machine
Then oven dried is crossed in face, obtaining coating layer thickness is 3 μm, the single side coated separator that overall thickness is 18 μm.
Embodiment 7
By 4.0kg magnesium hydroxide (Dmax≤ 1 μm), 0.5kg graphene oxide (O:C/=0.9, specific surface area >=80m2/ g),
0.5kgPVDF, 6kg poly-methyl pyrrole alkanone are added in blender and stir 18h, and being configured to solid content is 45.5% stable homogeneous
Aaerosol solution.The suspension prepared is uniformly coated on above the polypropylene basement membrane with a thickness of 30 μm by coating machine, so
Oven dried is crossed afterwards, and obtaining coating layer thickness is 10 μm, the single side coated separator that overall thickness is 40 μm.
Embodiment 8
By 4.0kg silica (Dmax≤ 20 μm), 0.5kg graphite oxide (O:C/=0.9, specific surface area >=80m2/ g),
0.5kgPVDF, 6kg poly-methyl pyrrole alkanone are added in blender and stir for 24 hours, and being configured to solid content is 45.5% stable homogeneous
Aaerosol solution.The suspension prepared is uniformly coated on above the polyethylene based film with a thickness of 30 μm by coating machine, so
Oven dried is crossed afterwards, and obtaining coating layer thickness is 10 μm, the single side coated separator that overall thickness is 40 μm.
Embodiment 9
By 4.0kg aluminium nitride (Dmax≤ 50 μm), 0.5kg fluorographite (F:C/=1.2, specific surface area >=150m2/ g),
0.5kgCMC, 0.5kg butadiene-styrene rubber, 4kg deionized water, 2kg ethyl alcohol, 2kg isopropanol are added in blender and stir 12h, configure
It is the aaerosol solution of 45.5% stable homogeneous at solid content.The suspension prepared is uniformly coated on thickness by coating machine
Above 30 μm of polypropylene-polyethylene compound substrate membranes, oven dried is then crossed, obtaining coating layer thickness is 10 μm, overall thickness 40
μm single side coated separator.
Comparative example 1
As a comparison using commercialized polypropylene screen
Comparative example 2
By 3.7kg aluminum oxide (Dmax≤500nm), 0.3kgPVDF, 6kg poly-methyl pyrrole alkanone is added in blender and stirs
Mix the aaerosol solution for being configured to that solid content is 40.0% stable homogeneous for 24 hours.The suspension prepared is uniform by coating machine
It is coated on above the polypropylene basement membrane with a thickness of 12 μm, then crosses oven dried, obtaining coating layer thickness is 4 μm, and overall thickness is 16 μ
The single side coated separator of m.
The test result of physical property see the table below:
As can be seen from the above table, the aluminum oxide diaphragm with the commercialization polypropylene screen of comparative example 1 or comparative example 2 compares,
Porosity, air permeability, imbibition rate, ionic conductivity or the peel strength of embodiment of the present invention are above two comparative examples；
The thermal contraction of embodiment of the present invention is below two comparative examples.
In embodiment 1, due to the introducing of fluorographite, aluminum nitride particle can be preferably dispersed on fluorographite lamella
Face, so that coating is more uniform, prepared aluminium nitride/fluorographite coated separator distribution of pores is more uniform, prepared
Battery performance it is more preferable.
It is recorded according to embodiment 1 and carries out electrochemical property test, the result is shown in Figure 1-Fig. 5.
Fig. 1 is the aluminium nitride/fluorographite coated separator for preparing of the embodiment of the present invention 1 in 0.1C ~ 10C under different sections
High rate performance test result figure.
Fig. 2 is that comparative example 1 is commercialized high rate performance test result figure of the polypropylene screen in 0.1C ~ 10C under different sections.
Fig. 3 is that high rate performance of the aluminum oxide coating diaphragm of the preparation of comparative example 2 in 0.1C ~ 5C under different sections is surveyed
Test result figure.
Fig. 4 is above-mentioned difference diaphragm room temperature 1C circulation figure.
Fig. 5 is aluminium nitride/fluorographite coated separator prepared by above-described embodiment 1 and three oxidations two prepared by comparative example 2
55 DEG C of 1C of aluminized coating diaphragm recycle figure.
It can be seen from the figure that opposing with the commercialization polypropylene screen of comparative example 1 or the aluminum oxide diaphragm of comparative example 2
Than the high rate performance of embodiment 1 of the present invention, 1C cycle performance and 55 DEG C of cycle performances are above two comparative examples.
The addition of aluminium nitride and fluorographite is so that the performance of prepared diaphragm is obviously improved, with the performance of battery prepared by the diaphragm
More preferably.
The bound of each raw material cited by the present invention and each raw material of the present invention, section value and technological parameter
Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.It is described above
It is the preferred embodiment of the present invention, of course, the scope of rights of the present invention cannot be limited by this, it is noted that for this
For the those of ordinary skill of technical field, without departing from the principle of the present invention, several improvement and change can also be made
Dynamic, these, which improve and change, is also considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high-performance coating diaphragm, it is characterised in that:
The following steps are included:
Step 1: coating material one, coating material two and binder are stirred evenly in a solvent, are configured to aaerosol solution；
Step 2: aaerosol solution is uniformly coated on membrane surface and drying, obtains coated separator；
Coating material one in the step 1 includes aluminium nitride, aluminum oxide, boron nitride, magnesium hydroxide, calcium hydroxide, and two
One or more of silica；
Coating material two in the step 1 includes fluorographite, graphite oxide, fluorinated graphite, fluorinated graphene, oxygen
Graphite alkene, one or more of Fluorinated graphene oxide.
2. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 1
Coating material one particle size be 1nm-5 μm.
3. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 1
Coating material two specific surface area be 0.1-1000m2/g。
4. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 1
Binder include Kynoar, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, polyacrylic acid, polypropylene is fine, phenolic resin, asphalt mixtures modified by epoxy resin
One or more of rouge.
5. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 1
Solvent include water, ethyl alcohol, isopropanol, poly-methyl pyrrole alkanone, ethylene glycol, glycerol, one or more of n-butanol.
6. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 1
Suspension solid content be 10-99%.
7. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 1
Suspension coating material one: coating material two: binder: the mass ratio of solvent be 10-90:10-90:1-10:10-90.
8. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 2
Basement membrane be polyethylene film, polypropylene screen, polyethylene and polypropylene composite film, non-woven membrane, one of cellulose membrane or several
Kind.
9. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: in the step 2
Basement membrane thickness be 5-100 μm.
10. a kind of preparation method of high-performance coating diaphragm according to claim 1, it is characterised in that: the step 2
In coating with a thickness of 1-20 μm: coating in the step 2 is single or double coating.
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| CN110911621A (en) * | 2019-10-30 | 2020-03-24 | 华中科技大学 | Multifunctional lithium-sulfur battery diaphragm, preparation method and application |
| CN111564591A (en) * | 2020-04-30 | 2020-08-21 | 北京航空航天大学 | Lithium metal battery diaphragm modified slurry and application thereof |
| CN112993486A (en) * | 2021-02-09 | 2021-06-18 | 北京理工大学 | Method for improving multiplying power and cycle life of silicon-based negative electrode battery |
| CN113321444A (en) * | 2021-07-08 | 2021-08-31 | 南方科技大学 | Fluorinated graphene heat-conducting film and preparation method and application thereof |
| CN117467319A (en) * | 2023-12-05 | 2024-01-30 | 扬宣电子(清远)有限公司 | High-heat-conductivity PCB (printed circuit board) laminated aluminum substrate and preparation method thereof |
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| CN110911621A (en) * | 2019-10-30 | 2020-03-24 | 华中科技大学 | Multifunctional lithium-sulfur battery diaphragm, preparation method and application |
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| CN111564591A (en) * | 2020-04-30 | 2020-08-21 | 北京航空航天大学 | Lithium metal battery diaphragm modified slurry and application thereof |
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| CN112993486A (en) * | 2021-02-09 | 2021-06-18 | 北京理工大学 | Method for improving multiplying power and cycle life of silicon-based negative electrode battery |
| CN113321444A (en) * | 2021-07-08 | 2021-08-31 | 南方科技大学 | Fluorinated graphene heat-conducting film and preparation method and application thereof |
| CN113321444B (en) * | 2021-07-08 | 2023-11-03 | 南方科技大学 | Fluorinated graphene heat-conducting film and preparation method and application thereof |
| CN117467319A (en) * | 2023-12-05 | 2024-01-30 | 扬宣电子(清远)有限公司 | High-heat-conductivity PCB (printed circuit board) laminated aluminum substrate and preparation method thereof |
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