CN110444714A - A kind of lithium ion battery ceramic aramid fiber coating diaphragm and preparation method thereof - Google Patents
A kind of lithium ion battery ceramic aramid fiber coating diaphragm and preparation method thereof Download PDFInfo
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- CN110444714A CN110444714A CN201810417144.5A CN201810417144A CN110444714A CN 110444714 A CN110444714 A CN 110444714A CN 201810417144 A CN201810417144 A CN 201810417144A CN 110444714 A CN110444714 A CN 110444714A
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- diaphragm
- aramid fiber
- coating
- nanoscale
- slurry
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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
- 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
-
- 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 invention discloses a kind of lithium ion battery ceramic aramid fiber coating diaphragms and preparation method thereof, comprising the following steps: S1, measures n,N-dimethylacetamide, aramid fiber, lithium chloride and nanoscale Al2O3；S2, lithium chloride is dissolved in n,N-dimethylacetamide solution, places into aramid fiber and obtains transparent slurry, then Ghana's meter level Al in the slurry2O3, stir to get stable coating slurry；S3, the first coagulating bath and the second gelation preparation；Slurry is taken out after S4, deaeration；S5, coating obtain diaphragm；S6, be placed in again after the diaphragm after coating is placed in the first coagulating bath in the second gelation impregnate obtain cured coating diaphragm；S7, drying obtain final lithium ion battery and coat diaphragm with ceramic aramid fiber.Not only there is the coating of diaphragm of the present invention 3D solid pore structure to improve the imbibition rate and wellability of diaphragm, but also the addition of inorganic ceramic particle further enhances the heat resistance of diaphragm.
Description
Technical field
The invention belongs to electrochemical fields, and in particular to a kind of lithium ion battery ceramic aramid fiber coating diaphragm and its preparation
Method.
Background technique
Lithium ion battery is widely used in 3C electronic product with its excellent performance, also succeeds in electric car field
Using.In the development of new-energy automobile, the research and development of lithium ion battery automobile become hot spot, at the same time, promote lithium-ion electric
The safety in pond is also extremely urgent.The security performance of lithium ion battery is mainly determined by diaphragm.Existing polyolefins diaphragm by
Lower in heat shrink temperature, can no longer meet safety of the battery under the extreme cases such as high fever or high current charge-discharge needs
It asks.One Main way of diaphragm development at present be simplified technique, reduce cost, increase heat resistance, improve intensity and lithium from
Electron conductivity etc..
Poly (PMIA, also known as meta-aramid) is developed early, using wide, yield is big, development is fast
High-temperature fibre kind, strand main chain is made of the phenyl ring amido bond of meta position, and there is very strong hydrogen bond network structure to make
It is special that it shows mechanical performance, thermal stability, self-extinguishment and chemical corrosion resistance outstanding etc..Based on these of meta-aramid
Excellent properties can be used as the substrate of high temp resistance lithium ion cell diaphragm and apply material.
In the prior art using aramid fiber as the lithium ion battery separator of carrier and its technology of preparation, Hebei Cangzhou jewel
The patent publication No. of diaphragm Science and Technology Ltd. provides two for CN105552284A, CN104993089A, CN104979515A
Kind contains the composite diaphragm by aramid fiber and the compound PVDF coating of aramid fiber；In addition, section's science and technology is limited in Xinxiang City, Henan Province
The patent publication No. of company for CN107768581 provide a kind of coating diaphragm being made of aramid fiber, POSS and ionic liquid and its
Preparation method.At present when preparing aramid fiber coating diaphragm, the scheme mostly used greatly is as follows, by dissolving aramid fiber in (DMAC
(NMP、DMSO)-LiCl(CaCl2, KCl)) in equal solvent, and cooperate various additives (pore creating material, adhesive, emulsifier)
Coating slurry is formed, slurry is then coated on to the side or two sides of micropore polyolefin barrier diaphragm, then cross MJPZ and is gone
Except additive, finally drying obtains coating diaphragm.Slurry constituent is complicated in these schemes, price is also higher, preparation process
Complexity, and simple water process of crossing is difficult to remove the impurity components such as additive (pore creating material, adhesive, emulsifier) completely,
Influence diaphragm quality.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of ceramic aramid fiber coating diaphragm of lithium ion battery and its
Preparation method.
In order to achieve the above object, technical scheme is as follows:
The present invention provides a kind of ceramic aramid fiber coating diaphragm of lithium ion battery, according to the raw material system of following proportion by weight
It is standby to form:
DMAC N,N' dimethyl acetamide 94%-97%；
Lithium chloride 1%-2.5%；
Aramid fiber 1%-4%；
Al2O30-2%.
The present invention also provides a kind of lithium ion battery preparation methods of ceramic aramid fiber coating diaphragm, comprising the following steps:
S1, DMAC N,N' dimethyl acetamide, aramid fiber, lithium chloride and nanoscale Al are measured2O3；
S2, lithium chloride is dissolved in n,N-dimethylacetamide solution under the conditions of 60-100 DEG C, places into aramid fiber,
Transparent slurry is obtained after 6-8 hours, and nanoscale Al is then added in the slurry2O3, stir 0.5-1 hours and obtain stable painting
Cover slurry；
S3, the first coagulating bath preparation: DMAC N,N' dimethyl acetamide and pure water are uniformly mixed and obtain the first coagulating bath；
The preparation of the second gelation: pure water；
S4, prepared slurry is put into deaeration machine, takes out slurry after the bubble in slurry has all taken off；
S5, scraper height is adjusted, slurry is poured on coating machine, the diaphragm after being coated with；
S6, be placed in again after the diaphragm after coating is placed in the first coagulating bath in the second gelation impregnate obtain cured painting
Cover diaphragm；
S7, the diaphragm after solidification is placed in baking oven, drying obtains final lithium ion battery and coats diaphragm with ceramic aramid fiber.
As a preferred option, nanoscale Al in step S12O3First part of nanoscale Al is weighed respectively2O3, second part receive
Meter level Al2O3With third part nanoscale Al2O3, first part of nanoscale Al2O3, second part of nanoscale Al2O3With third part nanoscale
Al2O3Weight be incremental；First part of nanoscale Al is sequentially added in step S2 in the slurry2O3, second part of nanoscale Al2O3
With third part nanoscale Al2O3。
As a preferred option, the coating speed in step S5 is 5-10m/s.
As a preferred option, the diaphragm after coating in step S6 is placed in the first coagulating bath to be placed in again after 5-10 minutes
It is impregnated 5-10 minutes in the second gelation.
As a preferred option, the temperature of baking oven is 60-100 DEG C in step S7, and drying time is 0.5-1 hours.
The invention has the following advantages: the present invention is molten with DMAC N,N' dimethyl acetamide (DMAC)-lithium chloride (LiCl)
Liquid is that solvent dissolves aramid fiber, and aramid fiber is as one of coating material, nanometer Al2O3 particle is as another compound
Coating material.Using DMAC/H2The double solvents of O is as one of coagulating bath.The coating of diaphragm not only has 3D solid hole knot
Structure improves the imbibition rate and wellability of diaphragm, and the addition of inorganic ceramic particle further enhances the heat resistance of diaphragm.
Detailed description of the invention
Fig. 1 is the trend chart using coating paste viscosity prepared by the present invention
Fig. 2 is to use coating surface surface sweeping electron microscopic picture prepared by the present invention.
Fig. 3 is the change curve of the air permeability of the diaphragm prepared using this discovery.
Fig. 4 is the change curve of the porosity of the diaphragm prepared using this discovery.
Fig. 5 is the imbibition rate change curve of diaphragm prepared by the present invention.
Fig. 6 is the percent thermal shrinkage change curve after being heated 1h in the environment of 150 DEG C using diaphragm prepared by the present invention.
Fig. 7 is using diaphragm prepared by the present invention in Li2CoO2/ Li battery O.2C the cycle performance figure under multiplying power.
Specific embodiment
The following detailed description of the preferred embodiment of the present invention.
Embodiment 1
In order to reach the purpose of the present invention, a kind of lithium ion battery use is provided in one of embodiment of the invention
Ceramic aramid fiber coats diaphragm, is prepared according to the raw material of following proportion by weight:
DMAC N,N' dimethyl acetamide 97% (450g)；
Lithium chloride 2.15% (10g)；
Aramid fiber 1313 1.08% (5g)；
Al2O30% (0g).
Embodiment 2
DMAC N,N' dimethyl acetamide 95.44% (450g)；
Lithium chloride 1.91% (9g)；
Aramid fiber 1313 2.12% (10g)；
Al2O30.53% (g2.5).
Embodiment 3
DMAC N,N' dimethyl acetamide 94% (450g)；
Lithium chloride 1.67% (8g)；
Aramid fiber 1313 3.14% (15g)；
Al2O31% (5g).
Embodiment 4
DMAC N,N' dimethyl acetamide 92.4% (450g)；
Lithium chloride 1.44% (7g)；
Aramid fiber 1313 4% (20g)；
Al2O32% (10g).
In order to further optimize implementation result of the invention, the present invention also provides a kind of ceramic aramid fibers of lithium ion battery
Coat the preparation method of diaphragm, comprising the following steps:
S1, DMAC N,N' dimethyl acetamide, aramid fiber 1313, lithium chloride and nanoscale Al are measured2O3；
S2, lithium chloride is dissolved in n,N-dimethylacetamide solution under the conditions of 60-100 DEG C, places into aramid fiber 1313
Fiber obtains transparent slurry after 6-8 hours, nanoscale Al is then added in the slurry2O3, stirring obtains steady for 0.5-1 hours
Fixed coating slurry；
S3, the first coagulating bath preparation: DMAC N,N' dimethyl acetamide and pure water are uniformly mixed and obtain the first coagulating bath；
The preparation of the second gelation: pure water；
S4, prepared slurry is put into deaeration machine, takes out slurry after the bubble in slurry has all taken off；
S5, scraper height is adjusted, slurry is poured on coating machine, the diaphragm after being coated with；
S6, be placed in again after the diaphragm after coating is placed in the first coagulating bath in the second gelation impregnate obtain cured painting
Cover diaphragm；
S7, the diaphragm after solidification is placed in baking oven, drying obtains final lithium ion battery and coats diaphragm with ceramic aramid fiber.
In order to further optimize implementation result of the invention, nanoscale Al in step S12O3First part is weighed respectively to receive
Meter level Al2O3, second part of nanoscale Al2O3With third part nanoscale Al2O3, first part of nanoscale Al2O3, second part of nanoscale
Al2O3With third part nanoscale Al2O3Weight be incremental；First part of nanoscale is sequentially added in step S2 in the slurry
Al2O3, second part of nanoscale Al2O3With third part nanoscale Al2O3。
In order to further optimize implementation result of the invention, the coating speed in step S5 is 5-10m/s.
In order to further optimize implementation result of the invention, the diaphragm after coating in step S6 is placed in the first coagulating bath
It is placed in the second gelation and impregnates 5-10 minutes again after 5-10 minutes.
In order to further optimize implementation result of the invention, the temperature of baking oven is 60-100 DEG C in step S7, this implementation
Optional 60 DEG C, 80 DEG C or 100 DEG C of mode, drying time is 0.5-1 hours, optional 0.5 hour, 0.8 hour of present embodiment or
1 hour.
Fig. 1 is the trend chart using coating paste viscosity prepared by the present invention, it can be seen that 2% or less oxygen is being added
When changing aluminium, slurry viscosity increases as alumina content increases, and aluminium oxide can disperse well in the slurry；Content is more than
After 2%, viscosity tends towards stability, at this time the Al in slurry2O3Sedimentation is had begun, viscosity is caused to be basically unchanged.Illustrate to aoxidize
Aluminium content 2% and it is following when, aramid fiber/Al2O3The phenomenon that slurry is more stable, is not in sedimentation.
Fig. 2 is to use coating surface surface sweeping electron microscopic picture prepared by the present invention, and coating shows 3D solid pore structure,
Nanometer Al2O3Particle is more uniformly adhered on aramid fiber 1313, forms what nanofiber was cross-linked with each other with nano particle
Structure.This is beneficial to the imbibition rate and porosity that promote diaphragm.
Fig. 3 and 4 is the air permeability of the diaphragm prepared using this discovery and the change curve of porosity, compared to common
PE diaphragm, although the introducing of coating reduces the air permeability and porosity of diaphragm, with Al2O3Addition, diaphragm it is saturating
Manner is gradually promoted with porosity, under 2% alumina content, air permeability already close to in common PE diaphragm.
Fig. 5 is the imbibition rate change curve using diaphragm prepared by the present invention.The introducing of coating, significantly increase every
The imbibition rate of film, under 2% alumina content, imbibition rate is 3~4 times of common PE diaphragm already close to 350%.
Fig. 6 is the percent thermal shrinkage change curve after being heated 1h in the environment of 150 DEG C using diaphragm prepared by the present invention,
The introducing of coating is greatly improved the heat resistance of diaphragm, this will increase safety in utilization of the battery under extreme heated environment.
Fig. 7 is using diaphragm prepared by the present invention in Li2CoO2/ Li battery O.2C the cycle performance figure under multiplying power, coating
Introducing significantly increase the cyclical stability of battery.
The present invention dissolves aramid fiber, virtue by solvent of n,N-dimethylacetamide (DMAC)-lithium chloride (LiCl) solution
Synthetic fibre fiber is as one of coating material, nanometer Al2O3Particle is as another compound coating material.Using DMAC/H2O's answers
Bonding solvent is as one of coagulating bath.Not only there is the coating of diaphragm 3D solid pore structure to improve the imbibition rate and leaching of diaphragm
Lubricant nature, and the addition of inorganic ceramic particle further enhances the heat resistance of diaphragm.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to this hair
Bright protection scope.
Claims (6)
1. a kind of lithium ion battery coats diaphragm with ceramic aramid fiber, which is characterized in that according to the raw material system of following proportion by weight
It is standby to form:
2. a kind of lithium ion battery as described in claim 1 preparation method of ceramic aramid fiber coating diaphragm, which is characterized in that
The following steps are included:
S1, n,N-dimethylacetamide, aramid fiber, lithium chloride and nanoscale Al are measured2O3；
S2, lithium chloride is dissolved in n,N-dimethylacetamide solution under the conditions of 60-100 DEG C, places into aramid fiber, 6-8
Transparent slurry is obtained after hour, nanoscale Al is then added in the slurry2O3, stir 0.5-1 hours and obtain stable coating materials
Material；
S3, the first coagulating bath preparation: n,N-dimethylacetamide and pure water are uniformly mixed and obtain the first coagulating bath；Second is solidifying
Admittedly the preparation bathed: pure water；
S4, prepared slurry is put into deaeration machine, takes out slurry after the bubble in slurry has all taken off；
S5, scraper height is adjusted, slurry is poured on coating machine, the diaphragm after being coated with；
S6, be placed in again after the diaphragm after coating is placed in the first coagulating bath in the second gelation impregnate obtain it is cured coating every
Film；
S7, the diaphragm after solidification is placed in baking oven, drying obtains final lithium ion battery and coats diaphragm with ceramic aramid fiber.
3. the lithium ion battery according to claim 2 preparation method of ceramic aramid fiber coating diaphragm, which is characterized in that step
Nanoscale Al in rapid S12O3First part of nanoscale Al is weighed respectively2O3, second part of nanoscale Al2O3With third part nanoscale Al2O3,
First part of nanoscale Al2O3, second part of nanoscale Al2O3With third part nanoscale Al2O3Weight be incremental；It is being starched in step S2
First part of nanoscale Al is sequentially added in material2O3, second part of nanoscale Al2O3With third part nanoscale Al2O3。
4. the lithium ion battery according to claim 2 preparation method of ceramic aramid fiber coating diaphragm, which is characterized in that step
Coating speed in rapid S5 is 5-10m/s.
5. the lithium ion battery according to claim 2 preparation method of ceramic aramid fiber coating diaphragm, which is characterized in that step
Diaphragm after coating in rapid S6, which is placed in the first coagulating bath after 5-10 minutes to be placed in again in the second gelation, to be impregnated 5-10 minutes.
6. the lithium ion battery according to claim 2 preparation method of ceramic aramid fiber coating diaphragm, which is characterized in that step
The temperature of baking oven is 60-100 DEG C in rapid S7, and drying time is 0.5-1 hours.
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| CN201810417144.5A CN110444714A (en) | 2018-05-03 | 2018-05-03 | A kind of lithium ion battery ceramic aramid fiber coating diaphragm and preparation method thereof |
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| CN201810417144.5A CN110444714A (en) | 2018-05-03 | 2018-05-03 | A kind of lithium ion battery ceramic aramid fiber coating diaphragm and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111668426A (en) * | 2020-06-22 | 2020-09-15 | 欣旺达电动汽车电池有限公司 | Diaphragm and preparation method thereof, lithium ion battery and electric automobile |
| CN112490581A (en) * | 2020-10-28 | 2021-03-12 | 河北金力新能源科技股份有限公司 | Meta-aramid fiber and oil PDVF composite coating diaphragm and preparation method thereof |
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| CN103474609A (en) * | 2013-09-27 | 2013-12-25 | 中材科技股份有限公司 | Overlapped coating composite lithium battery diaphragm and preparation method thereof |
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| CN112490581A (en) * | 2020-10-28 | 2021-03-12 | 河北金力新能源科技股份有限公司 | Meta-aramid fiber and oil PDVF composite coating diaphragm and preparation method thereof |
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