CN109167008A - Lithium battery low moisture ceramic diaphragm preparation method, aqueous slurry and ceramic diaphragm - Google Patents
Lithium battery low moisture ceramic diaphragm preparation method, aqueous slurry and ceramic diaphragm Download PDFInfo
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- CN109167008A CN109167008A CN201811032128.0A CN201811032128A CN109167008A CN 109167008 A CN109167008 A CN 109167008A CN 201811032128 A CN201811032128 A CN 201811032128A CN 109167008 A CN109167008 A CN 109167008A
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- powder
- aqueous slurry
- preparation
- ceramic diaphragm
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
-
- 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 belongs to lithium battery diaphragm preparation technical fields, and in particular to a kind of lithium battery preparation method of low moisture ceramic diaphragm, aqueous slurry and low moisture ceramic diaphragm.Wherein this lithium battery includes the following steps: step S1 with the preparation method of low moisture ceramic diaphragm, prepares ceramers powder；Ceramers powder is prepared into aqueous slurry by step S2；And step S3, aqueous slurry is coated on lithium ion battery separator surface, and carry out baking and water removal is gone to form ceramic diaphragm, to reduce the water imbibition of ceramic diaphragm.
Description
Technical field
The present invention relates to lithium battery diaphragm preparation technical fields, and in particular to a kind of lithium battery low moisture ceramic diaphragm
Preparation method, aqueous slurry and low moisture ceramic diaphragm.
Background technique
For lithium ion battery due to big with energy density, operating temperature range is wide, and steady storage time of discharging is long, storage and
Many electronic technology fields such as it is long a little that the time is recycled, therefore is widely used in computer, automobile and mobile phone at present.And
The composition of lithium ion battery mainly includes positive and negative pole material, electrolyte and the big critical material of diaphragm four.
Currently, the polyolefine materials such as polypropylene (PP), polyethylene (PE) are the major matrix materials of lithium ion battery separator,
But no matter polypropylene (PP), polyethylene (PE) or other thermoplastic macromolecule materials, can be due to fusing when close to fusing point
Contraction distortion brings potential risk to the safety of lithium ion battery.To meet the following high power power category lithium ion battery
Demand, lithium ion battery separator need to consider further promoted thermal stable temperature limitation range.In existing basis material system
On the basis of, it is the important directions of current diaphragm material research and development, but ceramic diaphragm is general by way of coated ceramic coating
Using nanoscale aluminum oxide particle, specific surface area easily absorbs water in 4-8m2/g；Furthermore due to ceramic powders and bonding
The consistency problem of agent easily causes ceramics to fall situations such as dividing, and seriously affects the electrical property and security performance of lithium battery.
Summary of the invention
The object of the present invention is to provide a kind of lithium battery preparation method of low moisture ceramic diaphragm, aqueous slurry and low water
Divide ceramic diaphragm, after ceramers powder is prepared into aqueous slurry, is coated on lithium ion battery separator surface and forms pottery
Porcelain diaphragm to reduce the water imbibition of ceramic diaphragm, while increasing the compatibility between ceramic powders and binder, increases bonding
Power.
In order to solve the above-mentioned technical problems, the present invention provides a kind of lithium battery preparation methods of low moisture ceramic diaphragm
Include the following steps: step S1, prepares ceramers powder；Ceramers powder is prepared into aqueous by step S2
Slurry；And step S3, aqueous slurry is coated on lithium ion battery separator surface, and carry out baking and go to remove water.Specifically, institute
The coating method for stating the aqueous slurry in step S3 is such as, but not limited to: micro- gravure roller coating or spraying；And it is applied in aqueous slurry
It needs to grind by sand mill before cloth, milling time 1~4 hour, 500~1200RPM of grinding rate.In the step S3
Baking temperature is 40~80 DEG C, and baking time is 1~3min.
Further, the method for ceramers powder being prepared in the step S1 includes the following steps: step S11, right
Ceramic powder vacuumizes water removal；The ceramic powder vacuumized after removing water is immersed in polymer monomer solvent by step S12；With
And step S13, ceramic powder, which is taken out, after being sufficiently impregnated is dried in vacuo.
Specifically, carrying out within 12-48 hours vacuumizing water removal first by 80~100 DEG C of ceramic powder heating temperature；It then will pottery
Ceramic powder is impregnated into polymer monomer solvent 1-7 days, is sufficiently impregnated it；Followed by after taking-up at 60~100 DEG C, reaction
0.5~2 hour, make to adhere to upper organic oligomer in ceramic powder hole；It is finally dried in vacuo, ceramers powder is made
Material.
Optionally, the ceramic powder in step S11 includes but is not limited to: aluminum oxide, magnesium hydroxide, magnesia, sulphur
One or more of sour barium, boehmite, silica, titanium dioxide.
Further, the polymer monomer solvent includes: the polymer monomer and 0.1~0.5 weight of 80~120 parts by weight
The initiator of part.Optionally, the polymer monomer includes but is not limited to: acrylic ester monomer (such as propyl acrylate, methyl
Methyl acrylate, methacrylic acid etc.), butadiene, one of vinyl monomer (such as styrene, vinyl acetate) or several
Kind.Optionally, the initiator includes but is not limited to: peroxide initiator (such as benzoyl peroxide, cumyl peroxide
Deng), azo-initiator (such as azo-bis-isobutyl cyanide), redox initiator (such as hydrogen peroxide/sulfuric acid ferrous iron system)
One or more of.
Further, the aqueous slurry includes the substance of following parts by weight: ceramers powder: 20~50 parts；
Deionized water: 40~80 parts；Binder: 1~20 part；And dispersing agent: 0.1~5 part.
Optionally, the binder includes but is not limited to: polyacrylate binder, polyvinyl alcohol adhesive, poly-vinegar
One or more of vinyl acetate binder etc..Wherein, the solid content of all kinds of binders is 40~50%, preferably 45%.
Optionally, the dispersing agent includes but is not limited to: hydroxyethyl cellulose, sodium carboxymethylcellulose, ammonium polyacrylate,
One or more of Sodium Polyacrylate, sodium alginate etc..
In conclusion the preparation method of the lithium battery of the application low moisture ceramic diaphragm by by ceramic powder with polymerize
Object monomer reacts under certain condition, so that ceramic powder surface is covered one layer of organic oligomer, and be prepared into after the drying aqueous
Slurry is coated on membrane surface and obtains ceramic diaphragm, not only ceramic diaphragm water absorbing properties can be made low, in production, transports, makes
Not adsorption moisture, impurity during, and the two can be increased by the compatibility between ceramic powder and binder
Between cohesive force, improve adhesion strength, be not easy to lose powder, to ensure that the electrical property and security performance of lithium battery.
Another aspect, the present invention also provides a kind of aqueous slurry, the substance including following parts by weight: organically-modified pottery
Ceramic powder: 20~50 parts；Deionized water: 40~80 parts；Binder: 1~20 part；And dispersing agent: 0.1~5 part.
Specific ingredient about ceramers powder, binder and dispersing agent is referring to foregoing lithium battery with low
The substance of corresponding parts by weight in the preparation method of moisture ceramic diaphragm, details are not described herein.
On the other hand, the present invention also provides a kind of ceramic diaphragms, comprising: aqueous slurry；The aqueous slurry is suitable for applying
Cloth forms the ceramic diaphragm on lithium ion battery separator surface, and after baking water removal.
Optionally, the aqueous slurry includes the substance of following parts by weight: ceramers powder: 20~50 parts；
Deionized water: 40~80 parts；Binder: 1~20 part；And dispersing agent: 0.1~5 part.Wherein, ceramers powder, viscous
The specific ingredient of knot agent and dispersing agent is accordingly weighed referring to foregoing lithium battery in the preparation method of low moisture ceramic diaphragm
Measure the substance of number.
Coating method and baking removal process about aqueous slurry is referring to foregoing lithium battery low moisture ceramics
Related content in the preparation method of diaphragm, details are not described herein.
The invention has the advantages that the preparation method of lithium battery low moisture ceramic diaphragm of the invention is by will be organic
After modified ceramic powder is prepared into aqueous slurry, it is coated on lithium ion battery separator surface and forms ceramic diaphragm, there is water imbibition
Can be low, adsorption moisture, impurity, advantage not easily to fall off not ensure that the electrical property of lithium battery in production, transport and use process
Energy and security performance.
Specific embodiment
In this application, the polymer monomer solvent and aqueous slurry in the preparation method of lithium battery low moisture ceramic diaphragm
The composition content of material can be there are many embodiment, and (each component is by weight in Tables 1 and 2 as shown in Table 1 and Table 2 respectively
Number proportion).But due to needing to compare detection test with embodiment 6 (ceramic diaphragm directly prepared using ceramic powder),
The composition content of polymer monomer solvent and aqueous slurry needs to keep close or identical, to guarantee the reliability of testing result,
Some embodiments are now only enumerated, as shown in embodiment 1-5.
The composition content of 1 polymer monomer solvent of table
The composition content of 2 aqueous slurry of table
Embodiment 1
6kg aluminum oxide powder is toasted for 24 hours at 80 DEG C, is then added to the methyl methacrylate (MMA) of 10kg
In monomer, then 30g benzoyl peroxide (BPO) is added, is impregnated 4 days under room temperature, normal pressure, then taken out and in 80 DEG C of reaction 1h,
Finally for 24 hours, ceramers powder is made in 40 DEG C of dryings in vacuum drying oven.By above-mentioned ceramers powder, go from
Sub- water, polymethyl methacrylate binder, sodium carboxymethylcellulose, Sodium Polyacrylate are stirred by 30:60:5:0.5:0.5 ingredient
It mixes, the sand mill sand milling time is 1 hour, revolving speed 1000RPM, obtains aqueous slurry.Above-mentioned aqueous slurry is used into dimple roller coating
Mode for cloth is coated in 14umPP diaphragm one side, and 65 DEG C of baking 2min obtain the ceramic diaphragm of total thickness 16um.
Embodiment 2
6kg aluminum oxide powder is toasted for 24 hours at 80 DEG C, is then added in the propyl acrylate monomer of 10kg, then
It adds 30g azo-bis-isobutyl cyanide (AIBN), after impregnating 5 days under room temperature, normal pressure, then takes out and in 70 DEG C of reaction 1.5h, finally
For 24 hours, ceramers powder is made in 40 DEG C of dryings in vacuum drying oven.By above-mentioned ceramers powder, deionized water,
Polymethyl methacrylate binder, sodium carboxymethylcellulose, Sodium Polyacrylate are stirred by 30:60:5.5:0.5:0.5 ingredient,
The sand mill sand milling time is 1.5 hours, revolving speed 800RPM, obtains aqueous slurry.Above-mentioned aqueous slurry is used into micro- gravure roller coating
Mode is coated in 14umPP diaphragm one side, and 70 DEG C of baking 2min obtain the ceramic diaphragm of total thickness 16um.
Embodiment 3
6kg aluminum oxide powder is toasted for 24 hours at 80 DEG C, is then added in the styrene monomer of 10kg, then add
40g azo-bis-isobutyl cyanide (AIBN) impregnates 5 days under room temperature, normal pressure, then takes out and in 80 DEG C of reaction 1.5h, finally in vacuum
For 24 hours, ceramers powder is made in 40 DEG C of dryings in baking oven.By above-mentioned ceramers powder, deionized water, phenylpropyl alcohol cream
Liquid binder, sodium carboxymethylcellulose, ammonium polyacrylate are stirred by 36:60:4.5:0.5:0.5 ingredient, and the time is sanded in sand mill
It is 2 hours, revolving speed 600RPM, obtains aqueous slurry.Above-mentioned aqueous slurry is coated in 14umPP using dimple roller coating mode for cloth
Diaphragm one side, 65 DEG C of baking 2min obtain the ceramic diaphragm of total thickness 16um.
Embodiment 4
6kg boehmite powder is toasted for 24 hours at 80 DEG C, is then added to the mix monomer (methyl methacrylate of 10kg
5kg, butyl acrylate 5kg) in, then 40g benzoyl peroxide (BPO) is added, it impregnates 4 days, is then taken out simultaneously under room temperature, normal pressure
In 80 DEG C of reaction 1h, finally for 24 hours, ceramers powder is made in 40 DEG C of dryings in vacuum drying oven.By ceramers
Powder, deionized water, polyacrylate binder, sodium carboxymethylcellulose, ammonium polyacrylate are matched by 36:60:4.5:0.5:0.5
Material stirring, sand mill sand milling time are 1 hour, revolving speed 1000RPM, obtain aqueous slurry.Above-mentioned aqueous slurry is used into dimple
Roller coating mode for cloth is coated in 14umPP diaphragm one side, and 65 DEG C of baking 2min obtain the ceramic diaphragm of total thickness 16um.
Embodiment 5
6kg aluminum oxide powder is toasted for 24 hours at 80 DEG C, is then added to the vinyl acetate monomer of 10kg, then add
50g benzoyl peroxide (BPO) impregnates 5 days under room temperature, normal pressure, then takes out and in 80 DEG C of reaction 1h, finally in vacuum drying oven
In 40 DEG C of dryings for 24 hours, ceramers powder is made.Ceramers powder, deionized water, poly-vinegar acid is made by above-mentioned
Ethylene binder, sodium carboxymethylcellulose, ammonium polyacrylate are stirred by 35:60:5:0.5:0.5 ingredient, and the time is sanded in sand mill
It is 1 hour, revolving speed 1000RPM, obtains aqueous slurry.Above-mentioned aqueous slurry is coated in 14umPP using dimple roller coating mode for cloth
Diaphragm one side, 65 DEG C of baking 2min obtain the ceramic diaphragm of total thickness 16um.
Comparative example 6
By aluminum oxide powder 80 DEG C baking for 24 hours, then with deionized water, polyacrylate binder, carboxymethyl
Sodium cellulosate, Sodium Polyacrylate are stirred by 35:60:5:1:1 ingredient, and the sand mill sand milling time is 1 hour, and revolving speed 1000RPM is obtained
Obtain aqueous slurry.Above-mentioned aqueous slurry is coated in 14umPP diaphragm one side, 65 DEG C of baking 2min using dimple roller coating mode for cloth
Obtain the ceramic diaphragm of total thickness 16um.
Contrasting detection test:
Embodiment 1-6 ceramic diaphragm obtained is passed through karl Fischer analyzer at 130 DEG C respectively to detect, respectively
The correlation data of the ceramic diaphragm of embodiment is as shown in table 3, wherein after the correlation data includes: moisture content and coats
Gurley value and the thermal contraction performance that the mechanical direction (longitudinal direction) after 1h is toasted at 130 DEG C.
The correlation data of the ceramic diaphragm of each embodiment of table 3
| Serial number | Water content/ppm | Air permeability/s | It is heat-shrinked |
| Embodiment 1 | 542 | 282 | 1.7 |
| Embodiment 2 | 482 | 274 | 2 |
| Embodiment 3 | 397 | 281 | 1.7 |
| Embodiment 4 | 470 | 279 | 1.5 |
| Embodiment 5 | 580 | 267 | 2 |
| Embodiment 6 | 2870 | 245 | 2 |
3 are shown in Table, the ceramic diaphragm of embodiment 1-5 has been all made of ceramers powder described herein as preparation
Material；And the embodiment as a comparison of embodiment 6, ceramic material is directlyed adopt, does not use this ceramers powder.Detection pair
As follows than result: moisture content significantly reduces in the ceramic diaphragm of embodiment 1-5, and permeability slightly increases, thermal contraction performance
There is no significant changes.Therefore, the ceramic diaphragm that prepared by the preparation method of the lithium battery of the application low moisture ceramic diaphragm is not only
With the advantage that traditional ceramics diaphragm is not easily to fall off, also reduce water imbibition, improve gas permeability, make lithium battery electrical property and
Security performance is preferably guaranteed.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of lithium battery preparation method of low moisture ceramic diaphragm characterized by comprising
Prepare ceramers powder；
Ceramers powder is prepared into aqueous slurry；And
Aqueous slurry is coated on lithium ion battery separator surface, and is toasted.
2. preparation method according to claim 1, which is characterized in that
The method for preparing ceramers powder includes:
Water removal is vacuumized to ceramic powder；
The ceramic powder vacuumized after removing water is immersed in polymer monomer solvent；And
Ceramic powder is taken out after being sufficiently impregnated to be dried in vacuo.
3. preparation method according to claim 2, which is characterized in that
The polymer monomer solvent includes: the polymer monomer of 80 ~ 120 parts by weight and the initiator of 0.1 ~ 5 parts by weight.
4. preparation method according to claim 3, which is characterized in that
The polymer monomer is one or more of acrylic ester monomer, butadiene, vinyl monomer.
5. preparation method according to claim 3, which is characterized in that
The initiator is one or more of peroxide initiator, azo-initiator, redox initiator.
6. preparation method according to claim 1, which is characterized in that
The aqueous slurry includes the substance of following parts by weight:
Ceramers powder: 20~50 parts；
Deionized water: 40~80 parts；
Binder: 1~20 part；And
Dispersing agent: 0.1~5 part.
7. preparation method according to claim 6, which is characterized in that
The binder is one of polyacrylate binder, polyvinyl alcohol adhesive, polyvinyl acetate binder
Or it is several.
8. preparation method according to claim 6, which is characterized in that
The dispersing agent is hydroxyethyl cellulose, in sodium carboxymethylcellulose, ammonium polyacrylate, Sodium Polyacrylate, sodium alginate
One or more.
9. a kind of aqueous slurry, which is characterized in that the substance including following parts by weight:
Ceramers powder: 20~50 parts；
Deionized water: 40~80 parts；
Binder: 1~20 part；And
Dispersing agent: 0.1~5 part.
10. a kind of ceramic diaphragm characterized by comprising
Aqueous slurry；
The aqueous slurry is suitable for being coated on lithium ion battery separator surface, and forms the ceramic diaphragm after baking water removal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811032128.0A CN109167008B (en) | 2018-09-05 | 2018-09-05 | Preparation method of low-moisture ceramic diaphragm for lithium battery, aqueous slurry and ceramic diaphragm |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811032128.0A CN109167008B (en) | 2018-09-05 | 2018-09-05 | Preparation method of low-moisture ceramic diaphragm for lithium battery, aqueous slurry and ceramic diaphragm |
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| CN109167008B CN109167008B (en) | 2021-05-11 |
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| CN110212139A (en) * | 2019-06-26 | 2019-09-06 | 江苏厚生新能源科技有限公司 | Environment-friendly type Ultralow Water ceramic coating membrane and preparation method, solution and slurry |
| CN110408075A (en) * | 2019-08-28 | 2019-11-05 | 广东工业大学 | A kind of composite isolated film and preparation method thereof |
| CN111416088A (en) * | 2020-03-26 | 2020-07-14 | 江苏厚生新能源科技有限公司 | Preparation method of lithium battery ceramic diaphragm |
| CN112142995A (en) * | 2020-08-24 | 2020-12-29 | 深圳市德立新材料科技有限公司 | Organic-inorganic composite grape particle structure material, slurry, diaphragm and preparation method |
| CN113214766A (en) * | 2021-03-08 | 2021-08-06 | 新乡市中科科技有限公司 | High-temperature-resistant binder, preparation method thereof and high-temperature-resistant coating film prepared from binder |
| CN114050375A (en) * | 2021-11-15 | 2022-02-15 | 江苏厚生新能源科技有限公司 | Preparation method of modified aluminum oxide and PMMA mixed slurry coating diaphragm |
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| CN112142995A (en) * | 2020-08-24 | 2020-12-29 | 深圳市德立新材料科技有限公司 | Organic-inorganic composite grape particle structure material, slurry, diaphragm and preparation method |
| CN113214766A (en) * | 2021-03-08 | 2021-08-06 | 新乡市中科科技有限公司 | High-temperature-resistant binder, preparation method thereof and high-temperature-resistant coating film prepared from binder |
| CN114050375A (en) * | 2021-11-15 | 2022-02-15 | 江苏厚生新能源科技有限公司 | Preparation method of modified aluminum oxide and PMMA mixed slurry coating diaphragm |
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