CN113097651A - Lithium ion battery diaphragm - Google Patents
Lithium ion battery diaphragm Download PDFInfo
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- CN113097651A CN113097651A CN202110332623.9A CN202110332623A CN113097651A CN 113097651 A CN113097651 A CN 113097651A CN 202110332623 A CN202110332623 A CN 202110332623A CN 113097651 A CN113097651 A CN 113097651A
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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
- 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
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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
The lithium ion battery diaphragm is characterized by comprising at least one lithium battery diaphragm, wherein the lithium battery diaphragm comprises a substrate layer of a base film subjected to surface modification and at least one film layer dispersed with nano particles.
Description
Technical Field
The invention relates to a lithium ion battery diaphragm.
Background
The application is an application number 201810696513.9, is named as a lithium battery diaphragm and a divisional application of the lithium battery diaphragm, and the disclosure content of the main case is fully introduced.
In the construction of lithium batteries, the separator is one of the key internal components. The performance of the diaphragm determines the interface structure, internal resistance and the like of the battery, directly influences the capacity, circulation, safety performance and other characteristics of the battery, and the diaphragm with excellent performance plays an important role in improving the comprehensive performance of the battery. The separator has a main function of separating the positive electrode and the negative electrode of the battery to prevent short circuit due to contact between the two electrodes, and also has a function of allowing electrolyte ions to pass therethrough. The separator material is non-conductive, and the physical and chemical properties of the separator have a great influence on the performance of the battery. The battery is different in kind and the separator used is different. In the lithium battery system, since the electrolyte is an organic solvent system, a separator material resistant to an organic solvent is required, and a polyolefin porous film having a high strength and a thin film is generally used.
In recent years, the polymer electrolyte has been commercialized for use in a lithium ion battery, and the polymer electrolyte serves as a channel for ion migration and a separator between positive and negative electrode materials in the lithium ion battery. The polymer electrolyte can be classified into a solid polymer electrolyte and a gel polymer electrolyte, and as a practical polymer electrolyte separator, the following requirements must be satisfied: firstly, the ionic conductivity is high so as to reduce the internal resistance of the battery; the transfer coefficient of the lithium ion is basically unchanged to eliminate concentration polarization; negligible electronic conductivity to ensure effective isolation between electrodes; the electrode material has high chemical and electrochemical stability; low cost, proper chemical composition and environment friendship.
The basic properties such as gas property, porosity, pore size, thickness and the like cannot be well controlled within a certain range, so that the method cannot be effectively applied and cannot meet the requirements of the high-end field of the lithium battery.
Disclosure of Invention
The invention aims to provide a lithium ion battery diaphragm, which is characterized by comprising at least one layer of lithium battery diaphragm,
the lithium battery diaphragm comprises a substrate layer of a base film subjected to surface modification and at least one film layer dispersed with nano particles;
the lithium battery diaphragm is prepared by the following method:
mixing N-butyl alcohol, N, N-dimethylformamide, nano-silica, polyvinylidene fluoride and carbon tetrachloride, controlling the pH value to be 5-7, stirring and heating to 50-70 ℃, wherein the stirring speed is 1500r/min and the stirring time is 1-6h to obtain mixed slurry;
step two, modifying the surface of the base film
Placing the base film in a 2-methoxy-4-methylphenol aqueous solution, soaking for 30-120min, taking out, washing for 3-6 times by using deionized water, and then placing in a dryer for drying to obtain a surface modified film;
step three, coating
Placing the base film with the modified surface in the second step on a coating machine, and passing the mixed slurry in the first step through an electrostatic spraying device at a rate of 2-4mL/dm2Uniformly spraying the modified film on the lithium battery diaphragm, transferring the film into a drying oven, and drying the film for 5-6 hours at the temperature of 70-80 ℃ to obtain the lithium battery diaphragm;
the nano-silica in the step one is mesoporous silica nano-particles subjected to surface modification, and is prepared by the following method:
step A, preparation of mesoporous silica nanoparticles
(1) Placing hexadecyl trimethyl ammonium bromide into deionized water, mechanically stirring for 15-30min, adding isopropanol and 25% ammonia water after stirring, stirring for 30min at 50-80 ℃, adding tetraethyl orthosilicate and a first composition, heating to 60-100 ℃ at the heating rate of 10-15 ℃/min, stirring for 2-4h, stopping stirring, standing for 15-30h to obtain layered solution, cooling to room temperature, centrifuging by adopting a centrifuge, respectively cleaning precipitates by adopting ethanol and deionized water for 3-6 times, and then drying in vacuum to obtain mesoporous silica nanoparticles;
the mass ratio of the hexadecyl trimethyl ammonium bromide to the deionized water to the first composition to the isopropyl alcohol to the ammonia water to the tetraethyl orthosilicate is 1-3:50-300:10-30:5-20:3-8: 2-4; the first composition is prepared by mixing thiophene, pyrrole and N, N-dimethylformamide according to the mass ratio of 3-6:2-4: 0.5-2;
step B, surface modification of mesoporous silica nanoparticles
Placing the mesoporous silica nanoparticles prepared in the step one, nano polyaniline, ethylenediamine and methanol in a mass ratio of 5-10:6-20:1-4:30-60 in a beaker, stirring at 40-60 ℃, then performing rotary evaporation under reduced pressure to remove the solvent, washing the obtained product with diethyl ether, heating to 40-50 ℃, magnetically stirring the washed product, the first compound and dichloromethane for 30-50min, heating to 60-90 ℃, adding ammonium persulfate under the protection of nitrogen, performing stirring reaction for 10-20h, cooling to room temperature, and washing the precipitate with deionized water for 3-6 times to obtain surface-modified mesoporous silica nanoparticles;
the mass ratio of the mesoporous silica nanoparticles to the first compound to the dichloromethane to the ammonium persulfate is 3-8:6-10:1-5: 2-4;
the first compound is a polyethylene oxide-polypropylene oxide two-block polymer;
the preparation method of the polyethylene oxide-polypropylene oxide two-block polymer comprises the following steps: mixing polyethylene oxide, polypropylene oxide and stannous isooctanoate to obtain a mixture;
the mass ratio of the polyethylene oxide to the polypropylene oxide to the stannous isooctanoate is 5-10:3-9:0.5-1, nitrogen is filled into the mixture for 30min to ensure that oxygen in the mixture is removed, the mixture is transferred into a four-neck flask replaced by nitrogen to be polymerized, the mixture is stirred at the temperature of 80-120 ℃ to react for 15-20h, the reaction product is placed into deionized water with the pH value of 4.0-5.0 to be dialyzed for 1-3 days, and then ethanol is adopted to wash for 3-6 times, so that the polyethylene oxide-polypropylene oxide two-block polymer is obtained.
2. The lithium ion battery separator according to claim 1, wherein the lithium battery separator has a thickness of 8 to 30 μm.
3. The lithium ion battery separator according to claim 1, wherein the lithium battery separator has a thickness of 10 to 20 μm.
4. The lithium ion battery separator according to claim 1, wherein the porosity of the lithium battery separator is 66-83%.
5. The lithium ion battery separator according to claim 1, wherein the mass ratio of N-butanol, N, N-dimethylformamide, nano-silica, polyvinylidene fluoride and carbon tetrachloride is 30-60:10-15:1-5:4-8: 0.5-3.
6. The lithium ion battery separator according to claim 1, wherein the base film is a polyamide film.
Has the advantages that:
the nano-microporous battery diaphragm has the advantages of good safety, high tensile strength, good heat resistance and good porosity.
Detailed Description
The invention will be further illustrated with reference to the following specific examples.
A lithium battery separator is characterized in that the separator comprises a substrate layer of a base film subjected to surface modification and at least one film layer dispersed with nano particles.
The thickness of the lithium battery diaphragm is 8-30 μm.
The thickness of the lithium battery diaphragm is 10-20 μm.
The porosity of the lithium battery diaphragm is 66-83%.
The porosity of the lithium battery separator was 70%.
The porosity of the lithium battery separator was 75%.
The lithium battery diaphragm is prepared by the following method:
mixing N-butyl alcohol, N, N-dimethylformamide, nano-silica, polyvinylidene fluoride and carbon tetrachloride, controlling the pH value to be 5-7, stirring and heating to 50-70 ℃, wherein the stirring speed is 1500r/min and the stirring time is 1-6h to obtain mixed slurry;
step two, modifying the surface of the film
Placing the base film in a 2-methoxy-4-methylphenol aqueous solution, soaking for 30-120min, taking out, washing for 3-6 times by using deionized water, and then placing in a dryer for drying to obtain a surface modified film;
step three, coating
Placing the modified film on the surface of the second step on a coating machine, and passing the mixed slurry of the first step through an electrostatic spraying device at a rate of 2-4mL/dm2And uniformly spraying the modified film, transferring the film into a drying oven, and drying the film for 5-6 hours at the temperature of 70-80 ℃ to obtain the lithium battery diaphragm.
The mass ratio of the N-butanol to the N, N-dimethylformamide to the nano-silicon dioxide to the polyvinylidene fluoride to the carbon tetrachloride is 30-60:10-15:1-5:4-8: 0.5-3.
The base film is a polyamide film.
The slurry in the first step is polyvinylidene fluoride mixed liquid.
A lithium ion battery separator is characterized by comprising at least one layer of the lithium battery separator.
A composite separator for a battery, comprising at least one lithium battery separator as described above.
Use of a lithium ion battery separator as claimed in any preceding claim in a lithium ion battery separator.
The mesoporous nanoparticles in the step one of the invention are surface-modified porous nanoparticles, and are prepared by the following method:
step A, preparation of mesoporous silica nanoparticles
(1) Placing hexadecyl trimethyl ammonium bromide into deionized water, mechanically stirring for 15-30min, adding isopropanol and 25% ammonia water after stirring, stirring for 30min at 50-80 ℃, adding tetraethyl orthosilicate and a first composition, heating to 60-100 ℃ at the heating rate of 10-15 ℃/min, stirring for 2-4h, stopping stirring, standing for 15-30h to obtain layered solution, cooling to room temperature, centrifuging by adopting a centrifuge, respectively cleaning precipitates by adopting ethanol and deionized water for 3-6 times, and then drying in vacuum to obtain mesoporous silica nanoparticles;
the mass ratio of the hexadecyl trimethyl ammonium bromide to the deionized water to the first composition to the isopropyl alcohol to the ammonia water to the tetraethyl orthosilicate is 1-3:50-300:10-30:5-20:3-8: 2-4; the first composition is prepared by mixing thiophene, pyrrole and N, N-dimethylformamide according to the mass ratio of 3-6:2-4: 0.5-2;
step B, surface modification of mesoporous silica nanoparticles
Placing the mesoporous silica nanoparticles prepared in the step one, nano polyaniline, ethylenediamine and methanol in a mass ratio of 5-10:6-20:1-4:30-60 in a beaker, stirring at 40-60 ℃, then performing rotary evaporation under reduced pressure to remove the solvent, washing the obtained product with diethyl ether, heating to 40-50 ℃, magnetically stirring the washed product, the first compound and dichloromethane for 30-50min, heating to 60-90 ℃, adding ammonium persulfate under the protection of nitrogen, performing stirring reaction for 10-20h, cooling to room temperature, and washing the precipitate with deionized water for 3-6 times to obtain surface-modified mesoporous silica nanoparticles;
the mass ratio of the mesoporous silica nanoparticles to the first compound to the dichloromethane to the ammonium persulfate is 3-8:6-10:1-5: 2-4;
the first compound is a polyethylene oxide-polypropylene oxide two-block polymer;
the preparation method of the polyethylene oxide-polypropylene oxide two-block polymer comprises the following steps: mixing polyethylene oxide, polypropylene oxide and stannous isooctanoate to obtain a mixture (the mass ratio of the polyethylene oxide to the polypropylene oxide to the stannous isooctanoate is 5-10:3-9:0.5-1), filling nitrogen for 30min to ensure that oxygen in the mixture is removed, transferring the mixture into a four-neck flask replaced by nitrogen for polymerization, reacting for 15-20h at 80-120 ℃ under stirring, placing the reaction product into deionized water with the pH value of 4.0-5.0 for dialysis for 1-3 days, and then washing for 3-6 times by using ethanol to obtain the polyethylene oxide-polypropylene oxide two-block polymer.
Through research and discovery
(1) A large number of experiments show that the particle size of the mesoporous silica nanoparticle in the step A can be 20-40nm by adding the first composition, the particle size of the mesoporous silica nanoparticle with the particle size of 20-30nm can account for 70% -80%, the particle size of the nanoparticle prepared without adding the first composition is 30-200nm in general, and the proportion of 50-200nm is 70-90%;
(2) and B, the surface-modified mesoporous silica nanoparticles are surface-coated polyaniline nanoparticles, and the mesoporous silica nanoparticles are subjected to performance modification, so that the particles are combined with the matrix through electrostatic action and hydrogen bonds, the binding force is enhanced, and the particles are not easy to fall off in the using process.
(3) In the step B, the first compound is added to effectively reduce the particle size of polyaniline nanoparticles on the surface of the mesoporous silica nanoparticles to be 1-5% and 75% and the particle size of polyaniline nanoparticles 5-10nm to be 20%, and the polyaniline nanoparticles are uniformly coated on the surface of the mesoporous silica nanoparticles.
(4) The surface modification of the base film is carried out by placing the base film in the 2-methoxy-4-methylphenol aqueous solution, the 2-methoxy-4-methylphenol aqueous solution can be autoxidized and polymerized on the surface and micropores of the base film, a large amount of active groups with negative charges such as hydroxyl, phenolic hydroxyl, carboxyl, amino and the like are introduced, the combination with slurry after coating is more compact, and the integral strength of the film is improved, and the specific data are as follows.
(II) test experiment
(1) Tensile strength
The measurement was carried out by using a long film sample having a width of 25mm in accordance with GB/T1040.1-2006 using a CMT4000 electron testing machine manufactured by MTS.
(2) Average pore diameter
The membrane was tested for pore size distribution and mean pore size using a mercury intrusion gauge at pressures of 20-2000Psi according to ISO 15901.1-2006.
(3) Porosity of the material
Testing the prosthetic Density (g/cm) of the diaphragm3) Diaphragm weight/(thickness area), to theoretical value 0.94g/cm3Divided by the porosity of the microporous separator.
(4) Strength of needling
The measuring instrument was a CMT4000 type electron testing machine of MTS, and the maximum load when the polyolefin porous membrane was inserted with a needle having a spherical tip (curvature radius R: 0.5mm) and a diameter of 1mm at a speed of 2mm/s was measured.
Through detection, the lithium ion battery composite diaphragm prepared by the invention has uniform pore size distribution, the porosity reaches 66-83%, preferably 70%, more preferably 75%, the average pore size is less than 60nm, and the tensile strength is as follows: 190 MPa, preferably 260 MPa, 280MPa in the MD direction, and 190 MPa, preferably 260 MPa, 280MPa in the TD direction; the shrinkage rate is lower than 0.5% at 250 ℃, the film thickness is 8-30 μm, preferably 10-20 μm, after the lithium battery using the battery diaphragm is circularly charged and discharged for 800 times, the residual capacity is 95-97%, the service life of the battery is effectively prolonged, and the needling strength is 410-460gf, preferably 415 gf.
It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Claims (6)
1. A lithium ion battery diaphragm is characterized in that the diaphragm comprises at least one layer of lithium battery diaphragm,
the lithium battery diaphragm comprises a substrate layer of a base film subjected to surface modification and at least one film layer dispersed with nano particles;
the lithium battery diaphragm is prepared by the following method:
mixing N-butyl alcohol, N, N-dimethylformamide, nano-silica, polyvinylidene fluoride and carbon tetrachloride, controlling the pH value to be 5-7, stirring and heating to 50-70 ℃, wherein the stirring speed is 1500r/min and the stirring time is 1-6h to obtain mixed slurry;
step two, modifying the surface of the base film
Placing the base film in a 2-methoxy-4-methylphenol aqueous solution, soaking for 30-120min, taking out, washing for 3-6 times by using deionized water, and then placing in a dryer for drying to obtain a surface modified film;
step three, coating
Placing the base film with the modified surface in the second step on a coating machine, and passing the mixed slurry in the first step through an electrostatic spraying device at a rate of 2-4mL/dm2Uniformly spraying the modified film on the lithium battery diaphragm, transferring the film into a drying oven, and drying the film for 5-6 hours at the temperature of 70-80 ℃ to obtain the lithium battery diaphragm;
the nano-silica in the step one is mesoporous silica nano-particles subjected to surface modification, and is prepared by the following method:
step A, preparation of mesoporous silica nanoparticles
(1) Placing hexadecyl trimethyl ammonium bromide into deionized water, mechanically stirring for 15-30min, adding isopropanol and 25% ammonia water after stirring, stirring for 30min at 50-80 ℃, adding tetraethyl orthosilicate and a first composition, heating to 60-100 ℃ at the heating rate of 10-15 ℃/min, stirring for 2-4h, stopping stirring, standing for 15-30h to obtain layered solution, cooling to room temperature, centrifuging by adopting a centrifuge, respectively cleaning precipitates by adopting ethanol and deionized water for 3-6 times, and then drying in vacuum to obtain mesoporous silica nanoparticles;
the mass ratio of the hexadecyl trimethyl ammonium bromide to the deionized water to the first composition to the isopropyl alcohol to the ammonia water to the tetraethyl orthosilicate is 1-3:50-300:10-30:5-20:3-8: 2-4; the first composition is prepared by mixing thiophene, pyrrole and N, N-dimethylformamide according to the mass ratio of 3-6:2-4: 0.5-2;
step B, surface modification of mesoporous silica nanoparticles
Placing the mesoporous silica nanoparticles prepared in the step one, nano polyaniline, ethylenediamine and methanol in a mass ratio of 5-10:6-20:1-4:30-60 in a beaker, stirring at 40-60 ℃, then performing rotary evaporation under reduced pressure to remove the solvent, washing the obtained product with diethyl ether, heating to 40-50 ℃, magnetically stirring the washed product, the first compound and dichloromethane for 30-50min, heating to 60-90 ℃, adding ammonium persulfate under the protection of nitrogen, performing stirring reaction for 10-20h, cooling to room temperature, and washing the precipitate with deionized water for 3-6 times to obtain surface-modified mesoporous silica nanoparticles;
the mass ratio of the mesoporous silica nanoparticles to the first compound to the dichloromethane to the ammonium persulfate is 3-8:6-10:1-5: 2-4;
the first compound is a polyethylene oxide-polypropylene oxide two-block polymer;
the preparation method of the polyethylene oxide-polypropylene oxide two-block polymer comprises the following steps: mixing polyethylene oxide, polypropylene oxide and stannous isooctanoate to obtain a mixture;
the mass ratio of the polyethylene oxide to the polypropylene oxide to the stannous isooctanoate is 5-10:3-9:0.5-1, nitrogen is filled into the mixture for 30min to ensure that oxygen in the mixture is removed, the mixture is transferred into a four-neck flask replaced by nitrogen to be polymerized, the mixture is stirred at the temperature of 80-120 ℃ to react for 15-20h, the reaction product is placed into deionized water with the pH value of 4.0-5.0 to be dialyzed for 1-3 days, and then ethanol is adopted to wash for 3-6 times, so that the polyethylene oxide-polypropylene oxide two-block polymer is obtained.
2. The lithium ion battery separator according to claim 1, wherein the lithium battery separator has a thickness of 8 to 30 μm.
3. The lithium ion battery separator according to claim 1, wherein the lithium battery separator has a thickness of 10 to 20 μm.
4. The lithium ion battery separator according to claim 1, wherein the porosity of the lithium battery separator is 66-83%.
5. The lithium ion battery separator according to claim 1, wherein the mass ratio of N-butanol, N, N-dimethylformamide, nano-silica, polyvinylidene fluoride and carbon tetrachloride is 30-60:10-15:1-5:4-8: 0.5-3.
6. The lithium ion battery separator according to claim 1, wherein the base film is a polyamide film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110332623.9A CN113097651A (en) | 2018-06-29 | 2018-06-29 | Lithium ion battery diaphragm |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110332623.9A CN113097651A (en) | 2018-06-29 | 2018-06-29 | Lithium ion battery diaphragm |
| CN201810696513.9A CN108682775B (en) | 2018-06-29 | 2018-06-29 | Lithium battery diaphragm and application thereof |
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| CN109860480A (en) * | 2018-12-29 | 2019-06-07 | 桑顿新能源科技有限公司 | A kind of gel state lithium ion battery diaphragm and preparation method thereof |
| CN114914631A (en) * | 2022-06-29 | 2022-08-16 | 上海恩捷新材料科技有限公司 | Ultrahigh-strength diaphragm and preparation method thereof |
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| US8067108B1 (en) * | 2007-02-14 | 2011-11-29 | Electrochem Solutions, Inc. | Hybrid battery for use over extended temperature range |
| KR101073981B1 (en) * | 2009-09-30 | 2011-10-17 | 경북대학교 산학협력단 | Nano Composite for Platinum Free Electro-catalyst and Method for Preparation Thereof |
| JPWO2012165624A1 (en) * | 2011-06-03 | 2015-02-23 | 富士シリシア化学株式会社 | Separator and electrochemical element |
| KR101958644B1 (en) * | 2013-05-21 | 2019-03-15 | 주식회사 엘지화학 | Polyolefin separator and method for preparing thereof |
| CN103474609B (en) * | 2013-09-27 | 2015-12-09 | 中材科技股份有限公司 | A kind of folded painting composite lithium battery membrane |
| CN105185940B (en) * | 2015-10-23 | 2018-10-09 | 旭成（福建）科技股份有限公司 | The preparation method and applications of polyolefin/nano crystal fibre element composite diaphragm |
| JP6655776B2 (en) * | 2015-12-17 | 2020-02-26 | パナソニックＩｐマネジメント株式会社 | Silica airgel, heat insulating material and method for producing silica airgel |
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| CN108682775A (en) | 2018-10-19 |
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