CN108682775A - A kind of lithium battery diaphragm and its application - Google Patents
A kind of lithium battery diaphragm and its application Download PDFInfo
- Publication number
- CN108682775A CN108682775A CN201810696513.9A CN201810696513A CN108682775A CN 108682775 A CN108682775 A CN 108682775A CN 201810696513 A CN201810696513 A CN 201810696513A CN 108682775 A CN108682775 A CN 108682775A
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- China
- Prior art keywords
- lithium battery
- diaphragm
- film
- battery diaphragm
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
-
- 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
A kind of lithium battery diaphragm and its application, which is characterized in that this approach includes the following steps, uniformly sprays on the film of property mixed slurry using coating machine, then continues in drying box, dry 5~6h at 70~80 DEG C, you can lithium battery diaphragm.The lithium battery diaphragm of the present invention is that a kind of good safety, punctured resistance and tensile strength are high, has preferable heat resistance, porosity.
Description
Technical field
The present invention relates to a kind of lithium battery diaphragm and its applications.
Background technology
In the structure of lithium battery, diaphragm is one of the interior layer assembly of key.The performance of diaphragm determines the interface knot of battery
Structure, internal resistance etc. directly affect the characteristics such as capacity, cycle and the security performance of battery, and the diaphragm haveing excellent performance is to improving battery
Comprehensive performance play an important role.The main function of diaphragm is that the positive and negative electrode of battery is made to separate, and prevents the two poles of the earth from contacting
And it is short-circuit, additionally have the function of electrolyte ion capable of being made to pass through.Diaphragm material is nonconducting, physicochemical properties pair
The performance of battery has a great impact.The type of battery is different, and the diaphragm of use is also different.For lithium battery series, due to electricity
Solution liquid is organic solvent system, thus needs the diaphragm material of organic solvent-resistant, the general polyene for using high-strength thin-film
Hydrocarbon perforated membrane.
In recent years, polymer dielectric is had been achieved with into commercialization for lithium ion battery, polymer dielectric lithium from
Be both in sub- battery Ion transfer channel and positive and negative pole material between diaphragm effect.Polymer dielectric can be divided into solid
Body polymer dielectric and gel polymer electrolyte, as practical polymer electrolyte diaphragm must satisfy it is following must
Want condition：1. there is high ionic conductivity, to reduce the internal resistance of cell；2. the carry-over factor of lithium ion is basically unchanged, to eliminate
Concentration polarization；3. negligible electron conduction, to ensure effectively to be isolated between electrode；4. electrode material have high chemistry and
Electrochemical stability；5. cheap price, suitable chemical composition ensure environmentally friendly.
The basic performances such as gas, porosity, pore size, thickness cannot well control in a certain range, therefore
It is unable to get effective application, cannot meet the needs of lithium battery high-end field.
Invention content
Patent of the present invention is designed to provide a kind of lithium battery diaphragm, which is characterized in that contains one layer of warp in the diaphragm
Cross the base layer of the basis film of surface modification, and at least one layer of film layer for being scattered with nano particle.
The lithium battery diaphragm thickness is 8-30 μm.
The lithium battery diaphragm thickness is 10-20 μm.
The porosity of the lithium battery diaphragm is 66~83%.
The porosity of the lithium battery diaphragm is 70%.
The porosity of the lithium battery diaphragm is 75%.
The lithium battery diaphragm is prepared by the following method：
Step 1, by n-butanol, n,N-Dimethylformamide, nano silicon dioxide, Kynoar and carbon tetrachloride into
Row mixing, control ph 5-7 are stirred and heated to 50-70 DEG C, and the rate of stirring is 1000-1500r/min, stirring when
Between obtain mixed slurry for 1-6h；
Step 2, film surface are modified
Basis film is placed in 2- methoxyl group -4- methylphenol aqueous solutions, 30-120min is impregnated, uses and goes after taking-up
Ionized water rinses 3-6 and obtains the film of surface modification all over drying in dryer is placed on；
Step 3, coating
Step 2 surface film modified is placed on coating machine, step 1 mixed slurry is passed through into electrostatic application
It sets, with 2-4mL/dm2, even application then continues on modified film in drying box, dry 5~6h at 70~80 DEG C,
Lithium battery diaphragm can be obtained.
The mass ratio of the n-butanol, n,N-Dimethylformamide, nano silicon dioxide, Kynoar and carbon tetrachloride
For 30-60:10-15:1-5:4-8:0.5-3.
The basis film is polyamide film.
A kind of lithium ion battery separator, it is characterised in that include at least one layer of foregoing lithium battery diaphragm.
A kind of battery composite diaphragm, it is characterised in that include at least one layer of foregoing lithium battery diaphragm.
A kind of application of lithium ion battery separator as described in before claim in lithium ion battery separator.
Advantageous effect：
The nanometer micropore battery diaphragm of the present invention is that a kind of safety is good, tensile strength is high, has preferable heat resistance, hole
Gap rate.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.
A kind of lithium battery diaphragm, which is characterized in that the base for the basis film being modified by surface containing one layer in the diaphragm
Body layer, and at least one layer of film layer for being scattered with nano particle.
The lithium battery diaphragm thickness is 8-30 μm.
The lithium battery diaphragm thickness is 10-20 μm.
The porosity of the lithium battery diaphragm is 66~83%.
The porosity of the lithium battery diaphragm is 70%.
The porosity of the lithium battery diaphragm is 75%.
The lithium battery diaphragm is prepared by the following method：
Step 1, by n-butanol, n,N-Dimethylformamide, nano silicon dioxide, Kynoar and carbon tetrachloride into
Row mixing, control ph 5-7 are stirred and heated to 50-70 DEG C, and the rate of stirring is 1000-1500r/min, stirring when
Between obtain mixed slurry for 1-6h；
Step 2, film surface are modified
Basis film is placed in 2- methoxyl group -4- methylphenol aqueous solutions, 30-120min is impregnated, uses and goes after taking-up
Ionized water rinses 3-6 and obtains the film of surface modification all over drying in dryer is placed on；
Step 3, coating
Step 2 surface film modified is placed on coating machine, step 1 mixed slurry is passed through into electrostatic application
It sets, with 2-4mL/dm2, even application then continues on modified film in drying box, dry 5~6h at 70~80 DEG C,
Lithium battery diaphragm can be obtained.
The mass ratio of the n-butanol, n,N-Dimethylformamide, nano silicon dioxide, Kynoar and carbon tetrachloride
For 30-60:10-15:1-5:4-8:0.5-3.
The basis film is polyamide film.
Slurry in step 1 is Kynoar mixed liquor.
A kind of lithium ion battery separator, it is characterised in that include at least one layer of foregoing lithium battery diaphragm.
A kind of battery composite diaphragm, it is characterised in that include at least one layer of foregoing lithium battery diaphragm.
A kind of application of lithium ion battery separator as described in before claim in lithium ion battery separator.
(1) medium hole nano particles in the present invention described in step 1 are the hole nano-particle being modified by surface, specifically
It prepares with the following method：
Step A, prepared by mesoporous silicon dioxide nano particle
(1) cetyl trimethylammonium bromide is placed in deionized water, mechanical agitation 15-30min, is added after stirring
Enter isopropanol and a concentration of 25% ammonium hydroxide, 30min is stirred at 50-80 DEG C, tetraethyl orthosilicate and first chamber is added
And be warming up to after 60-100 DEG C of stirring 2-4h with the heating rate of 10-15 DEG C/min and stop stirring, standing 15-30h is layered
Solution, sediment is respectively washed all over rear true by 3-6 using ethyl alcohol and deionized water using centrifuge after being cooled to room temperature
Sky is dried to obtain mesoporous silica nano-particle；
The cetyl trimethylammonium bromide, deionized water, isopropanol, ammonium hydroxide, tetraethyl orthosilicate and the first combination
The mass ratio of object is 1-3:50-300:10-30:5-20:3-8:2-4；The first chamber is by thiophene, pyrroles and N, N- diformazans
Base formamide is 3-6 with mass ratio:2-4:0.5-2 is mixed to prepare；
The surface of step B, mesoporous silica nano-particle are modified
Mesoporous silica nano-particle prepared by step 1, nano polyaniline, ethylenediamine and methanol are with mass ratio
5-10:6-20:1-4:30-60 is placed in beaker at 40C~60 DEG C and stirs, and then depressurizes rotary evaporation and removes solvent, gained
Product is washed with ether, is warming up to 40-50 DEG C, by product, the first compound and the dichloromethane magnetic agitation 30- after washing
50min is warming up to 60-90 DEG C, Ammonium Persulfate 98.5 is added under the protection of nitrogen, is stirred to react 10-20h, is cooled to room temperature, will precipitate
Object cleans 3-6 times using deionized water and obtains the mesoporous silica nano-particle of surface modification；
The mesoporous silica nano-particle, the first compound, dichloromethane and Ammonium Persulfate 98.5 mass ratio be 3-8:
6-10:1-5:2-4；
First compound is polyethylene oxide-polypropylene oxide bi-block copolymer；
The preparation method of the polyethylene oxide-polypropylene oxide bi-block copolymer includes the following steps：By polycyclic oxygen
Ethane, polypropylene oxide and stannous iso caprylate are mixed to get mixture, and (polyethylene oxide, polypropylene oxide and isooctyl acid are sub-
The mass ratio of tin is 5-10:3-9:0.5-1), and to this mixture nitrogen charging 30min it to ensure to exclude oxygen therein, will mix
Object, which is transferred in the four-hole boiling flask after nitrogen is replaced, to be polymerize, and reacts 15-20h, the production of reaction under being stirred at 80-120 DEG C
Object is placed in the deionized water that pH is 4.0-5.0 and dialyses 1-3 days, uses ethyl alcohol to clean 3-6 times later, had both obtained polycyclic oxygen second
Alkane-polypropylene oxide bi-block copolymer.
It is found by research
(1) pass through many experiments to find to enable to the mesoporous silicon oxide to receive by the way that first chamber is added in step A
The grain size of rice grain is 20-40nm, and grain size can account for 70%-80% for 20-30nm's, be added without first group under normal conditions
The grain size for closing nano-particle made from object is 30-200nm, and the ratio of 50-200nm is 70-90%；
(2) mesoporous silica nano-particle that surface is modified in step B is that surface coats nano polyaniline nano particle,
It is modified by the performance for mesoporous silica nano-particle so that passing through electrostatic interaction and hydrogen bond knot between particle and matrix
It closes so that its binding force enhances, not easy to fall off during use.
(3) effectively to reduce mesoporous silica nano-particle surface polyphenyl by the way that the first compound is added in step B
The grain size of amine nano particle between 1-5 can reach 75%, 5-10nm can reach 20%, be uniformly wrapped in mesoporous
Silica nanoparticle surface, due to grain diameter smaller, bonding strength is to improve film between capable of effectively promoting interface
Tensile strength.
(4) changed by the way that basis film to be placed in the surface of progress basis film in 2- methoxyl group -4- methylphenol aqueous solutions
Property, 2- methoxyl group -4- methylphenols aqueous solution can autoxidation be aggregated in matrix film surface and micropore, introduce a large amount of such as hydroxyls
The negatively charged active group such as base, phenolic hydroxyl group, carboxyl, amino, after coating and the combination of slurry even closer to improve film whole
The intensity of body, specific data are as follows.
(2) test experiments
(1) tensile strength
According to GB/T1040.1-2006 standards, using the strip film print that width is 25mm, using MTS companies
CMT4000 type electronic, horological test-run a machines are measured.
(2) average pore size
According to ISO15901.1-2006 standards, the aperture point of diaphragm is tested under 20-2000Psi pressure using mercury injection apparatus
Cloth and average pore size.
(3) porosity
Test the prosthese density (g/cm of diaphragm3)=diaphragm weight/(thickness * areas), with theoretical value 0.94g/cm3It is divided by,
It is considered as the porosity of micro-pore septum.
(4) needle pierces intensity
Measuring instrument is that the CMT4000 type electronic, horological test-run a machines of MTS companies are tested, and measurement is spherical surface (curvature with front end
Radius R：0.5mm) the needle of diameter 1mm penetrates peak load when polyolefin porous membrane with the speed of 2mm/s.
After testing, lithium ion battery composite separation membrane even aperture distribution produced by the present invention, porosity are excellent up to 66~83%
70%, more preferable 75% is selected, average pore size is less than 60nm, tensile strength：The directions MD 190-300MPa, preferably 260-280MPa,
The directions TD 190-300MPa, preferably 260-280MPa；Shrinking percentage is less than 0.5% at 250 DEG C, and film thickness is 8-30 μm, preferably 10-
20 μm, using the lithium battery of battery diaphragm of the present invention after cycle charge-discharge 800 times, remaining capacity is 95~97%, is effectively prolonged
Battery is grown, needle pierces intensity 410-460gf, preferably 415gf.
It should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.In addition, it should also be understood that,
After reading the content taught by the present invention, those skilled in the art can make various modifications or changes to the present invention, these
Equivalent form is also fallen within the scope of the appended claims of the present application.
Claims (10)
1. a kind of lithium battery diaphragm, which is characterized in that the matrix for the basis film being modified by surface containing one layer in the diaphragm
Layer, and at least one layer of film layer for being scattered with nano particle.
2. a kind of lithium battery diaphragm as described in claim 1, which is characterized in that the lithium battery diaphragm thickness is 8-30 μm.
3. a kind of lithium battery diaphragm as claimed in claim 4, which is characterized in that the lithium battery diaphragm thickness is 10-20 μm.
4. a kind of lithium battery diaphragm as described in claim 1, which is characterized in that the porosity of the lithium battery diaphragm is 66~
83%, preferably 70%, more preferable 75%.
5. a kind of lithium battery diaphragm as described in claim 1, which is characterized in that the lithium battery diaphragm is made by the following method
It is standby：
Step 1 is mixed n-butanol, n,N-Dimethylformamide, nano silicon dioxide, Kynoar and carbon tetrachloride
It closes, control ph 5-7 is stirred and heated to 50-70 DEG C, and the rate of stirring is 1000-1500r/min, and the time of stirring is
1-6h obtains mixed slurry；
Step 2, film surface are modified
Basis film is placed in 2- methoxyl group -4- methylphenol aqueous solutions, 30-120min is impregnated, deionization is used after taking-up
Water rinses 3-6 and obtains the film of surface modification all over drying in dryer is placed on；
Step 3, coating
Step 2 surface film modified is placed on coating machine, by step 1 mixed slurry by electrostatic spraying apparatus,
With 2-4mL/dm2, even application then continues on modified film in drying box, dry 5~6h at 70~80 DEG C, i.e.,
Lithium battery diaphragm can be obtained.
6. a kind of lithium battery diaphragm as claimed in claim 5, which is characterized in that the n-butanol, n,N-Dimethylformamide,
The mass ratio of nano silicon dioxide, Kynoar and carbon tetrachloride is 30-60:10-15:1-5:4-8:0.5-3.
7. a kind of lithium battery diaphragm as claimed in claim 5, which is characterized in that the basis film is polyamide film.
8. a kind of lithium ion battery separator, it is characterised in that include at least one layer of lithium battery as described in one of claim 1-7
Diaphragm.
9. a kind of battery composite diaphragm, it is characterised in that comprising at least one layer of lithium battery as described in one of claim 1-7 every
Film.
10. a kind of lithium ion battery separator as described in one of claim 1-7 is in the application of lithium ion battery separator.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810696513.9A CN108682775B (en) | 2018-06-29 | 2018-06-29 | Lithium battery diaphragm and application thereof |
| CN202110332623.9A CN113097651A (en) | 2018-06-29 | 2018-06-29 | Lithium ion battery diaphragm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810696513.9A CN108682775B (en) | 2018-06-29 | 2018-06-29 | Lithium battery diaphragm and application thereof |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110332623.9A Division CN113097651A (en) | 2018-06-29 | 2018-06-29 | Lithium ion battery diaphragm |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108682775A true CN108682775A (en) | 2018-10-19 |
| CN108682775B CN108682775B (en) | 2021-05-07 |
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ID=63812501
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110332623.9A Withdrawn CN113097651A (en) | 2018-06-29 | 2018-06-29 | Lithium ion battery diaphragm |
| CN201810696513.9A Active CN108682775B (en) | 2018-06-29 | 2018-06-29 | Lithium battery diaphragm and application thereof |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110332623.9A Withdrawn CN113097651A (en) | 2018-06-29 | 2018-06-29 | Lithium ion battery diaphragm |
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| CN (2) | CN113097651A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2024001488A1 (en) * | 2022-06-29 | 2024-01-04 | Shanghai Energy New Materials Technology Co., Ltd. | Ultrahigh strength separators and preparation methods thereof |
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| WO2011040681A1 (en) * | 2009-09-30 | 2011-04-07 | 경북대학교 산학협력단 | Nanocomplex for a platinum-free electrocatalyst, and method for manufacturing same |
| US8067108B1 (en) * | 2007-02-14 | 2011-11-29 | Electrochem Solutions, Inc. | Hybrid battery for use over extended temperature range |
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| KR20140136807A (en) * | 2013-05-21 | 2014-12-01 | 주식회사 엘지화학 | Polyolefin separator and method for preparing thereof |
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2018
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| US8067108B1 (en) * | 2007-02-14 | 2011-11-29 | Electrochem Solutions, Inc. | Hybrid battery for use over extended temperature range |
| WO2011040681A1 (en) * | 2009-09-30 | 2011-04-07 | 경북대학교 산학협력단 | Nanocomplex for a platinum-free electrocatalyst, and method for manufacturing same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2024001488A1 (en) * | 2022-06-29 | 2024-01-04 | Shanghai Energy New Materials Technology Co., Ltd. | Ultrahigh strength separators and preparation methods thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108682775B (en) | 2021-05-07 |
| CN113097651A (en) | 2021-07-09 |
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