CN108807787A - A kind of preparation method of lithium battery power diaphragm - Google Patents
A kind of preparation method of lithium battery power diaphragm Download PDFInfo
- Publication number
- CN108807787A CN108807787A CN201810407882.1A CN201810407882A CN108807787A CN 108807787 A CN108807787 A CN 108807787A CN 201810407882 A CN201810407882 A CN 201810407882A CN 108807787 A CN108807787 A CN 108807787A
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- China
- Prior art keywords
- film
- preparation
- diaphragm
- solution
- microporous polyolefin
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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
- 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
- H01M50/431—Inorganic material
-
- 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 present invention provides a kind of preparation methods of lithium battery power diaphragm, include the following steps：1）Prepare synthesis cotton film cloth：2）Prepare MIcroporous polyolefin film：3）Ceramic diaphragm is synthesized, ceramic diaphragm provided by the invention solves heat resistance（180 degree is not shunk, 200 degree of contractions<1%）, puncture-resistant, lower shrinkage, Electolyte-absorptive speed and amount solve the time and efficiency that battery toasts, improve safety.Solve the strength demand of diaphragm simultaneously, it is laminating after diaphragm, micropore film strength is utilized, is the more diversification of the adaptable range of product.
Description
Technical field
The invention belongs to lithium ion battery separator technologies, and in particular to a kind of preparation method of lithium battery power diaphragm.
Background technology
Market lithium ion battery separator used at present is mostly polyethylene, polypropylene, single-layer or multi-layer and ceramic coated.This
Class diaphragm limits heat resistance because of the matrix of itself, therefore improper to lithium-ion-power cell, because of its poor heat resistance, causes
Diaphragm is easy to shrink and battery is made to generate short circuit, meanwhile, also there is prodigious secret worry in secure context.
At present the shortcomings that polyolefine material class diaphragm：Temperature tolerance is poor（About 95 degree of diaphragms start to shrink at）, porosity is low, to ion
Migration causes obstacle, Electolyte-absorptive overlong time, and temperature tolerance is low, and when battery toasts, temperature is low, needs longer time
Moisture is dried, production efficiency and a large amount of resource of waste are seriously affected；Simultaneously as the limitation of polyolefine material preparation process, when
When this kind of diaphragm encounters hard object puncture, caused injury is irreversible.
Invention content
In view of this, the present invention provides a kind of preparation methods of lithium battery power diaphragm.
The present invention is achieved by the following technical solution：
A kind of preparation method of lithium battery power diaphragm, includes the following steps：
1）Prepare synthesis cotton film：The synthesis cotton film includes following ingredient：0.1D is short fine 40 ~ 55%, ether 25 ~ 35%, acetone 3
~ 5%, glacial acetic acid 4 ~ 7%, methylcellulose 0.3 ~ 0.5%, ethyl alcohol 1 ~ 2%, finish 1 ~ 2%, toluene 1 ~ 2%, resin 2 ~ 3%, surplus are
Diluent；
2）Prepare MIcroporous polyolefin film：Using vistanex, nucleating agent, solvent as raw material, using mass ratio as vistanex：At
Core agent：Solvent=1000~2000：20~50：2000~3000 are prepared into polyolefin solution；Then polyolefin solution will be prepared into
It squeezes out and gel sheet, stretching, film forming solvent removes surface impurity, drying, MIcroporous polyolefin film is made in heat treatment shaping；
3）Synthesize ceramic diaphragm：Will in synthesis cotton film with the one of which of the MIcroporous polyolefin film of 4 ~ 15 grams of specifications or several
It is combined using papermaking wet processing.
Further, the preparation for synthesizing cotton film by following steps：
1）It is 50% 0.1D is short fine and methylcellulose is with ether, acetone, toluene, diluent dissolving, mixing, then by resin,
Finish is added, and is further uniformly mixed, obtained solution A；
2）Ethyl alcohol and glacial acetic acid are mixed, solution B is obtained；
3）Solution A and solution B are placed in 20 ~ 40min of supersound process under ultrasonic wave, the various composition in solution is made to be uniformly mixed simultaneously
Uniform lotion is made；
4）The short fibres of the 0.1D of surplus are completely immersed in step（3）In the lotion being prepared, after impregnating 30 ~ 50min, liquid is then taken off
It is quiet to dry in the air to obtain synthesis cotton film.
Further, the diluent is one or more of ethyl alcohol, ethylene glycol, butanol, isopropanol, acetic acid.
Further, the finish is one or more in rapeseed oil, peanut oil, soya-bean oil, corn oil.
Further, the resin is vistanex.
Further, the vistanex is by ethylene, propylene, 1- butylene, 1- amylenes, 1- hexenes, 1- octenes, 4- first
Base -1- amylenes or its equivalent alpha-olefin and cycloolefin are polymerized alone or combined polymerization forms.
Further, the nucleating agent is 3,4- dimethylbenzylidensorbitols.
Further, the thickness of the synthesis cotton film cloth is 10 ~ 40um.
Further, the thickness of the MIcroporous polyolefin film is 5 ~ 20um.
Beneficial effects of the present invention are：
The wet method ceramic diaphragm of the invention, solves heat resistance（180 degree is not shunk, 200 degree of contractions<1%）, puncture-resistant, low receipts
Contracting, Electolyte-absorptive speed and amount solve time and the efficiency of battery baking, improve safety.It solves simultaneously every film strength
Demand, it is laminating after diaphragm, micropore film strength is utilized, is the more diversification of the adaptable range of product.
Description of the drawings
Fig. 1 is the stereoscan photograph of MIcroporous polyolefin film,
Fig. 2 is the stereoscan photograph for synthesizing cotton film cloth.
Specific implementation mode
Technical scheme of the present invention is further explained below by embodiment, but protection scope of the present invention not by
The limitation of embodiment in any form.
Embodiment 1
A kind of preparation method of lithium battery power diaphragm, includes the following steps：
1）Prepare synthesis cotton film：The synthesis cotton film includes following ingredient：0.1D is short fine 40 ~ 55%, ether 25 ~ 35%, acetone 3
~ 5%, glacial acetic acid 4 ~ 7%, methylcellulose 0.3 ~ 0.5%, ethyl alcohol 1 ~ 2%, finish 1 ~ 2%, toluene 1 ~ 2%, resin 2 ~ 3%, surplus are
Diluent；
2）Prepare MIcroporous polyolefin film：Using vistanex, nucleating agent, solvent as raw material, using mass ratio as vistanex：At
Core agent：Solvent=1000~2000：20~50：2000~3000 are prepared into polyolefin solution；Then polyolefin solution will be prepared into
It squeezes out and gel sheet, stretching, film forming solvent removes surface impurity, drying, MIcroporous polyolefin film is made in heat treatment shaping；
3）Synthesize ceramic diaphragm：Will in synthesis cotton film with the one of which of the MIcroporous polyolefin film of 4 ~ 15 grams of specifications or several
It is combined using papermaking wet processing.
Embodiment 2：
It carries out being combined ceramic diaphragm using wet processing using 6 grams of synthesis cotton film cloth and 4 grams of MIcroporous polyolefin film,
The ceramic diaphragm is produced applied to Novel lithium ion power battery.The Novel lithium ion power battery of production is gone to be detected.
Testing result is：Ionic conductivity is higher than 10-3 S/cm, aperture 195nm, and film thickness is 15 μm, film air penetrability
For 130s/100ml, shrinking percentage < 1% at 200 DEG C, shrinking percentage is 0 at 180 DEG C.
Embodiment 3：
Using 6 grams, 10 grams, 20 grams of synthesis cotton film cloth with 4 grams, 20 grams, 15 grams of MIcroporous polyolefin film using wet processing
It carries out being combined ceramic diaphragm, which produces applied to Novel lithium ion power battery.Go production novel lithium from
Sub- power battery is detected.
Testing result is：Ionic conductivity is higher than 10-3 S/cm, aperture 130nm, and film thickness is 60 μm, film air penetrability
For 190s/100ml, shrinking percentage < 1% at 200 DEG C, shrinking percentage is 0 at 180 DEG C.
Embodiment 4：
Using 20 grams of synthesis cotton film cloth and 15 grams of MIcroporous polyolefin film using wet processing be combined ceramics every
Film, the ceramic diaphragm are produced applied to Novel lithium ion power battery.The Novel lithium ion power battery of production is gone to be detected.
Testing result is：Ionic conductivity is higher than 10-3 S/cm, aperture 180nm, and film thickness is 45 μm, film air penetrability
For 140s/100ml, shrinking percentage < 1% at 200 DEG C, shrinking percentage is 0 at 180 DEG C.
Embodiment 5：
Using 6 grams of synthesis cotton film cloth and 15 grams of MIcroporous polyolefin film using wet processing be combined ceramics every
Film, the ceramic diaphragm are produced applied to Novel lithium ion power battery.The Novel lithium ion power battery of production is gone to be detected.
Testing result is：Ionic conductivity is higher than 10-3 S/cm, aperture 175nm, and film thickness is 25 μm, film air penetrability
For 135s/100ml, shrinking percentage < 1% at 200 DEG C, shrinking percentage is 0 at 180 DEG C.
Embodiment 6：
Using 20 grams of synthesis cotton film cloth and 4 grams of MIcroporous polyolefin film using wet processing be combined ceramics every
Film, the ceramic diaphragm are produced applied to Novel lithium ion power battery.The Novel lithium ion power battery of production is gone to be detected.
Testing result is：Ionic conductivity is higher than 10-3 S/cm, aperture 185nm, and film thickness is 23 μm, film air penetrability
For 130s/100ml, shrinking percentage < 1% at 200 DEG C, shrinking percentage is 0 at 180 DEG C.
With reference to the above embodiments 1 to embodiment 5：Ceramic diaphragm provided by the invention can be existing at present with effective solution
Temperature tolerance it is poor（About 95 degree of diaphragms start to shrink at）, porosity is low, obstacle, Electolyte-absorptive time mistake are caused to the migration of ion
The defect of long conventional membrane, and temperature tolerance is low, when battery toasts, temperature is low, and longer time is needed to dry moisture, serious shadow
Ring production efficiency and a large amount of resource of waste；Simultaneously as the limitation of polyolefine material preparation process, when this kind of diaphragm encounters firmly
When object punctures, caused injury is irreversible.The shortcomings that for current diaphragm, the wet method ceramic diaphragm of the invention, solution
It has determined heat resistance（180 degree is not shunk, 200 degree of contractions<1%）, puncture-resistant, lower shrinkage, Electolyte-absorptive speed and amount, solution are electric
The time of pond baking and efficiency, improve safety.Solve the strength demand of diaphragm simultaneously, it is laminating after diaphragm, be utilized micro-
Hole film strength is the more diversification of the adaptable range of product.
Ceramic diaphragm provided by the invention is because combine the lithium ion made by wet nonwoven fabrics and MIcroporous polyolefin film
Battery diaphragm, function have filled up the unicity of single use MIcroporous polyolefin film or non-woven fabrics ceramic diaphragm, have increased diaphragm
Safety, solve the heat-shrinkable of MIcroporous polyolefin film, forthright equal and non-woven fabrics ceramic diaphragm the large aperture of less porous gap and
The performance of intensity difference etc..The laminating film makes power lithium-ion battery in big multiplying power charge and discharge, because inside battery generation is higher
Temperature can effectively take precautions against, and the good temperature tolerance of laminating diaphragm can make battery short because of the easy contraction generation of high temperature
Road；Because combining the characteristic of two kinds of films, in terms of battery manufacture process, because of good temperature tolerance, good intensive properties are good
The advantages such as good voidage are toasted using 110 ~ 120 degree of temperature, will not have an impact to inside battery material, remove simultaneously
Outside net place's moisture, electricity consumption can also be reduced, to improve production efficiency and save cost.In addition, electrolyte oozes when fluid injection
Saturating speed also improves production efficiency；In secure context, because the characteristics of the high temperature resistant of laminating diaphragm, lower shrinkage, battery core receives firmly
Short circuit is generated when object pierces through, diaphragm will not be shunk immediately, and battery is protected not come into contact in a large area oxygen and generate burning.
The above are merely some embodiments of the present invention.For those of ordinary skill in the art, this hair is not being departed from
Under the premise of bright concept, various modifications and improvements can be made, these are all within the scope of protection of the present invention.
Claims (9)
1. a kind of preparation method of lithium battery power diaphragm, which is characterized in that include the following steps：
1）Prepare synthesis cotton film：The synthesis cotton film includes following ingredient：0.1D is short fine 40 ~ 55%, ether 25 ~ 35%, acetone 3
~ 5%, glacial acetic acid 4 ~ 7%, methylcellulose 0.3 ~ 0.5%, ethyl alcohol 1 ~ 2%, finish 1 ~ 2%, toluene 1 ~ 2%, resin 2 ~ 3%, surplus are
Diluent；
2）Prepare MIcroporous polyolefin film：Using vistanex, nucleating agent, solvent as raw material, using mass ratio as vistanex：At
Core agent：Solvent=1000~2000：20~50：2000~3000 are prepared into polyolefin solution；Then polyolefin solution will be prepared into
It squeezes out and gel sheet, stretching, film forming solvent removes surface impurity, drying, MIcroporous polyolefin film is made in heat treatment shaping；
3）Synthesize ceramic diaphragm：Will in synthesis cotton film with the one of which of the MIcroporous polyolefin film of 4 ~ 15 grams of specifications or several
It is combined using papermaking wet processing.
2. preparation method according to claim 1, which is characterized in that the preparation for synthesizing cotton film by following steps：
1）It is 50% 0.1D is short fine and methylcellulose is with ether, acetone, toluene, diluent dissolving, mixing, then by resin,
Finish is added, and is further uniformly mixed, obtained solution A；
2）Ethyl alcohol and glacial acetic acid are mixed, solution B is obtained；
3）Solution A and solution B are placed in 20 ~ 40min of supersound process under ultrasonic wave, the various composition in solution is made to be uniformly mixed simultaneously
Uniform lotion is made；
4）The short fibres of the 0.1D of surplus are completely immersed in step（3）In the lotion being prepared, after impregnating 30 ~ 50min, liquid is then taken off
It is quiet to dry in the air to obtain synthesis cotton film.
3. preparation method according to claim 1 or 2, which is characterized in that the diluent be ethyl alcohol, ethylene glycol, butanol,
One or more of isopropanol, acetic acid.
4. preparation method according to claim 1 or 2, which is characterized in that the finish be rapeseed oil, peanut oil, soya-bean oil,
It is one or more in corn oil.
5. preparation method according to claim 1, which is characterized in that the resin is vistanex.
6. preparation method according to claim 5, which is characterized in that the vistanex is by ethylene, propylene, 1- fourths
Alkene, 1- amylenes, 1- hexenes, 1- octenes, 4-methyl-1-pentene or its equivalent alpha-olefin and cycloolefin are polymerized alone or are copolymerized
It closes.
7. preparation method according to claim 1, which is characterized in that the nucleating agent is 3,4- dimethyl benzylidene sorbs
Alcohol.
8. preparation method according to claim 1, which is characterized in that the thickness of the synthesis cotton film cloth is 10 ~ 40um.
9. preparation method according to claim 1, which is characterized in that the thickness of the MIcroporous polyolefin film is 5 ~ 20um.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810407882.1A CN108807787A (en) | 2018-05-02 | 2018-05-02 | A kind of preparation method of lithium battery power diaphragm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810407882.1A CN108807787A (en) | 2018-05-02 | 2018-05-02 | A kind of preparation method of lithium battery power diaphragm |
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|---|---|
| CN108807787A true CN108807787A (en) | 2018-11-13 |
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| CN201810407882.1A Pending CN108807787A (en) | 2018-05-02 | 2018-05-02 | A kind of preparation method of lithium battery power diaphragm |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111370623A (en) * | 2020-03-18 | 2020-07-03 | 江苏厚生新能源科技有限公司 | Alumina ceramic diaphragm, preparation method thereof, powder, ceramic slurry and lithium battery |
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| CN102522517A (en) * | 2011-12-22 | 2012-06-27 | 中国科学院青岛生物能源与过程研究所 | Cellulose/inorganic particle composite diaphragm for lithium secondary battery and preparation method thereof |
| CN102522515A (en) * | 2011-12-22 | 2012-06-27 | 中国科学院青岛生物能源与过程研究所 | Cellulose/polymer fiber composite diaphragm material for lithium secondary battery and preparation method thereof |
| CN105576178A (en) * | 2016-02-29 | 2016-05-11 | 黄博然 | Wet nonwoven fabric ceramic diaphragm of lithium ion power battery and preparation method thereof |
| CN107437630A (en) * | 2016-05-26 | 2017-12-05 | 上海恩捷新材料科技股份有限公司 | A kind of lithium battery isolation membrane and its production and use |
| CN107910478A (en) * | 2017-11-14 | 2018-04-13 | 广东骏东科技有限公司 | A kind of high temperature resistant is not easy the ceramic diaphragm shunk and its manufacture method and application |
| CN108075090A (en) * | 2017-11-14 | 2018-05-25 | 广东骏东科技有限公司 | A kind of preparation method of lithium-ion-power cell ceramic diaphragm |
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2018
- 2018-05-02 CN CN201810407882.1A patent/CN108807787A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102522517A (en) * | 2011-12-22 | 2012-06-27 | 中国科学院青岛生物能源与过程研究所 | Cellulose/inorganic particle composite diaphragm for lithium secondary battery and preparation method thereof |
| CN102522515A (en) * | 2011-12-22 | 2012-06-27 | 中国科学院青岛生物能源与过程研究所 | Cellulose/polymer fiber composite diaphragm material for lithium secondary battery and preparation method thereof |
| CN105576178A (en) * | 2016-02-29 | 2016-05-11 | 黄博然 | Wet nonwoven fabric ceramic diaphragm of lithium ion power battery and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111370623A (en) * | 2020-03-18 | 2020-07-03 | 江苏厚生新能源科技有限公司 | Alumina ceramic diaphragm, preparation method thereof, powder, ceramic slurry and lithium battery |
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Application publication date: 20181113 |