CN102306726A - Compound modified polyolefin lithium ion battery separator and manufacturing method thereof - Google Patents
Compound modified polyolefin lithium ion battery separator and manufacturing method thereof Download PDFInfo
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Abstract
The invention provides a compound modified polyolefin lithium ion battery separator and a manufacturing method thereof. The battery separator is formed by compounding a one-sided or double-sided polyolefin microporous membrane with a layer of thin film, wherein the thin film is formed by dissolving a polymer and inorganic fillers in a solvent; the polymer is polyvinylidene fluoride-hexafluoropropylene, and the inorganic fillers are oxides; and the weight ratio of the polymer to the inorganic fillers is 100:(2-30). The battery separator prepared by the method provided by the invention has the advantages of good wettability, thermal blackout effect and low heat shrinkage, thus the interfacial characteristics between the cathode and anode materials and the separator can be improved, and the safety performance and cycle performance of the battery can be enhanced.
Description
Technical field
The present invention relates to a kind of improved polyolefin lithium ion battery separator and preparation method thereof, belong to energy storage device applications such as battery and capacitor.
Background technology
Battery diaphragm is meant the membrane for polymer in the middle of lithium ion cell positive and negative pole, is one of part of lithium ion battery most critical, and battery security is had direct influence.Its effect has: isolate positive and negative electrode and the electronics in the battery can not be passed freely through; Ion in the electrolyte solution is freely passed through between both positive and negative polarity.The effect that battery diaphragm is isolated both positive and negative polarity make battery overcharge or situation that temperature raises under can limit the rising of electric current, prevent battery short circuit even blast, have the self-closing protective effect of micropore, battery user and equipment are played the effect of safeguard protection.
At present, the lithium ion battery separator material is mainly porous polymer film, like polypropylene (PP), polypropylene, polyethylene/polypropylene (PP/PE/PP) film, and nonwoven fabrics such as glass fibre non-woven, non-woven fabrics of synthetic fiber, ceramic fiber paper, or the like.Polyolefin film is ripe relatively as the technology of lithium ion battery separator material; This is because polyethylene, microporous polypropylene membrane have higher porosity, lower resistance, high tear resistance, antiacid alkali ability, better elastic and to the maintenance performance of aprotic solvent, so the Study on Li-ion batteries using initial stage of development just adopts it as its diaphragm material preferably.But it is relatively poor to the electrolyte compatibility that polyethylene, polypropylene diaphragm exist, and the shortcoming of heat resistance limited (being usually less than 150 ℃), makes the overall performance of battery and fail safe reduce.To this, many scholars have done a large amount of diagram modification work, and are good in the hope of obtaining wetability; The modified diaphragm material that temperature tolerance is high; As improve the wettability of barrier film through the polyolefin surfaces crosslinking technology, improve the barrier film temperature tolerance through methods such as surface-coated polymer and ceramic materials, or the like.
Generally speaking; Technical staff's until data polyethylene in present technique field, the special construction and the performance of polypropylene screen; It is carried out the study on the modification of polymer/inorganic material, and intention remedies the shortcoming of simple polyalkene diaphragm in battery applications, further improves the security performance of lithium ion battery.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes prior art, a kind of composite modified polyolefin lithium ion battery separator is provided, and this barrier film has good wetability, the characteristic that hot blackout effect and thermal contraction are little.In addition, the present invention also will provide the preparation method of this battery diaphragm.
Technical problem according to the invention is realized by following technical scheme.
A kind of composite modified polyolefin lithium ion battery separator, said battery diaphragm is made up of microporous polyolefin film one side or two-sided compound thin film; Said film is dissolved in solvent by polymer and inorganic filler and forms; Said polymer is Kynoar-hexafluoropropylene (PVDF-HFP), and said inorganic filler is an oxide; The weight ratio of said polymer and inorganic filler is 100:2～30.
Above-mentioned composite modified polyolefin lithium ion battery separator, said microporous polyolefin film is a microporous polypropylene membrane, polyethene microporous membrane or microporous polypropylene membrane/polyethene microporous membrane/three layers of composite membrane of microporous polypropylene membrane.
Above-mentioned composite modified polyolefin lithium ion battery separator, said inorganic filler particle diameter is 5～100nm, the specific area >=200m2/g of inorganic filler.
Above-mentioned composite modified polyolefin lithium ion battery separator, said oxide are a kind of or its mixture in silicon dioxide, alundum (Al, titanium dioxide, magnesia, calcium oxide or the zirconium dioxide.
Above-mentioned composite modified polyolefin lithium ion battery separator, said solvent are dimethyl formamide, triethyl phosphate, N-methyl pyrrolidone or dimethyl sulfoxide (DMSO).
A kind of method for preparing above-mentioned composite modified polyolefin lithium ion battery separator, it carries out as follows:
A. prepare the colloidal sol shaped polymer: polymer and inorganic filler are dissolved in the solvent by proportioning (100:2～30), are stirred to dissolving fully, form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: microporous polyolefin film is carried out corona pre-treatment, machine walking speed 20m/min, corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the one side of the microporous polyolefin film after step b surface treatment or two-sided through coating machine, and wet coating layer thickness 1～20 μ m of control single face must apply the battery diaphragm of wet film, and is subsequent use;
D. dry finished product: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, dry composite modified polyolefin lithium ion battery separator; Wherein, baking temperature is 20～90 ℃, drying time＞20 hour.
The preparation method of above-mentioned composite modified polyolefin lithium ion battery separator, among the said step a, polymer and inorganic filler are dissolved in solvent under nitrogen protection, and solution temperature is 20～100 ℃.
Composite modified polyolefin lithium ion battery separator according to the invention, the film that contains polymer and inorganic filler by microporous polyolefin film one side or two-sided compound one deck constitutes; Wherein polymer is Kynoar-hexafluoropropylene, and inorganic filler is an oxide; The weight ratio of polymer and inorganic filler is 100:2～30.Because the present invention has adopted technique scheme, and polymer is improved the wetability and the interfacial property of barrier film, inorganic filler is able to give full play to the barrier film heat resistance.This battery diaphragm has good wetability, the characteristic that hot blackout effect and thermal contraction are little, and its percent thermal shrinkage in the time of 130 ℃ is 3.5%.Shown excellent cycle performance after being assembled into battery by prepared composite improved polyalkene lithium ion battery separator of the present invention, go through 50 circulations after, capacity still keeps 94.53%, has improved the interfacial property between positive and negative pole material and the barrier film greatly.
Description of drawings
Fig. 1 is made into the cycle performance test result of battery for No. 1,2,3, modified diaphragm and Celgard2400 barrier film.
Embodiment
Below in conjunction with specific embodiment the present invention is explained further details.
Embodiment 1
A. prepare the colloidal sol shaped polymer: with 1g PVDF-HFP (molecular weight 900; 000) and) < 50nm, surface group are that the modified manometer silicon dioxide of vinyl dissolves in the 45ml dimethyl formamide (DMF) under N2 protection to the 0.2g diameter; Temperature is controlled at 70 ℃; Be stirred well to dissolving fully; Form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: with thickness is that the microporous polypropylene membrane of 20 μ m carries out corona pre-treatment, machine walking speed 20m/min, and corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the one side of the microporous polypropylene membrane after step b surface treatment through coating machine, and the wet coating layer thickness of control single face must apply the battery diaphragm of wet film less than 5 μ m, and is subsequent use;
D. the dry finished product that gets: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 20 ℃, and 20 hours drying times, getting thickness is the composite modified polyolefin lithium ion battery separator of 25 μ m.
A. prepare the colloidal sol shaped polymer: with 1g PVDF-HFP (molecular weight 900; 000) and) < 50nm, surface group are that the modified manometer silicon dioxide of vinyl dissolves in the 40ml dimethyl formamide (DMF) under N2 protection to the 0.1g diameter; Temperature is controlled at 100 ℃; Be stirred well to dissolving fully; Form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: with thickness is that the polyethene microporous membrane of 20 μ m carries out corona pre-treatment, machine walking speed 20m/min, and corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the one side of the polyethene microporous membrane after step b surface treatment through coating machine, and the wet coating layer thickness of control single face must apply the battery diaphragm of wet film less than 5 μ m, and is subsequent use;
D. the dry finished product that gets: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 90 ℃, and 23 hours drying times, getting thickness is the composite modified polyolefin lithium ion battery separator of 25 μ m.
Embodiment 3
A. prepare the colloidal sol shaped polymer: with 1g PVDF-HFP (molecular weight 900; 000) and) < 50nm, surface group are that the modified manometer silicon dioxide of vinyl dissolves in the 40ml dimethyl formamide (DMF) under N2 protection to the 0.05g diameter; Temperature is controlled at 60 ℃; Be stirred well to dissolving fully; Form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: with thickness is that microporous polypropylene membrane/polyethene microporous membrane/three layers of composite membrane of microporous polypropylene membrane of 40 μ m carry out corona pre-treatment, machine walking speed 20m/min, and corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the one side of three layers of composite membrane after step b surface treatment through coating machine, and the wet coating layer thickness of control single face must apply the battery diaphragm of wet film less than 5 μ m, and is subsequent use;
D. the dry finished product that gets: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 70 ℃, and 25 hours drying times, getting thickness is the composite modified polyolefin lithium ion battery separator of 45 μ m.
Embodiment 4
A. prepare the colloidal sol shaped polymer: with 1g PVDF-HFP (molecular weight 900; 000) and) < the 100nm alundum (Al dissolves in the 50ml triethyl phosphate (TEP) down in N2 protection the 0.02g diameter, and temperature is controlled at 20 ℃, is stirred well to fully to dissolve; Form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: with thickness is that microporous polypropylene membrane/polyethene microporous membrane/three layers of composite membrane of microporous polypropylene membrane of 30 μ m carry out corona pre-treatment, machine walking speed 20m/min, and corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the two-sided of three layers of composite membrane after step b surface treatment through coating machine, and the wet coating layer thickness of control single face must apply the battery diaphragm of wet film less than 10 μ m, and is subsequent use;
D. the dry finished product that gets: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 80 ℃, and 22 hours drying times, getting thickness is the composite modified polyolefin lithium ion battery separator of 40 μ m.
Embodiment 5
A. prepare the colloidal sol shaped polymer: with 1g PVDF-HFP (molecular weight 900; 000) and) < titanium dioxide of 100nm dissolves in the 60ml N-methyl pyrrolidone (NMP) down in N2 protection the 0.3g diameter, and temperature is controlled at 40 ℃, is stirred well to fully to dissolve; Form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: with thickness is that the microporous polypropylene membrane of 20 μ m carries out corona pre-treatment, machine walking speed 20m/min, and corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the two-sided of microporous polypropylene membrane after step b surface treatment through coating machine, and the wet coating layer thickness of control single face must apply the battery diaphragm of wet film less than 15 μ m, and is subsequent use;
D. the dry finished product that gets: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 50 ℃, and 21 hours drying times, getting thickness is the composite modified polyolefin lithium ion battery separator of 35 μ m.
Embodiment 6
A. prepare the colloidal sol shaped polymer: with 1g PVDF-HFP (molecular weight 900; 000) and) < magnesia of 100nm dissolves in the 40ml dimethyl sulfoxide (DMSO) (DMSO) down in N2 protection the 0.08g diameter, and temperature is controlled at 30 ℃, is stirred well to fully to dissolve; Form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: with thickness is that the polyethene microporous membrane of 20 μ m carries out corona pre-treatment, machine walking speed 20m/min, and corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the two-sided of polyethene microporous membrane after step b surface treatment through coating machine, and the wet coating layer thickness of control single face must apply the battery diaphragm of wet film less than 20 μ m, and is subsequent use;
D. the dry finished product that gets: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 60 ℃, and 24 hours drying times, getting thickness is the composite modified polyolefin lithium ion battery separator of 40 μ m.
Embodiment 7
Get the composite modified polyolefin lithium ion battery separator of embodiment 1,2,3,4,5,6 gained, test its heat-shrinkable under free state respectively.
Shrinkage under table 1 different temperatures
Can see, in the time of 160 ℃, still can keep original shape, simple PP film, PE film have good temperature tolerance, and be significant to the fail safe that improves battery.
Embodiment 8
Adopt winding method and aluminum-plastic composite membrane to pack Celgard2400, the composite modified polyolefin lithium ion battery separator of embodiment 1,2,3 gained and the lithium cobaltate cathode sheet for preparing and graphite cathode; Inject electrolyte and sealing behind the vacuumize 24h; Accomplish electric core and make, and carry out the charge-discharge performance test.
The result: 4 kinds of barrier films show that through the discharge capacity of preceding 50 circulations the lithium battery that the composite modified polyolefin lithium ion battery separator of the present invention is formed has excellent cycle performance.
Fig. 1 is made into the cycle performance test result of battery for No. 1,2,3, modified diaphragm and Celgard2400 barrier film.Can know that by figure battery integral body in capacity performance is higher than the Celgard2400 diaphragm cell behind 2,3,1 diagram modification, its first capacity be respectively 681.8mAh, 677.9mAh, 669.2 mAh, 651.3 mAh; 2,3,1, the Celgard2400 diaphragm cell through 50 circulations after, capability retention is respectively 94.53%, 94.08%, 93.98%, 93.52%.Comprehensive above result can know that modification metacneme battery not only capacity is bringd into play, and has shown better cycle performance, No. 2 modified diaphragm batteries especially, and after circulating for 50 times, capacity still keeps 94.53%.
Claims (7)
1. a composite modified polyolefin lithium ion battery separator is characterized in that, said battery diaphragm is made up of in its one side or two-sided compound thin film microporous polyolefin film; Said film is prepared from polymer, inorganic filler and solvent; Said polymer is Kynoar-hexafluoropropylene, and said inorganic filler is an oxide; The weight ratio of said polymer and inorganic filler is 100:2～30.
2. composite modified polyolefin lithium ion battery separator according to claim 1 is characterized in that said microporous polyolefin film is a microporous polypropylene membrane, polyethene microporous membrane or microporous polypropylene membrane/polyethene microporous membrane/three layers of composite membrane of microporous polypropylene membrane.
3. composite modified polyolefin lithium ion battery separator according to claim 2 is characterized in that said inorganic filler particle diameter is 5～100nm, the specific area>=200m of inorganic filler
2/ g.
4. composite modified polyolefin lithium ion battery separator according to claim 3 is characterized in that, said oxide is a kind of or its mixture in silicon dioxide, alundum (Al, titanium dioxide, magnesia, calcium oxide or the zirconium dioxide.
5. composite modified polyolefin lithium ion battery separator according to claim 4 is characterized in that, said solvent is dimethyl formamide, triethyl phosphate, N-methyl pyrrolidone or dimethyl sulfoxide (DMSO).
6. one kind prepares like claim 1,2,3, the method for composite modified polyolefin lithium ion battery separator as described in 4 or 5, it is characterized in that it carries out as follows:
A. prepare the colloidal sol shaped polymer: polymer and inorganic filler are dissolved in the solvent by proportioning, are stirred to dissolving fully, form the colloidal sol shaped polymer, subsequent use;
B. microporous polyolefin film surface preparation: microporous polyolefin film is carried out corona pre-treatment, machine walking speed 20m/min, corona discharge power 500W, 2～10 kilovolts of corona voltages, subsequent use;
C. coated film: step a gained colloidal sol shaped polymer is coated in the one side of the microporous polyolefin film after step b surface treatment or two-sided through coating machine, and wet coating layer thickness 1～20 μ m of control single face must apply the battery diaphragm of wet film;
D. dry finished product: the battery diaphragm that step c gained is applied wet film is transferred in the vacuum drying chamber, and baking temperature is 20～90 ℃, drying time＞20 hour, composite modified polyolefin lithium ion battery separator.
7. the preparation method of composite modified polyolefin lithium ion battery separator according to claim 6 is characterized in that, among the said step a, polymer and inorganic filler are dissolved in solvent under nitrogen protection, and solution temperature is 20～100 ℃.
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| CN103066229A (en) * | 2012-12-28 | 2013-04-24 | 广东精进能源有限公司 | Composite polymer separator and preparation method thereof |
| CN103236510A (en) * | 2013-04-18 | 2013-08-07 | 中南大学 | Lithium ion secondary battery polymer separation film corona processing method |
| CN103378332A (en) * | 2012-04-28 | 2013-10-30 | 苏州纳新新能源科技有限公司 | Composite film for battery |
| WO2013185335A1 (en) * | 2012-06-15 | 2013-12-19 | 新乡市中科科技有限公司 | Lithium ion battery composite separator |
| CN103545474A (en) * | 2013-10-29 | 2014-01-29 | 中国第一汽车股份有限公司 | Poly-dopamine modified lithium-ion battery diaphragm and preparation method thereof |
| CN103579561A (en) * | 2012-07-25 | 2014-02-12 | 三星Sdi株式会社 | Separator for rechargeable lithium battery, and rechargeable lithium battery including same |
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| WO2013185335A1 (en) * | 2012-06-15 | 2013-12-19 | 新乡市中科科技有限公司 | Lithium ion battery composite separator |
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| CN103066229A (en) * | 2012-12-28 | 2013-04-24 | 广东精进能源有限公司 | Composite polymer separator and preparation method thereof |
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| CN103236510A (en) * | 2013-04-18 | 2013-08-07 | 中南大学 | Lithium ion secondary battery polymer separation film corona processing method |
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| CN103545474B (en) * | 2013-10-29 | 2016-01-20 | 中国第一汽车股份有限公司 | A kind of lithium ion battery separator of poly-dopamine modification and preparation method |
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