CN107394088A - A kind of high performance lithium ion battery barrier film and preparation method thereof - Google Patents

A kind of high performance lithium ion battery barrier film and preparation method thereof Download PDF

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Publication number
CN107394088A
CN107394088A CN201710497643.5A CN201710497643A CN107394088A CN 107394088 A CN107394088 A CN 107394088A CN 201710497643 A CN201710497643 A CN 201710497643A CN 107394088 A CN107394088 A CN 107394088A
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China
Prior art keywords
lithium ion
ion battery
barrier film
preparation
high performance
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CN201710497643.5A
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杨仁党
盛杰
王阳
刘旭
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South China University of Technology SCUT
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South China University of Technology SCUT
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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
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Cell Separators (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention belongs to lithium ion battery separator and biological material crossing domain, and in particular to a kind of high performance lithium ion battery barrier film and preparation method thereof.The preparation method is：Cellulose acetate is dissolved in dimethyl acetamide and acetone solvent；Kynoar hexafluoropropene is dissolved in dimethyl acetamide and acetone solvent and adds nano micro crystal cellulose and is uniformly dispersed, then ready spinning material is subjected to feeding and electrostatic spinning by the syringe needle of concentric assembling, the electrostatic spinning film prepared is immersed after spinning in the lithium hydroxide solution of appropriate concentration and react a period of time, barrier film is finally taken out by being dried in vacuo away moisture, produces the high performance lithium ion battery barrier film.Prepared lithium ion battery separator, tensile strength are more than 40MPa, and ionic conductivity is more than 2mS cm‑1, good thermal stability.

Description

A kind of high performance lithium ion battery barrier film and preparation method thereof
Technical field
The invention belongs to lithium ion battery separator and biological material crossing domain, and in particular to a kind of high-performance lithium ion Battery diaphragm and preparation method thereof.
Background technology
With the fast development of mancarried electronic aid, wearable device, electric automobile, energy storage device, to the performance of battery It is required that more and more higher.And lithium ion battery because its have high-energy-density, high working voltage, have extended cycle life, self discharge is small and Many advantages, such as memory-less effect and widely use.Key components of the barrier film as lithium ion battery, largely determine The performance of lithium ion battery is determined.
Traditional commercialized polyalkene diaphragm, such as polypropylene screen, polyethylene film, although there is some good characteristics, It is its shortcoming it is also obvious that deriving from petroleum-based feedstock, non-renewable, non-degradable, does not meet environment-friendly, sustainable development Main trend.Biomass material, particularly cellulosic material, rich reserves are renewable, degradable, are readily available, and price is suitable, It is that instead of the optimal selection of petroleum-based feedstock.
Electrostatic spinning technique is a kind of technology that polymer solution is drawn into fiber under certain electric field force effect. Fibre diameter prepared by this method is in Nano grade.By change spinning material can with the excellent lithium ion battery of processability every Film.
The content of the invention
To solve the shortcomings that prior art and weak point, primary and foremost purpose of the invention be to provide a kind of high-performance lithium from The preparation method of sub- battery diaphragm.The present invention using cellulose acetate, nano micro crystal cellulose, Kynoar-hexafluoropropene as Raw material, further handled with lithium hydroxide after preparing barrier film with method of electrostatic spinning, finally dry barrier film needed for obtaining.Wherein, receive Rice microcrystalline cellulose can not only improve barrier film intensity, improve diaphragm electrochemical performance, and the carboxyl on its surface is also used for for it Lithium ion binding site is provided in this special-purpose of lithium ion battery separator, can further improve membrane properties；Hydrogen-oxygen The more lithium ions of barrier film can be assigned to improve membrane properties by changing lithium processing, and gained membrane properties are excellent.
Another object of the present invention is to provide high performance lithium ion battery barrier film made from above-mentioned preparation method.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of high performance lithium ion battery barrier film, including following operating procedure：
(1) appropriate cellulose acetate is dissolved in mass ratio as 2：In 1 dimethyl acetamide and acetone mixed solvent, Obtain cellulose acetate solution；Appropriate Kynoar-hexafluoropropene is dissolved in mass ratio as 3：7 dimethyl acetamide In acetone mixed solvent, then add appropriate nano micro crystal cellulose and be uniformly dispersed, obtain Kynoar-hexafluoro third The mixed solution of alkene and nano micro crystal cellulose；
(2) feeding is carried out by the syringe needle of concentric assembling and electrostatic spinning prepares film；Wherein cellulose acetate solution By center syringe needle feeding, the mixed solution of Kynoar-hexafluoropropene and nano micro crystal cellulose is fed by outer ring syringe needle Material；
(3) lithium hydroxide solution that the electrostatic spinning film prepared is immersed to appropriate concentration reacts a period of time, then Barrier film is taken out by being dried in vacuo away moisture, you can barrier film needed for acquisition.
Cellulose acetate mass fraction is 14-16% in cellulose acetate solution described in step (1)；Kynoar- In the mixed solution of hexafluoropropene and nano micro crystal cellulose, Kynoar-hexafluoropropene mass fraction is 8-10%, nanometer Microcrystalline cellulose mass fraction is 0.5-2%.
Step (2) described electrospinning conditions：Spinning voltage 15-20kV, collect distance 15-18cm.
Step (3) the lithium hydroxide solution mass fraction is 1-5%, reaction time 0.5-3h.
A kind of high performance lithium ion battery barrier film, is made by above-mentioned preparation method, and described barrier film tensile strength is more than 40MPa, ionic conductivity are more than 2mS cm-1, good thermal stability, 3h size changing rates are less than 0.1% under the conditions of 200 DEG C.
Compared with prior art, the present invention has advantages below and beneficial effect：
Compared with traditional lithium ion battery separator and preparation method thereof, barrier film prepared by the present invention has higher machinery Intensity, more preferable transference number of ions and ionic conductivity, it not only improves barrier film intensity by adding nano micro crystal cellulose, and And to provide lithium ion binding site in lithium hydroxide processing procedure, possibility is provided further to improve diaphragm electrochemical performance.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
In embodiment using electronic universal tester test tensile strength, using electrochemical alternate impedance spectrum method test from Subconductivity rate, barrier film sample of the same area is taken to be positioned over held for some time observation change in size test thermostabilization in drying box Property.
Embodiment 1
1.2g cellulose acetates are dissolved in 6.8g dimethyl acetamides and acetone (mass ratio 2/1) solvent；By 1.0g Kynoar-hexafluoropropene is dissolved in 9.0g dimethyl acetamides and acetone (mass ratio 3/7) solvent, is then added 0.06g nano micro crystal celluloses are simultaneously uniformly dispersed.Feeding and electrostatic spinning are carried out by the syringe needle of concentric assembling.Acetate fiber Element passes through outer ring pin by center syringe needle feeding, speed 0.8ml/h, Kynoar-hexafluoropropene and nano micro crystal cellulose Head feeding, speed 0.8ml/h.Electrostatic spinning voltage 18kV, collects distance 15cm.The electrostatic spinning film prepared is immersed 2wt% lithium hydroxide solution reaction 1h, then takes out barrier film and is placed in 80 DEG C of vacuum drying chamber 24h, obtain lithium ion battery every Film.
Prepared lithium ion battery separator, tensile strength 41MPa, ionic conductivity are 2.3mS cm-1, heat endurance Well, 3h size changing rates are less than 0.1% under the conditions of 200 DEG C.
Embodiment 2
1.2g cellulose acetates are dissolved in 6.8g dimethyl acetamides and acetone (mass ratio 2/1) solvent；By 1.0g Kynoar-hexafluoropropene is dissolved in 9.0g dimethyl acetamides and acetone (mass ratio 3/7) solvent, is then added 0.09g nano micro crystal celluloses are simultaneously uniformly dispersed.Feeding and electrostatic spinning are carried out by the syringe needle of concentric assembling.Acetate fiber Element passes through outer ring pin by center syringe needle feeding, speed 0.8ml/h, Kynoar-hexafluoropropene and nano micro crystal cellulose Head feeding, speed 0.8ml/h.Electrostatic spinning voltage 18kV, collects distance 15cm.The electrostatic spinning film prepared is immersed 2wt% lithium hydroxide solution reaction 1h, then takes out barrier film and is placed in 80 DEG C of vacuum drying chamber 24h, obtain lithium ion battery every Film.
Prepared lithium ion battery separator, tensile strength 47MPa, ionic conductivity are 2.9mS cm-1, heat endurance Well, 3h size changing rates are less than 0.1% under the conditions of 200 DEG C.
Embodiment 3
1.2g cellulose acetates are dissolved in 6.8g dimethyl acetamides and acetone (mass ratio 2/1) solvent；By 1.0g Kynoar-hexafluoropropene is dissolved in 9.0g dimethyl acetamides and acetone (mass ratio 3/7) solvent, is then added 0.12g nano micro crystal celluloses are simultaneously uniformly dispersed.Feeding and electrostatic spinning are carried out by the syringe needle of concentric assembling.Acetate fiber Element passes through outer ring pin by center syringe needle feeding, speed 0.8ml/h, Kynoar-hexafluoropropene and nano micro crystal cellulose Head feeding, speed 0.8ml/h.Electrostatic spinning voltage 18kV, collects distance 15cm.The electrostatic spinning film prepared is immersed 2wt% lithium hydroxide solution reaction 1h, then takes out barrier film and is placed in 80 DEG C of vacuum drying chamber 24h, obtain lithium ion battery every Film.
Prepared lithium ion battery separator, tensile strength 52MPa, ionic conductivity are 3.3mS cm-1, heat endurance Well, 3h size changing rates are less than 0.1% under the conditions of 200 DEG C.
Embodiment 4
1.2g cellulose acetates are dissolved in 6.8g dimethyl acetamides and acetone (mass ratio 2/1) solvent；By 1.0g Kynoar-hexafluoropropene is dissolved in 9.0g dimethyl acetamides and acetone (mass ratio 3/7) solvent, is then added 0.15g nano micro crystal celluloses are simultaneously uniformly dispersed.Feeding and electrostatic spinning are carried out by the syringe needle of concentric assembling.Acetate fiber Element passes through outer ring pin by center syringe needle feeding, speed 0.8ml/h, Kynoar-hexafluoropropene and nano micro crystal cellulose Head feeding, speed 0.8ml/h.Electrostatic spinning voltage 18kV, collects distance 15cm.The electrostatic spinning film prepared is immersed 2wt% lithium hydroxide solution reaction 1.5h, then takes out barrier film and is placed in 80 DEG C of vacuum drying chamber 24h, obtain lithium ion battery Barrier film.
Prepared lithium ion battery separator, tensile strength 54MPa, ionic conductivity are 3.4mS cm-1, heat endurance Well, 3h size changing rates are less than 0.1% under the conditions of 200 DEG C.
Embodiment 5
1.2g cellulose acetates are dissolved in 6.8g dimethyl acetamides and acetone (mass ratio 2/1) solvent；By 1.0g Kynoar-hexafluoropropene is dissolved in 9.0g dimethyl acetamides and acetone (mass ratio 3/7) solvent, is then added 0.18g nano micro crystal celluloses are simultaneously uniformly dispersed.Feeding and electrostatic spinning are carried out by the syringe needle of concentric assembling.Acetate fiber Element passes through outer ring pin by center syringe needle feeding, speed 0.8ml/h, Kynoar-hexafluoropropene and nano micro crystal cellulose Head feeding, speed 0.8ml/h.Electrostatic spinning voltage 18kV, collects distance 15cm.The electrostatic spinning film prepared is immersed 2wt% lithium hydroxide solution reaction 1.5h, then takes out barrier film and is placed in 80 DEG C of vacuum drying chamber 24h, obtain lithium ion battery Barrier film.
Prepared lithium ion battery separator, tensile strength 50MPa, ionic conductivity are 3.3mS cm-1, heat endurance Well, 3h size changing rates are less than 0.1% under the conditions of 200 DEG C.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (5)

1. a kind of preparation method of high performance lithium ion battery barrier film, it is characterised in that including following operating procedure：
(1) appropriate cellulose acetate is dissolved in mass ratio as 2：In 1 dimethyl acetamide and acetone mixed solvent, obtain Cellulose acetate solution；Appropriate Kynoar-hexafluoropropene is dissolved in mass ratio as 3：7 dimethyl acetamide and third Ketone in the mixed solvent, then add appropriate nano micro crystal cellulose and be uniformly dispersed, obtain Kynoar-hexafluoropropene and The mixed solution of nano micro crystal cellulose；
(2) feeding is carried out by the syringe needle of concentric assembling and electrostatic spinning prepares film；Wherein cellulose acetate solution passes through The mixed solution of center syringe needle feeding, Kynoar-hexafluoropropene and nano micro crystal cellulose passes through outer ring syringe needle feeding；
(3) lithium hydroxide solution that the electrostatic spinning film prepared is immersed to appropriate concentration reacts a period of time, then takes out Barrier film is by being dried in vacuo away moisture, you can barrier film needed for acquisition.
A kind of 2. preparation method of high performance lithium ion battery barrier film according to claim 1, it is characterised in that step (1) cellulose acetate mass fraction is 14-16% in the cellulose acetate solution described in；Kynoar-hexafluoropropene and receive In the mixed solution of rice microcrystalline cellulose, Kynoar-hexafluoropropene mass fraction is 8-10%, nano micro crystal cellulose matter Amount fraction is 0.5-2%.
A kind of 3. preparation method of high performance lithium ion battery barrier film according to claim 1, it is characterised in that step (2) electrospinning conditions：Spinning voltage 15-20kV, collect distance 15-18cm.
A kind of 4. preparation method of high performance lithium ion battery barrier film according to claim 1, it is characterised in that step (3) the lithium hydroxide solution mass fraction is 1-5%, reaction time 0.5-3h.
5. a kind of high performance lithium ion battery barrier film, it is characterised in that it is high as one kind described in any one of Claims 1-4 The preparation method of performance lithium ion battery separator is made.
CN201710497643.5A 2017-06-27 2017-06-27 A kind of high performance lithium ion battery barrier film and preparation method thereof Pending CN107394088A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108417760A (en) * 2018-02-10 2018-08-17 郑州大学 A kind of sodium/sodium-ion battery nonwoven cloth diaphragm and preparation method thereof
CN110409224A (en) * 2019-06-10 2019-11-05 浙江金昌特种纸股份有限公司 A kind of preparation method of cellulose coating lithium ion battery diaphragm
CN114024096A (en) * 2021-06-17 2022-02-08 四川启睿克科技有限公司 Preparation method of battery diaphragm and battery diaphragm
CN115312975A (en) * 2022-07-25 2022-11-08 陈雄 Lithium ion battery diaphragm and preparation method thereof

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CN105185940A (en) * 2015-10-23 2015-12-23 旭成（福建）科技股份有限公司 Preparation method and application of polyolefin/nanocrystal cellulose composite diaphragm
CN106129310A (en) * 2016-08-31 2016-11-16 合肥国轩高科动力能源有限公司 A kind of preparation method of lithium ion battery separator

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CN105185940A (en) * 2015-10-23 2015-12-23 旭成（福建）科技股份有限公司 Preparation method and application of polyolefin/nanocrystal cellulose composite diaphragm
CN106129310A (en) * 2016-08-31 2016-11-16 合肥国轩高科动力能源有限公司 A kind of preparation method of lithium ion battery separator

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108417760A (en) * 2018-02-10 2018-08-17 郑州大学 A kind of sodium/sodium-ion battery nonwoven cloth diaphragm and preparation method thereof
CN108417760B (en) * 2018-02-10 2021-06-11 郑州大学 Non-woven fabric diaphragm of sodium/sodium ion battery and preparation method thereof
CN110409224A (en) * 2019-06-10 2019-11-05 浙江金昌特种纸股份有限公司 A kind of preparation method of cellulose coating lithium ion battery diaphragm
CN114024096A (en) * 2021-06-17 2022-02-08 四川启睿克科技有限公司 Preparation method of battery diaphragm and battery diaphragm
CN115312975A (en) * 2022-07-25 2022-11-08 陈雄 Lithium ion battery diaphragm and preparation method thereof
CN115312975B (en) * 2022-07-25 2024-01-12 上海比杰科技有限公司 Lithium ion battery diaphragm and preparation method thereof

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Application publication date: 20171124