CN106785032B - A kind of lithium ion battery polymer dielectric and preparation method - Google Patents
A kind of lithium ion battery polymer dielectric and preparation method Download PDFInfo
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- CN106785032B CN106785032B CN201710159748.XA CN201710159748A CN106785032B CN 106785032 B CN106785032 B CN 106785032B CN 201710159748 A CN201710159748 A CN 201710159748A CN 106785032 B CN106785032 B CN 106785032B
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
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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
Abstract
A kind of lithium ion battery polymer dielectric and preparation method, are related to lithium ion battery electrolyte field.It is specifically performed polymer with end silane-terminated polyether oligomer, for electric conducting lithium salt as lithium source, organic solvent is plasticizer, and tin class salt is polymer dielectric and its application in lithium ion polymer battery made of catalyst crosslinking curing.The polymer dielectric has both the characteristic of polypropylene oxide (PEO) and silicon rubber, has that excellent mechanical property, high-low temperature resistant stability, electrochemical stability window are stable, ionic conductivity is high and to may continue to work, preparation condition and simple process easily-controllable for lithium ion battery at 80 DEG C.The polymer dielectric has the good flexible on the one hand effective growth for inhibiting cathode Li dendrite, and the interface stability of lithium ion polymer battery on the other hand can be improved, be suitable for flexible lithium ion polymer battery.
Description
Technical field
The present invention relates to lithium ion battery electrolyte field, especially a kind of new type lithium ion battery polymer electrolytic
Matter.
Background technique
Lithium ion battery is due to shared in modern energy storage device with advantages such as high-energy density, high stability and fast charges
Specific gravity it is increasing, be used on electric vehicle and mobile electronic device extensively.Maximum advantage is to realize zero carbon
Bleed schedule promotes modern electric vehicle industry rapidly to develop, and then a large amount of fast charging and discharging performances of demand, safety and stability performance are good
Lithium ion battery.The structure and performance of lithium ion battery electrolyte mention lithium ion battery high rate performance and thermal stability
Height plays vital link.Traditional lithium ion battery separator generally uses polyolefin polymers (polypropylene (PP)) logical
It crosses addition liquid electrolyte (lithium hexafluoro phosphate+ethylene carbonate/propylene carbonate), but this kind of membrane for polymer moistens electrolyte
Moist difference, high pressure, which is easily decomposed, generates gas, causes liquid side leakage, causes safety accident.Although by addition fire retardant, using resistance to
Refractory ceramics diaphragm, the measures such as optimization battery structure design, can improve the safety of lithium ion battery, but nothing to a certain extent
Method fundamentally solves existing security risk.Therefore lithium ion polymer electrolyte replaces traditional liquid electrolyte, for lithium
Secondary cell development has epoch-making meaning.First, polymer dielectric can effectively prevent the generation of metal Li dendrite, make lithium
It is possibly realized as cathode, so that the electrochemistry capacitance of battery be greatly improved;Second, can arbitrary shape, may also be fabricated which multilayer
Formula superthin structure and miniaturization, the flexible lithium ion battery suitable for wearable electronic.
1973, Wright had found that the mixture of polyethylene glycol oxide (PEO) and electrolytic salt has ionic conduction for the first time
Property.1979, the confirmed discovery of Armand, and propose the electrolyte as solid state battery, so that electrostrictive polymer
Solution Quality Research enters a new developing stage.Exist in view of by the solid electrolyte of representative of PEO polymer dielectric class
There are still ionic conductivity, low (PEO room-temperature conductivity is about 10 under room temperature-7Scm-1) and lower electrochemical stability window
Mouthful, it is not able to satisfy the demand in market still, can not be widely used and promote.Although many scholars have carried out physical modification to PEO
(being blended, addition plasticizer) and chemical modification (graft modification), can improve the ionic conductivity (room of PEO to a certain extent
Temperature is up to 10-5~10-4Scm-1), but there are still interface problems.The performed polymer of gel-type polymer electrolyte is generally linear poly-
Object is closed, electrolyte is can absorb after synthesis and forms gel polymer electrolyte, ionic conductivity with higher in this way and good
Interface performance, however, there are also poor mechanical property, dimensional performance are unstable, it is also possible to and cause electrolyte side leakage dangerous,
Eradicate security risk.
The patent No. 201010607369.0 provides a kind of electrolyte of organic silicon amine containing polyether chain having a wide range of application
And its application in lithium battery, the electrolyte of organic silicon amine containing polyether chain of synthesis have good chemical property.Specially
Benefit numbers 201610055337.1 provides a kind of new type lithium ion battery polymer dielectric and preparation method thereof.But simultaneously
There is poor mechanical property, dimensional performance are unstable, it is also possible to cause electrolyte side leakage dangerous.The patent No.
201610055337.1 providing a kind of new type lithium ion battery polymer dielectric and preparation method thereof.By by silicon methoxy
For base end capped polyether oligomer as matrix polymer, boric acid class lithium salts can also the friendship of catalysis matrix polymer in situ in addition to as lithium source
Connection, to prepare the polymer dielectric of end group crosslinking.The polymer dielectric has good mechanical property, and has more
Ideal ionic conductivity and wider electrochemical stability window.But since boric acid class lithium salts has the effect of self-catalysis, cause
Curing time and curing degree are uncontrollable, difficulty increased for production technology, and volume production is difficult.
Therefore, on the basis of original research, the present invention develops a kind of new type lithium ion battery polymer dielectric
And its lithium ion polymer battery constituted.Selection end silane-terminated polyether oligomer is performed polymer, has methoxyl group, ethyoxyl
The end-silicane-group group of equal alkoxies is prepolymer reaction active group, impart polymer dielectric have it is excellent weather-proof, resistance to
Long property, heat-resisting, cold resistance, excellent technological operation performance and high elongation rate and high intensity;Polyether backbone is lithium ion ligand,
Approach is provided for the conduction of lithium ion.Film-forming is allowed to by the way that organic solvent and electric conducting lithium salt is added.It can be found that passing through
The content for adjusting tin catalyst can accurately control curing time and the curing degree of polymer, keep experimental technique simple
Change.New type lithium ion battery polymer dielectric solves Li dendrite and pierces through diaphragm, multiplying power discharging property difference and interfacial contact hardly possible
Topic, further improves the chemical property, high rate performance and security performance of lithium ion polymer battery.
Summary of the invention
The purpose of the present invention is overcoming problem of the prior art, provide a kind of new type lithium ion battery polymer dielectric and
Preparation method.
The technical solution of the present invention is as follows:
A kind of lithium ion battery polymer electrolyte, it is characterised in that: the raw material before crosslinking curing are the end of viscous state
Silante terminated polyethers performed polymer, electric conducting lithium salt, organic solvent and tin catalyst mixture, the viscous state end silane
The mass fraction that end capped polyether accounts for mixture is 10-60%, and the mass fraction that electric conducting lithium salt accounts for mixture is 10-60%, organic
The mass fraction that solvent accounts for mixture is 20-70%, and tin catalyst mass fraction is the matter for holding silane-terminated polyether performed polymer
Measure the 0.5-5% of score;Curing time and curing degree are controlled by adjusting tin catalyst content.
Further below preferably: the viscosity for holding Silante terminated polyethers performed polymer is 5000-30000 centipoise.
Electric conducting lithium salt is one or more of following: LiPF6、LiCF3SO3、LiN(CF3SO2)2、LiN(C2F5SO2)2、
LiN(CF3SO2)(C4F9SO2)、LiC(CF3SO2)3、LiC(C2F5SO2)3、LiAsF6、LiClO4。
Organic solvent is one or more of following: ethylene carbonate, propene carbonate, butylene carbonate rouge, carbonic acid two
Methyl esters, ethylene carbonate, methyl ethyl carbonate, gamma-butyrolacton, tetrahydrofuran, 2- methyltetrahydrofuran, acetonitrile, tetraethylene glycol two
Methyl ether, triethylene glycol dimethyl ether, diethylene glycol dimethyl ether, dimethyl sulfoxide;
Electric conducting lithium salt and organic solvent constitute electrolyte, and the concentration of electric conducting lithium salt in the electrolytic solution is 0.1-3mol L-1。
Tin catalyst is by one of following:: two (dodecyl sulphur) dibutyl tins, dioctyl tin replace dibutyl
Tin, dialkyl tin dimaleate, dibutyltin diacetate, two mercaptan tin alkyls, dilaurate dibutyl tin, bis- (acetyl
Pyruvic acid) dibutyl tin, stannous octoate, platinum water catalyst.
The preparation method of lithium ion battery polymer electrolyte described above, comprising the following steps: by electric conducting lithium salt and have
Solvent is made into electric conducting lithium salt electrolyte, and is uniformly mixed;Weigh the Silante terminated polyethers performed polymer in the end of corrresponding quality score
Mix with electric conducting lithium salt electrolyte and uniform stirring: the tin catalyst that corrresponding quality score is added stirs evenly;It will stir equal
Even polymer electrolytic mixed liquor is coated in Teflon mould, is heating and curing at 30-80 DEG C, according to use
The amount of catalyst generally formed a film at 2-12 hours.
Innovation and practicality of the invention is:
1. using the polyether oligomers with silane group for performed polymer, electric conducting lithium salt electrolyte is added, is rationally designed, is led to
The content of tin catalyst is overregulated to control curing time and the curing degree of reaction, prepares new type lithium ion battery polymer
Electrolyte.Polymer dielectric preparation process is simple, contractibility is small, electrochemical stability is strong, has good flexibility
On the one hand the effective growth for inhibiting cathode Li dendrite, on the other hand can be improved the interface stability of lithium ion polymer battery
Property.
2. polymer dielectric preparation process provided by the invention is simple, can quantify to produce.
3. the polymer dielectric has both the characteristic of polypropylene oxide (PEO) and silicon rubber, have excellent mechanical property,
High-low temperature resistant stability, electrochemical stability window stable (> 5.0V), (room temperature is up to 10 for ionic conductivity height-4Scm-1, 40 DEG C
Up to 10-3Scm-1) and lithium ion battery may continue to work at 80 DEG C.
Detailed description of the invention
Fig. 1 is stainless steel/polymer dielectric/stainless steel system AC impedance spectroscopy in embodiment 6, calculates lithium ion
Conductivity;
Fig. 2 is the steady-state current spectrogram of Li/ polymer dielectric/Li system in embodiment 6, calculates lithium ion transference number
Fig. 3 is the volt-ampere linear scan figure of polymer dielectric in embodiment 6.
Specific embodiment
Illustrate the present invention below by way of specific embodiment, providing embodiment is for a better understanding of the present invention, never
It is to limit the scope of the invention.The viscosity of polyethers performed polymer is 5000-30000 centipoise.
Embodiment 1
By 2.48g LiPF6It is dissolved into 5ml ethylene carbonate (EC) and propene carbonate (PC) (V:V=1:1), room temperature
Lower stirring makes it completely dissolved.The end 3g silane envelope is added to the electrolyte of lithium hexafluoro phosphate, ethylene carbonate and propene carbonate
The polypropylene oxide performed polymer of end polyethers stirs evenly, and 0.1g dioctyl tin is finally added dropwise and replaces dibutyl tin uniform stirring.?
On Teflon mould, using cellulose membrane as support frame, by the polymer dielectric stirred evenly blade coating to cellulose membrane
Two sides, 60 DEG C of heating, 6 hours film-formings under drying box.
Embodiment 2
By 1.89g LiC (CF3SO2)3Be dissolved into 4ml ethylene carbonate (EC) and tetraethyleneglycol dimethyl ether (TEGDME) (V:
V=1:1 in), stirring is made it completely dissolved at room temperature.To the electricity of lithium hexafluoro phosphate, ethylene carbonate and tetraethyleneglycol dimethyl ether
The polypropylene oxide performed polymer that the end 3g silane-terminated polyether is added in solution liquid stirs evenly and (indicates viscosity number-average molecular weight), finally drips
Add bis- mercaptan tin alkyl uniform stirring of 0.07g.On Teflon mould, using non-woven fabrics as support frame, it will stir evenly
Polymer dielectric scratch to the two sides of cellulose membrane, 80 DEG C of heating, 4 hours film-formings under drying box.
Embodiment 3
By 1.22g LiClO4Be dissolved into 3ml triethylene glycol dimethyl ether and tetraethyleneglycol dimethyl ether (TEGDME) (V:V=1:
1) in, stirring is made it completely dissolved at room temperature.To the electrolyte of lithium perchlorate, triethylene glycol dimethyl ether and tetraethyleneglycol dimethyl ether
The polypropylene oxide performed polymer that the end 2g silane-terminated polyether is added stirs evenly, and it is uniform that 0.04g platinum water catalyst is finally added dropwise
Stirring.On Teflon mould, using cellulose membrane as support frame, by the polymer dielectric stirred evenly blade coating to fibre
Tie up the two sides of plain film, 70 DEG C of heating, 4 hours film-formings under drying box.
Embodiment 4
By 0.78g LiClO4Be dissolved into 3ml ethylene carbonate (EC) and tetraethyleneglycol dimethyl ether (TEGDME) (V:V=1:
1) in, stirring is made it completely dissolved at room temperature.To lithium perchlorate, the electrolyte of ethylene carbonate and tetraethyleneglycol dimethyl ether adds
The polypropylene oxide performed polymer for entering the end 2g silane-terminated polyether stirs evenly, and 0.04g dialkyl tin dimaleate is finally added dropwise
Uniform stirring.On Teflon mould, using cellulose membrane as support frame, the polymer dielectric stirred evenly is scratched
To the two sides of cellulose membrane, 60 DEG C of heating, 4 hours film-formings under drying box.
Embodiment 5
By 1.89g LiN (CF3SO2)2Be dissolved into 3ml ethylene carbonate (EC) and tetraethyleneglycol dimethyl ether (TEGDME) (V:
V=1:1 in), stirring is made it completely dissolved at room temperature.To the electricity of lithium hexafluoro phosphate and ethylene carbonate and tetraethyleneglycol dimethyl ether
The polypropylene oxide performed polymer that the end 2g silane-terminated polyether is added in solution liquid stirs evenly, and two horse of 0.03g dialkyl tin is finally added dropwise
Carry out acid esters uniform stirring.On Teflon mould, using non-woven fabrics as support frame, the polymer dielectric that will stir evenly
The two sides for scratching cellulose membrane, 60 DEG C of heating, 6 hours film-formings under drying box.
Embodiment 6
By 1.12g LiN (CF3SO2)2It is dissolved into 2ml tetraethyleneglycol dimethyl ether (TEGDME), stirring keeps its complete at room temperature
Fully dissolved.The poly- of the end 2g silane-terminated polyether is added to the electrolyte of double trifluoromethanesulfonimide lithiums and tetraethyleneglycol dimethyl ether
Propylene oxide performed polymer stirs evenly, and 0.06g dilaurate dibutyl tin uniform stirring is finally added dropwise.In polytetrafluoroethylene (PTFE) mould
On tool, using non-woven fabrics as support frame, the polymer dielectric stirred evenly is scratched to the two sides of cellulose membrane, in drying box
10 hours film-formings of lower 50 DEG C of heating.
Embodiment 7
By 1.29g LiPF6With 0.78g LiC (C2F5SO2)3Be dissolved into 5ml triethylene glycol dimethyl ether and with tetraethylene glycol two
In methyl ether (TEGDME) (V:V=1:1), stirring is made it completely dissolved at room temperature.To lithium hexafluoro phosphate, lithium perchlorate, three second two
The polypropylene oxide performed polymer stirring that the end 3g silane-terminated polyether is added in the electrolyte of diethylene glycol dimethyl ether and tetraethyleneglycol dimethyl ether is equal
It is even, 0.03g stannous octoate uniform stirring is finally added dropwise.On Teflon mould, using non-woven fabrics as support frame, it will stir
Uniform polymer dielectric blade coating is to the two sides of cellulose membrane, 60 DEG C of heating, 4 hours film-formings under drying box.
Embodiment 8
By 0.67g LiPF6With 0.78g LiN (CF3SO2)2It is dissolved into 5ml ethylene carbonate (EC) and tetraethylene glycol diformazan
In ether (TEGDME) (V:V=1:1), stirring is made it completely dissolved at room temperature.To lithium hexafluoro phosphate, double trifluoromethanesulfonimides
The polypropylene oxide performed polymer of the end 1.6g silane-terminated polyether is added in the electrolyte of lithium, ethylene carbonate and tetraethyleneglycol dimethyl ether
It stirs evenly, 0.04g stannous octoate uniform stirring is finally added dropwise.On Teflon mould, using cellulose membrane as support rib
Frame, by the polymer dielectric stirred evenly blade coating to the two sides of cellulose membrane, 60 DEG C of heating are solidified into for 8 hours under drying box
Film.
Embodiment 9
By 0.89g LiN (CF3SO2)(C4F9SO2) and with 0.78g LiN (CF3SO2)2It is dissolved into 5ml tetraethylene glycol diformazan
In ether (TEGDME), stirring is made it completely dissolved at room temperature.To lithium perchlorate, double trifluoromethanesulfonimide lithiums and tetraethylene glycol
The polypropylene oxide performed polymer that the end 3g silane-terminated polyether is added in the electrolyte of dimethyl ether stirs evenly, and 0.04g bis- is finally added dropwise
Laurate dibutyl tin uniform stirring.It is poly- by what is stirred evenly using non-woven fabrics as support frame on Teflon mould
Polymer electrolyte is scratched to the two sides of cellulose membrane, 60 DEG C of heating, 8 hours film-formings under drying box.
Table 1 is the electrolyte performance table of the embodiment of the present invention.
Table 1
Claims (2)
1. a kind of lithium ion battery polymer electrolyte, which is characterized in that the raw material before crosslinking curing are the end silicon of viscous state
The polyethers performed polymer of alkane sealing end, electric conducting lithium salt, organic solvent and tin catalyst mixture, the described viscous state end silane envelope
The mass fraction that end polyethers accounts for mixture is 10-60%, and the mass fraction that electric conducting lithium salt accounts for mixture is 10-60%, You Jirong
The mass fraction that agent accounts for mixture is 20-70%, and tin catalyst mass fraction is the quality for holding silane-terminated polyether performed polymer
The 0.5-5% of score;Curing time and curing degree are controlled by adjusting tin catalyst content;Electric conducting lithium salt is in following
One or more: LiPF6、LiCF3SO3、LiN(CF3SO2)2、LiN(C2F5SO2)2、LiN(CF3SO2)(C4F9SO2)、LiC
(CF3SO2)3、LiC(C2F5SO2)3、LiAsF6、LiClO4;Organic solvent is one or more of following: ethylene carbonate, carbon
Acid propylene ester, butylene carbonate rouge, dimethyl carbonate, ethylene carbonate, methyl ethyl carbonate, gamma-butyrolacton, tetrahydrofuran, 2- first
Base tetrahydrofuran, acetonitrile, tetraethyleneglycol dimethyl ether, triethylene glycol dimethyl ether, diethylene glycol dimethyl ether, dimethyl sulfoxide;Hold silane
The viscosity of the polyethers performed polymer of sealing end is 5000-30000 centipoise, and holding its end group in silane-terminated polyether is silicon methoxyl group or ethoxy
The silane of base;Electric conducting lithium salt and organic solvent constitute electrolyte, and the concentration of electric conducting lithium salt in the electrolytic solution is 0.1-3mol L-1;
Preparation method includes the following steps: electric conducting lithium salt and organic solvent being made into electric conducting lithium salt electrolyte, and are uniformly mixed;
Weigh corrresponding quality score holds Silante terminated polyethers performed polymer to mix simultaneously uniform stirring with electric conducting lithium salt electrolyte: phase is added
The tin catalyst of mass fraction is answered to stir evenly;The polymer electrolytic mixed liquor stirred evenly is coated to polytetrafluoroethylene (PTFE) mould
It in tool, is heating and curing at 30-80 DEG C, was formed a film according to the amount of the catalyst of use at 2-12 hours.
2. a kind of lithium ion battery polymer electrolyte described in accordance with the claim 1, which is characterized in that tin catalyst be with
One of lower: two (dodecyl sulphur) dibutyl tins, dioctyl tin replace dibutyl tin, dialkyl tin dimaleate, two
Acetic acid dibutyl tin, two mercaptan tin alkyls, dilaurate dibutyl tin, bis- (acetopyruvic acid) dibutyl tins, stannous octoate,
Platinum water catalyst.
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CN108736062A (en) * | 2018-04-28 | 2018-11-02 | 浙江天能能源科技股份有限公司 | A kind of lithium ion battery composite solid electrolyte and preparation method thereof |
CN108899579B (en) * | 2018-06-14 | 2021-03-05 | 北京工业大学 | Preparation of self-crosslinking composite solid electrolyte and all-solid-state lithium ion battery formed by same |
CN108878959B (en) * | 2018-06-14 | 2020-09-25 | 北京工业大学 | Preparation and application of organic-inorganic composite solid electrolyte |
CN111370758B (en) * | 2020-03-16 | 2022-04-05 | 中山大学 | Polymer solid electrolyte based on bulk plasticization principle and preparation method thereof |
CN113437359B (en) * | 2021-05-18 | 2023-04-07 | 长沙矿冶研究院有限责任公司 | Preparation method of polypropylene oxide polymer solid electrolyte film |
CN116082640A (en) * | 2022-12-23 | 2023-05-09 | 中国科学院物理研究所 | Polymer for electrolyte and preparation method and application thereof |
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