CN108110315A - A kind of lithium ion battery self-healing polymers electrolyte preparation method - Google Patents
A kind of lithium ion battery self-healing polymers electrolyte preparation method Download PDFInfo
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- CN108110315A CN108110315A CN201711293196.8A CN201711293196A CN108110315A CN 108110315 A CN108110315 A CN 108110315A CN 201711293196 A CN201711293196 A CN 201711293196A CN 108110315 A CN108110315 A CN 108110315A
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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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- 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
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
The present invention discloses a kind of method for preparing selfreparing gel polymer electrolyte.Comprise the following steps：（1）Dimethyl silicone polymer and Kynoar are added to by acetone and N, in the solvent of N dimethylformamide mixed preparings, ultrasonic dissolution is configured to solution；（2）To step（1）Crosslinking agent mixing is added in acquired solution, obtains mixed solution；（3）By step（2）Solution evaporation solvent, obtains gel；（4）Chloroform ultrasonic dissolution is instilled in gained gel, obtains precursor solution, is coated on glass plate, when standing 5 is small, it is removed into solvent chloroform in air dry oven and obtains polymer film；（5）Resulting polymers film is immersed in liquid electrolyte, swelling activation obtains gel-form solid polymer electrolyte.Present invention process is simple, easy to operation.Prepared selfreparing gel electrolyte can be made into arbitrary shape, and stability is good, and electrical conductivity is high, is had a safety feature compared with conventional lithium ion battery, avoids leakage problem.
Description
Technical field
The present invention relates to the preparation methods of lithium ion battery electrolyte, particularly a kind of lithium ion battery self-healing polymers
Electrolyte preparation method belongs to lithium ion battery preparing technical field.
Background technology
In recent years, people have made great progress in the theoretical research of polymer dielectric and application aspect, prepare, close
Into many different electrolyte.But the polymer dielectric being currently known, room-temperature conductivity is low, in cyclic process, lithium
Dendrite may pass through polymer dielectric film, cause positive and negative electrode short-circuit, and dendrite easily pierces through, these all limit its lithium from
Practical application in sub- battery and power-type lithium ion battery.That improves polymer Li-ion battery performance is critical that apparatus
There are good ionic conductivity, electrochemical stability and the polymer dielectric having a safety feature.It is required that polymer dielectric is being protected
The performances such as excellent ionic conductivity, cyclical stability and chemical stability are obtained on the premise of holding good mechanical properties, are become
The emphasis of research.At present, although gel polymer electrolyte has been applied to merchandized handling, the existing peace of gelatin polymer
The contradiction between performance and ionic conductivity thoroughly solves not yet entirely.How polymer dielectric is keeping good mechanical properties
On the premise of obtain the performances such as excellent ionic conductivity, cyclical stability and chemical stability, become focus of attention.It is existing
Preparation method due to process it is complicated, cost is higher, and gelatin polymer film properties of product are unsatisfactory.
The content of the invention
It is an object of the invention to provide a kind of lithium ion battery self-healing polymers electrolyte preparing methods.
A kind of lithium ion battery self-healing polymers electrolyte preparation method that the present invention provides, comprises the following steps：
（1）By dimethyl silicone polymer（PDMS）It is added to Kynoar (PVdF) by acetone and N,N-dimethylformamide
In the solvent of mixed preparing, in 0~40 DEG C of ultrasonic dissolution, solution is configured to；
（2）To step（1）Crosslinking agent diethylenetriamine is added in acquired solution, mixed solution is obtained after mixing；
（3）By step（2）Gained mixed solution solvent flashing, obtains gel；
（4）In step（3）Chloroform is instilled in gained gel, when ultrasound 0.5~2 is small, gel is made to dissolve to obtain precursor solution, it will
Precursor solution is coated on glass plate, when standing 5 is small, places it in temperature in 60 DEG C of air dry ovens, to remove solvent
Chloroform obtains polymer film；
（5）By step（4）Resulting polymers film is immersed in liquid electrolyte, and swelling activation is adsorbed to saturation, is dried with filter paper more
Remaining electrolyte, you can obtain gel-form solid polymer electrolyte；
Wherein, liquid electrolyte is made of lithium salts and organic solvent, and the lithium salt in liquid electrolyte is 0.1~0.8M；Have
Solvent is by propene carbonate and ethylene carbonate in mass ratio 1：1 is mixed, alternatively, organic solvent selects ethylene carbonate
Ester, diethyl carbonate, propene carbonate, propylene carbonate, vinylene carbonate, dimethyl carbonate, methyl ethyl carbonate, 1,2- bis-
Ethyl Methyl Ether, tetrahydrofuran, dimethyl sulfoxide (DMSO), acetone, N- N-methyl 2-pyrrolidone Ns, N,N-dimethylformamide, N, N- dimethyl
One or more in acetamide.
The preparation method of the present invention, step（1）Middle acetone and n,N-Dimethylformamide preferred mass proportioning are 1：1.
The preparation method of the present invention, step（1）Middle 25 DEG C of preferable temperature.
The preparation method of the present invention, step（4）In preferably ultrasonic time 1 it is small when.
The preparation method of the present invention, step（5）In preferably lithium salt 0.5M.
The preparation method of the present invention, step（5）Described in lithium salts selects in liquid electrolyte is lithium hexafluoro phosphate, high chlorine
Sour lithium, LiBF4, trifluoromethanesulfonic acid lithium, dioxalic acid lithium borate, hexafluoroarsenate lithium lithium iodide, two（Trimethyl fluoride sulfonyl）It is sub-
One kind in amine lithium, but it is preferred that lithium hexafluoro phosphate.
Polymer dielectric is assembled into simulated battery by the present invention, using the electrochemical research such as AC impedance method to synthesis
Polymer dielectric carry out Electrochemical Properties.Positive and negative anodes are placed on above-mentioned gel electrolyte both sides, are assembled into battery.
The present invention provides compound positive and negative electrode material and containing conductive additive, binding agent and coordinative solvent, using painting
Electrode slice is made in slurry processes, the technological process through slurrying, smear, drying.
In prepared by electrode slice, by active material, Super-P, Kynoar according to 7：2：1 ratio weighs, and adds in N-
Methyl pyrrolidone ultrasonic dissolution, is applied to battery case, is dried to obtain electrode slice；In above-mentioned preparation method, the conductive addition
Agent is not limited to the one or more in carbon black, Super-P, Ketjen black；The binding agent and coordinative solvent are not limited to polyvinylidene fluoride
Alkene（PVDF）（With N-Methyl pyrrolidone（NMP）For solvent）Or polyacrylic acid（PAA）, sodium carboxymethylcellulose（CMC）, butylbenzene
Rubber/sodium carboxymethylcellulose, sodium alginate（SA）, gelatin（Using water as solvent）In one or more；It is preferably poly- inclined
Vinyl fluoride（PVDF）（With N-Methyl pyrrolidone（NMP）For solvent）.
What the present invention obtained has the beneficial effect that：
Selfreparing gel electrolyte made of the present invention can be made into arbitrary shape, and plasticity improves, stability
Good, electrical conductivity is high, and mechanical strength is good, is had a safety feature compared with conventional lithium ion battery, avoids leakage problem；Preparation process
Simply, easy to operation, with short production cycle, the feature of environmental protection is good.
Description of the drawings
Fig. 1 is the repairing performance figure of selfreparing gel electrolyte prepared by embodiment 1.
Fig. 2 is the electrochemical window figure of selfreparing gel electrolyte prepared by embodiment 1.
Fig. 3-A are the impedance diagram of selfreparing gel electrolyte different temperatures prepared by embodiment 1（Temperature is 20 DEG C）.
Fig. 3-B are the impedance diagrams of the selfreparing gel electrolyte different temperatures prepared for embodiment 1（Temperature is 65 DEG C）.
Fig. 4 is that selfreparing gel electrolyte ionic conductivity prepared by embodiment 1 varies with temperature curve.
Specific embodiment
Following embodiment does not limit the present invention for illustrating the present invention.
It needs to prompt, the experimental method in all embodiments, is conventional method unless otherwise specified, used examination
Agent and material unless otherwise specified, commercially obtain.
Embodiment 1 prepares gel electrolyte
（1）By dimethyl silicone polymer（PDMS）It is added to Kynoar (PVdF) by acetone and N,N-dimethylformamide
In the solvent of mixed preparing, under the conditions of 25 DEG C, ultrasonic dissolution is configured to solution；
（2）To step（1）Crosslinking agent is added in acquired solution（Diethylenetriamine）Mixing；
（3）By step（2）Mixed solution evaporation removes solvent, obtains gel；
（4）By step（3）Middle gained gel is put into the centrifuge tube of 5ml, is instilled 1ml chloroforms, when ultrasound 1.5 is small, is made its dissolving
After obtain precursor solution, be coated on glass plate, after standing 5 hours, place it in temperature and done for 60 DEG C of air blast
Solvent chloroform is removed in dry case and obtains polymer film；
（5）By step（4）Resulting polymers film is immersed in liquid electrolyte, and swelling activation is adsorbed to saturation, is dried with filter paper more
Remaining electrolyte, you can obtain gel-form solid polymer electrolyte.
The liquid electrolyte, is made of lithium salts and organic solvent, and lithium salts is lithium hexafluoro phosphate, concentration 0.5M；It is organic
Solvent is by agent propene carbonate and ethylene carbonate mixing by 1：1 quality proportioning is made.
Polymer dielectric is gone out into shape with the punching pin of a diameter of 19mm, is scraped from glass mold it using blade
It rises, using vernier caliper measurement polymer thickness, scope is generally 100-400 nm, is preferably 100-200nm.
Stainless steel mould is placed to polymer dielectric both sides obtained respectively, simulated battery application exchange is assembled into and hinders
The electrochemical research methods such as anti-, electrochemical workstation linear scan carry out chemical property to the polymer dielectric of synthesis and grind
Study carefully, simulated battery shows good performance.
Alternating current impedance instrument, test frequency are from low to high：0.1Hz-100 KHz
Linear scan section is 0 V-5 V；Speed is swept as 5 mV/s
Use transmission electron microscope（TEM, Tecnai F30, operating voltage are 200 kV）Characterization gained sample particle diameter scale is big
It is small.
Scanning electron microscope (SEM S4800) analyzes the microscopic appearance of sample
X-ray diffraction (XRD) carries out qualitative analysis to sample
The analysis of high-resolution-ration transmission electric-lens (HRTEM) sample inner structure, lattice diffraction
The present invention provide positive and negative electrode material preparation, by active material with carbon black, binding agent polyvinylidene fluoride in mass ratio
7:2:1 mixing, and add in solvent N-methyl pyrilidone, obtain composite electrode through technological processes such as slurrying, smear, dryings
Material.
Electrode material is placed to gel polymer electrolyte both sides respectively, is assembled into battery.Using charge and discharge instrument to above-mentioned
This battery carries out constant current charge-discharge test, and cyclic voltammetry is carried out to above-mentioned battery using electrochemical workstation.
Embodiment 2 prepares gel electrolyte
Difference from Example 1 is dimethyl silicone polymer（PDMS）Mass ratio with Kynoar (PVdF) is 1：
0.5, other conditions are same as Example 1.The gel polymer electrolyte of preparation is carried out by the test method of embodiment 1.
Embodiment 3 prepares gel electrolyte
Difference from Example 1 is dimethyl silicone polymer（PDMS）Mass ratio with Kynoar (PVdF) is 2：0.8,
Other conditions are same as Example 1.The gel polymer electrolyte of preparation is carried out by the test method of embodiment 1.
Embodiment 4 prepares gel electrolyte
Dimethyl silicone polymer as different from Example 1（PDMS）Mass ratio with Kynoar (PVdF) is 1：2, it is other
Condition is same as Example 1.Prepared gel polymer electrolyte is carried out by the test method of embodiment 1.
Embodiment 5 prepares gel electrolyte
Plasticizer acetone and N,N-dimethylformamide mixing match are 1 as different from Example 1:3 are made, other conditions with
Embodiment 1 is identical.Prepared gel polymer electrolyte is carried out by the test method of embodiment 1.
Embodiment 6 prepares gel electrolyte
Plasticizer acetone and N,N-dimethylformamide mixing match are 1.5 as different from Example 1:3 are made, other conditions
It is same as Example 1.Prepared gel polymer electrolyte is carried out by the test method of embodiment 1.
From above-described embodiment as can be seen that the selfreparing gel polymer electrolyte for preparing of the present invention have high conductivity,
High electrochemical stability and the performance of self-regeneration, avoid leakage safety issue, have a good application prospect.
Claims (6)
1. a kind of lithium ion battery self-healing polymers electrolyte preparation method, it is characterised in that comprise the following steps：
（1）By dimethyl silicone polymer（PDMS）It is added to Kynoar (PVdF) by acetone and N,N-dimethylformamide
In the solvent of mixed preparing, in 0~40 DEG C of ultrasonic dissolution, solution is configured to；
（2）To step（1）Crosslinking agent diethylenetriamine is added in acquired solution, mixed solution is obtained after mixing；
（3）By step（2）Gained mixed solution solvent flashing, obtains gel；
（4）In step（3）Chloroform is instilled in gained gel, when ultrasound 0.5~2 is small, gel is made to dissolve to obtain precursor solution, it will
Precursor solution is coated on glass plate, when standing 5 is small, places it in temperature in 60 DEG C of air dry ovens, to remove solvent
Chloroform obtains polymer film；
（5）By step（4）Resulting polymers film is immersed in liquid electrolyte, and swelling activation is adsorbed to saturation, is dried with filter paper more
Remaining electrolyte, you can obtain gel-form solid polymer electrolyte；
Wherein, liquid electrolyte is made of lithium salts and organic solvent, and the lithium salt in liquid electrolyte is 0.1~0.8M；Have
Solvent is by propene carbonate and ethylene carbonate in mass ratio 1：1 is mixed, alternatively, organic solvent selects ethylene carbonate
Ester, diethyl carbonate, propene carbonate, propylene carbonate, vinylene carbonate, dimethyl carbonate, methyl ethyl carbonate, 1,2- bis-
Ethyl Methyl Ether, tetrahydrofuran, dimethyl sulfoxide (DMSO), acetone, N- N-methyl 2-pyrrolidone Ns, N,N-dimethylformamide, N, N- dimethyl
One or more in acetamide.
2. preparation method according to claim 1, it is characterised in that step（1）Middle acetone and n,N-Dimethylformamide matter
Amount proportioning is 1：1.
3. preparation method according to claim 1, it is characterised in that step（1）25 DEG C of temperature.
4. preparation method according to claim 1, it is characterised in that step（4）When middle ultrasonic time 1 is small.
5. preparation method according to claim 1, it is characterised in that step（5）Middle lithium salt 0.5M.
6. preparation method according to claim 1, it is characterised in that step（5）Lithium salts is hexafluoro phosphorus in middle liquid electrolyte
Sour lithium.
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Cited By (6)
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| CN110571471A (en) * | 2019-09-27 | 2019-12-13 | 河北师范大学 | preparation method and application of solid electrolyte with post-wound rapid healing capacity |
| CN110690062A (en) * | 2019-10-21 | 2020-01-14 | 山东科技大学 | Preparation method of polyacrylic acid flexible composite hydrogel electrolyte |
| CN112259915A (en) * | 2020-09-25 | 2021-01-22 | 横店集团东磁股份有限公司 | Battery composite diaphragm and preparation method and application thereof |
| CN113506917A (en) * | 2021-06-29 | 2021-10-15 | 五邑大学 | Preparation method of self-repairing polymer electrolyte of lithium ion battery |
| CN114497748A (en) * | 2022-01-07 | 2022-05-13 | 上海工程技术大学 | Cellulose self-repairing gel electrolyte material and preparation method and application thereof |
| CN116154280A (en) * | 2023-04-23 | 2023-05-23 | 远景动力技术(鄂尔多斯市)有限公司 | Gel electrolyte of lithium battery and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110571471A (en) * | 2019-09-27 | 2019-12-13 | 河北师范大学 | preparation method and application of solid electrolyte with post-wound rapid healing capacity |
| CN110571471B (en) * | 2019-09-27 | 2022-12-09 | 河北师范大学 | Preparation method and application of solid electrolyte with post-wound rapid healing capacity |
| CN110690062A (en) * | 2019-10-21 | 2020-01-14 | 山东科技大学 | Preparation method of polyacrylic acid flexible composite hydrogel electrolyte |
| CN112259915A (en) * | 2020-09-25 | 2021-01-22 | 横店集团东磁股份有限公司 | Battery composite diaphragm and preparation method and application thereof |
| CN113506917A (en) * | 2021-06-29 | 2021-10-15 | 五邑大学 | Preparation method of self-repairing polymer electrolyte of lithium ion battery |
| CN114497748A (en) * | 2022-01-07 | 2022-05-13 | 上海工程技术大学 | Cellulose self-repairing gel electrolyte material and preparation method and application thereof |
| CN114497748B (en) * | 2022-01-07 | 2023-08-29 | 上海工程技术大学 | Cellulose self-repairing gel electrolyte material and preparation method and application thereof |
| CN116154280A (en) * | 2023-04-23 | 2023-05-23 | 远景动力技术(鄂尔多斯市)有限公司 | Gel electrolyte of lithium battery and application thereof |
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