CN108110315B - Preparation method of self-repairing polymer electrolyte of lithium ion battery - Google Patents
Preparation method of self-repairing polymer electrolyte of lithium ion battery Download PDFInfo
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- CN108110315B CN108110315B CN201711293196.8A CN201711293196A CN108110315B CN 108110315 B CN108110315 B CN 108110315B CN 201711293196 A CN201711293196 A CN 201711293196A CN 108110315 B CN108110315 B CN 108110315B
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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 invention discloses a method for preparing a self-repairing gel polymer electrolyte. The method comprises the following steps: (1) adding polydimethylsiloxane and polyvinylidene fluoride into a solvent prepared by mixing acetone and N, N-dimethylformamide, and dissolving by ultrasonic to prepare a solution; (2) adding a cross-linking agent into the solution obtained in the step (1) and mixing to obtain a mixed solution; (3) volatilizing the solvent from the solution in the step (2) to obtain gel; (4) dripping chloroform into the gel, performing ultrasonic dissolution to obtain a precursor solution, suspending the precursor solution on a glass plate, standing for 5 hours, and removing the solvent chloroform from the precursor solution in a forced air drying oven to obtain a polymer film; (5) and immersing the obtained polymer film into liquid electrolyte, and swelling and activating to obtain the polymer gel electrolyte. The invention has simple process and convenient operation. The prepared self-repairing gel electrolyte can be made into any shape, has good stability and high conductivity, has better safety performance than the traditional lithium ion battery, and avoids the problem of liquid leakage.
Description
Technical Field
The invention relates to a preparation method of a lithium ion battery electrolyte, in particular to a preparation method of a lithium ion battery self-repairing polymer electrolyte, belonging to the technical field of lithium ion battery preparation.
Background
In recent years, people have made great progress in theoretical research and application of polymer electrolytes, and a plurality of different electrolytes are prepared and synthesized. However, the currently known polymer electrolytes have low room temperature conductivity, lithium dendrites may penetrate through a polymer electrolyte membrane during cycling, the positive electrode and the negative electrode are short-circuited, and the dendrites are easily punctured, which limits the practical application of the polymer electrolytes in lithium ion batteries and power lithium ion batteries. The key to improve the performance of the polymer lithium ion battery is to use a polymer electrolyte with good ionic conductivity, electrochemical stability and safety performance. The polymer electrolyte is required to obtain excellent ionic conductivity, cycling stability, chemical stability and other properties on the premise of keeping good mechanical properties, and becomes a key point of research. At present, although gel polymer electrolytes have been applied to commercial production, the contradiction between safety performance and ionic conductivity of gel polymers has not been completely solved. How to obtain excellent ionic conductivity, cycling stability, chemical stability and other properties of the polymer electrolyte on the premise of maintaining good mechanical properties becomes a focus of attention. The existing preparation method has the disadvantages of complex process and high cost, and the performance of the gel polymer membrane product is unsatisfactory.
Disclosure of Invention
The invention aims to provide a preparation method of a self-repairing polymer electrolyte of a lithium ion battery.
The invention provides a preparation method of a lithium ion battery self-repairing polymer electrolyte, which comprises the following steps:
(1) adding Polydimethylsiloxane (PDMS) and polyvinylidene fluoride (PVdF) into a solvent prepared by mixing acetone and N, N-dimethylformamide, and ultrasonically dissolving at 0-40 ℃ to prepare a solution;
(2) adding a cross-linking agent diethylenetriamine into the solution obtained in the step (1), and mixing to obtain a mixed solution;
(3) volatilizing the solvent from the mixed solution obtained in the step (2) to obtain gel;
(4) dripping chloroform into the gel obtained in the step (3), performing ultrasonic treatment for 0.5-2 hours to dissolve the gel to obtain a precursor solution, suspending and coating the precursor solution on a glass plate, standing for 5 hours, placing the glass plate in a forced air drying oven at the temperature of 60 ℃, and removing the solvent chloroform to obtain a polymer film;
(5) immersing the polymer membrane obtained in the step (4) into liquid electrolyte, swelling and activating, adsorbing until saturation, and wiping redundant electrolyte with filter paper to obtain a polymer gel electrolyte;
the liquid electrolyte consists of lithium salt and an organic solvent, and the concentration of the lithium salt in the liquid electrolyte is 0.1-0.8M; the organic solvent is prepared from propylene carbonate and ethylene carbonate according to the mass ratio of 1: 1 or the organic solvent is one or more of ethylene carbonate, diethyl carbonate, propylene carbonate, vinylene carbonate, dimethyl carbonate, methyl ethyl carbonate, 1, 2-dimethoxyethane, tetrahydrofuran, dimethyl sulfoxide, acetone, N-methylpyrrolidone, N-dimethylformamide and N, N-dimethylacetamide.
In the preparation method, in the step (1), the preferable mass ratio of the acetone to the N, N-dimethylformamide is 1: 1.
in the production process of the present invention, the temperature in step (1) is preferably 25 ℃.
In the preparation method of the invention, the ultrasonic treatment time in the step (4) is preferably 1 hour.
In the preparation method of the present invention, the lithium salt concentration in step (5) is preferably 0.5M.
In the preparation method of the present invention, the lithium salt in the liquid electrolyte in step (5) is selected from one of lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium trifluoromethanesulfonate, lithium dioxalate borate, lithium hexafluoroarsenate iodide and lithium bis (trifluoromethylsulfonyl) imide, but is preferably selected from lithium hexafluorophosphate.
The polymer electrolyte is assembled into a simulated battery, and electrochemical performance of the synthesized polymer electrolyte is researched by applying electrochemical research methods such as alternating current impedance and the like. And placing the positive electrode and the negative electrode on two sides of the gel electrolyte to assemble the battery.
The invention provides a composite anode material and cathode material, and electrode slice prepared by using a coating method and through the process flows of pulping, smearing and drying, wherein the composite anode material and cathode material contain conductive additives, binders and corresponding solvents.
In the preparation of the electrode slice, the active substance, Super-P and polyvinylidene fluoride are mixed according to the weight ratio of 7:2:1, adding N-methyl pyrrolidone for ultrasonic dissolution, smearing on a battery shell, and drying to obtain an electrode plate; in the preparation method, the conductive additive is not limited to one or more of carbon black, Super-P and Ketjen black; the binder and the corresponding solvent are not limited to polyvinylidene fluoride (PVDF) (N-methylpyrrolidone (NMP) is used as a solvent) or one or more of polyacrylic acid (PAA), sodium carboxymethyl cellulose (CMC), styrene butadiene rubber/sodium carboxymethyl cellulose, Sodium Alginate (SA) and gelatin (water is used as a solvent); polyvinylidene fluoride (PVDF) is preferred (N-methylpyrrolidone (NMP) is used as solvent).
The invention has the following beneficial effects:
the self-repairing gel electrolyte prepared by the invention can be prepared into any shape, the plasticity is improved, and the stability is improved
The lithium ion battery has the advantages of good conductivity, high mechanical strength, better safety performance than the traditional lithium ion battery, and avoidance of liquid leakage; the preparation process is simple, convenient to operate, short in production period and good in environmental protection.
Drawings
Fig. 1 is a graph of the repair performance of the self-healing gel electrolyte prepared in example 1.
Fig. 2 is an electrochemical window diagram of a self-healing gel electrolyte prepared in example 1.
FIG. 3-A is an impedance plot of the self-healing gel electrolyte prepared in example 1 at various temperatures (20 deg.C).
FIG. 3-B is an impedance plot (65 ℃ C.) for various temperatures of the self-healing gel electrolyte prepared in example 1.
Fig. 4 is a curve of ion conductivity versus temperature for the self-healing gel electrolyte prepared in example 1.
Detailed Description
The following examples are intended to illustrate the invention without, however, limiting it.
It should be noted that the experimental procedures used in all the examples, unless otherwise specified, were conventional and that the reagents and materials used, unless otherwise specified, were commercially available.
Example 1 preparation of gel electrolyte
(1) Adding Polydimethylsiloxane (PDMS) and polyvinylidene fluoride (PVdF) into a solvent prepared by mixing acetone and N, N-dimethylformamide, and ultrasonically dissolving at 25 ℃ to prepare a solution;
(2) adding a cross-linking agent (diethylenetriamine) into the solution obtained in the step (1) and mixing;
(3) volatilizing the mixed solution obtained in the step (2) to remove the solvent to obtain gel;
(4) putting the gel obtained in the step (3) into a 5ml centrifugal tube, dripping 1ml chloroform, performing ultrasonic treatment for 1.5 hours to dissolve the gel to obtain a precursor solution, hanging the precursor solution on a glass plate, standing for 5 hours, and placing the precursor solution in a forced air drying oven at the temperature of 60 ℃ to remove the chloroform solvent to obtain a polymer film;
(5) and (4) immersing the polymer membrane obtained in the step (4) into liquid electrolyte, swelling and activating, adsorbing until the polymer membrane is saturated, and wiping the redundant electrolyte by using filter paper to obtain the polymer gel electrolyte.
The liquid electrolyte consists of lithium salt and an organic solvent, wherein the lithium salt is lithium hexafluorophosphate and has the concentration of 0.5M; the organic solvent is prepared by mixing propylene carbonate and ethylene carbonate according to the proportion of 1: 1, and the weight ratio is 1.
The polymer electrolyte is punched out of shape with a punch having a diameter of 19mm, scraped from the glass mold using a blade, and the polymer thickness is measured using a vernier caliper, generally in the range of 100-.
The stainless steel dies are respectively placed on two sides of the prepared polymer electrolyte to assemble a simulated battery, and the electrochemical performance of the synthesized polymer electrolyte is researched by applying electrochemical research methods such as alternating current impedance, electrochemical workstation linear scanning and the like, so that the simulated battery shows good performance.
The alternating-current impedance instrument has the following testing frequency from low frequency to high frequency: 0.1Hz-100 KHz
The linear scanning interval is 0V-5V; the sweeping speed is 5 mV/s
The particle size dimensions of the resulting samples were characterized by transmission electron microscopy (TEM, Tecnai F30, 200 kV operating voltage).
Analysis of the microscopic morphology of the samples by scanning Electron microscopy (SEM S4800)
Qualitative analysis of the samples by X-ray diffraction (XRD)
High Resolution Transmission Electron Microscopy (HRTEM) in-sample structural analysis, lattice diffraction
The invention provides a preparation method of a positive electrode material and a negative electrode material, which comprises the steps of mixing an active material, carbon black and a binding agent polyvinylidene fluoride according to the mass ratio of 7:2:1, adding a solvent N-methyl pyrrolidone, and carrying out pulping, smearing, drying and other process flows to obtain the composite electrode material.
And respectively placing the electrode materials on two sides of the gel polymer electrolyte to assemble the battery. And carrying out constant-current charge and discharge test on the battery by using a charge and discharge instrument, and carrying out cyclic volt-ampere test on the battery by using an electrochemical workstation.
Example 2 preparation of gel electrolyte
The difference from example 1 is that the mass ratio of Polydimethylsiloxane (PDMS) to polyvinylidene fluoride (PVdF) is 1: 0.5, and the other conditions were the same as in example 1. The prepared gel polymer electrolyte was subjected to the test method of example 1.
Example 3 preparation of gel electrolyte
The difference from the example 1 is that the mass ratio of the Polydimethylsiloxane (PDMS) to the polyvinylidene fluoride (PVdF) is 2: 0.8, and the other conditions were the same as in example 1. The prepared gel polymer electrolyte was subjected to the test method of example 1.
Example 4 preparation of gel electrolyte
Different from example 1, the mass ratio of Polydimethylsiloxane (PDMS) to polyvinylidene fluoride (PVdF) was 1: the other conditions were the same as in example 1. The prepared gel polymer electrolyte was subjected to the test method of example 1.
Example 5 preparation of gel electrolyte
The difference from the example 1 is that the plasticizer acetone and the N, N-dimethylformamide are mixed in the ratio of 1:3, and the other conditions are the same as the example 1. The prepared gel polymer electrolyte was subjected to the test method of example 1.
Example 6 preparation of gel electrolyte
The difference from the example 1 is that the plasticizer acetone and N, N-dimethylformamide are mixed in the ratio of 1.5:3, and the other conditions are the same as the example 1. The prepared gel polymer electrolyte was subjected to the test method of example 1.
The self-repairing gel polymer electrolyte prepared by the invention has high conductivity, high electrochemical stability and self-repairing performance, avoids the problem of leakage safety, and has a good application prospect.
Claims (6)
1. A preparation method of a self-repairing polymer electrolyte of a lithium ion battery is characterized by comprising the following steps:
(1) adding Polydimethylsiloxane (PDMS) and polyvinylidene fluoride (PVdF) into a solvent prepared by mixing acetone and N, N-dimethylformamide, and ultrasonically dissolving at 0-40 ℃ to prepare a solution;
(2) adding a cross-linking agent diethylenetriamine into the solution obtained in the step (1), and mixing to obtain a mixed solution;
(3) volatilizing the solvent from the mixed solution obtained in the step (2) to obtain gel;
(4) dripping chloroform into the gel obtained in the step (3), performing ultrasonic treatment for 0.5-2 hours to dissolve the gel to obtain a precursor solution, suspending and coating the precursor solution on a glass plate, standing for 5 hours, placing the glass plate in a forced air drying oven at the temperature of 60 ℃, and removing the solvent chloroform to obtain a polymer film;
(5) immersing the polymer membrane obtained in the step (4) into liquid electrolyte, swelling and activating, adsorbing until saturation, and wiping redundant electrolyte with filter paper to obtain a polymer gel electrolyte;
the liquid electrolyte consists of lithium salt and an organic solvent, and the concentration of the lithium salt in the liquid electrolyte is 0.1-0.8M; the organic solvent is prepared from propylene carbonate and ethylene carbonate according to the mass ratio of 1: 1, mixing to obtain the product; or the organic solvent is one or more of diethyl carbonate, propylene carbonate, vinylene carbonate, dimethyl carbonate, ethyl methyl carbonate, 1, 2-dimethoxyethane, tetrahydrofuran, dimethyl sulfoxide, acetone, N-methylpyrrolidone, N-dimethylformamide and N, N-dimethylacetamide.
2. The preparation method according to claim 1, wherein the mass ratio of acetone to N, N-dimethylformamide in step (1) is 1: 1.
3. the method according to claim 1, wherein the temperature in step (1) is 25 ℃.
4. The method according to claim 1, wherein the sonication time in step (4) is 1 hour.
5. The method according to claim 1, wherein the lithium salt concentration in the step (5) is 0.5M.
6. The method according to claim 1, wherein the lithium salt in the liquid electrolyte in the step (5) is lithium hexafluorophosphate.
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| 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 |
| CN110690062B (en) * | 2019-10-21 | 2021-05-28 | 山东科技大学 | Preparation method of polyacrylic acid flexible composite hydrogel electrolyte |
| CN112259915B (en) * | 2020-09-25 | 2022-07-12 | 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 |
| 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 |
| CN116154280B (en) * | 2023-04-23 | 2023-08-01 | 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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