CN105489932A - Method for preparing polymer electrolyte film for lithium-ion battery by ultraviolet crosslinking assay - Google Patents
Method for preparing polymer electrolyte film for lithium-ion battery by ultraviolet crosslinking assay Download PDFInfo
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- CN105489932A CN105489932A CN201510899142.0A CN201510899142A CN105489932A CN 105489932 A CN105489932 A CN 105489932A CN 201510899142 A CN201510899142 A CN 201510899142A CN 105489932 A CN105489932 A CN 105489932A
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- Prior art keywords
- film
- liquid
- lithium
- polymer electrolyte
- electrolyte film
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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
-
- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for preparing a polymer electrolyte film for a lithium-ion battery by an ultraviolet crosslinking assay, relates to a method for preparing a film, and aims at solving the problems that a liquid electrolyte in an existing lithium-ion battery is easy to leak and has a potential safety hazard, and an all-solid-state electrolyte film is low in conductivity. The method provided by the invention comprises the following steps: (1) carrying out drying treatment on BPO and EDMA; (2) weighing a methyl methacrylate (MMA) monomer and an initiator, and mixing and stirring the MMA monomer and the initiator; (3) weighing urethane acrylate (PUA), an ionic liquid, a crosslinking agent and a lithium salt, and carrying out constant-temperature heating, mixing and stirring; (4) mixing the solution obtained in the step (2) with the solution obtained in the step (3), and adding a solvent for stirring; and (5) casting the mixed solution into a film, carrying out irradiating by an ultraviolet curing lamp to form the film. The electrolyte film prepared by the method has good ionic conductivity, electrochemical capacity and thermodynamic stability and relatively high mechanical property; and improvement of the safety performance of the lithium-ion battery is facilitated.
Description
Technical field
The present invention relates to a kind of method preparing lithium ionic cell polymer electrolyte film.
Background technology
The energy problem day by day consumed is one of focus of paying close attention to most of our times, and existing energy sources and fossil are just increasingly exhausted, and in addition, the greenhouse gas that fossil energy produces and the waste that imperfect combustion produces are all the huge challenges to human development.Therefore, wind energy, solar energy, nuclear energy, biological energy source, the development and utilization of the clean alternative energy such as electric energy is just growing.Lithium ion battery is that one has high-energy-density, high coulombic efficiency, long circulation life, the high energy green power supply of stable charge/discharge, along with the development of science and technology and the intensification of exploration, each part of lithium ion battery has had the development of advancing by leaps and bounds, and is wherein very with electrolyte.
Electrolyte by liquid electrolyte to safer, mechanical property is better, the future development that thermodynamics is more stable.Polymer dielectric because of ionic liquid add be provided with the high conductivity suitable with liquid electrolyte and and the wetability of electrode good contact, again because becoming the focus of research after film-forming without flowable state liquid initiation potential safety hazard.So the selection of ionic liquid is the whole electrolyte system key factor of impact.Preparing a kind ofly has the polymer dielectric film of good ionic conductivity, electrochemistry, thermodynamic stability and higher mechanical performance to be improve the key of polymer Li-ion battery
UV-crosslinked method is adopted to take methyl acrylate as raw material monomer, add appropriate light trigger, by UV-irradiation, the ultraviolet light being absorbed specific wavelength by light trigger causes generation methyl methacrylate free radical, thus there is the reaction of a series of rapid polymerization, produce and there is cancellated polymethyl methacrylate, through crosslinked polyester material, there is excellent high temperature resistant type, solvent resistance, excellent chemical property and the mechanical property significantly strengthened.
Summary of the invention
The object of the invention is the method in order to find the efficient lithium ionic cell polymer electrolyte film of a kind of simple and easy to do preparation, the invention provides the method for a kind of UV-crosslinked legal system for lithium ionic cell polymer electrolyte film.
UV-crosslinked legal system of the present invention for the method for lithium ionic cell polymer electrolyte film,
It comprises the steps:
Step one: by dibenzoyl peroxide (BPO) before using, ethylene glycol dimethacrylate (EDMA), dry process.
Step 2: by methyl methacrylate (MMA) monomer, BPO is according to certain mass than after mixing, and vigorous stirring 20-30min, until stir.
Step 3: by urethane acrylate (PUA), the two fluoroform sulfimide (DEEYTFSI) of ionic liquid diethyl methyl ether base first ammonium, EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir.
Step 4: liquid mixing step 2 and step 3 obtained, add appropriate solvent DMF (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
Step 5: by the solution casting that mixes on the glass plate of cleaning, utilize ultra-violet curing light irradiation 6-8min, obtain DEEYTFSI/PUA/PMMA type ion liquid polymer dielectric film.
Step 6: by urethane acrylate (PUA), the two fluoroform sulfimide (Py of ionic liquid N-Methyl-N-propyl pyrrolidines
13tFSI), EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir.
Step 7: liquid mixing step 2 and step 6 obtained, add appropriate solvent DMF (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
Step 8: repeat step 5, obtain Py
13tFSI/PUA/PMMA type ion liquid polymer dielectric film.
Step 9: to be become by the barrier film blunderbuss of preparation diameter to be the disk of 16mm with circular hole blunderbuss.
The invention has the advantages that, UV-crosslinked curing process is adopted to prepare lithium ion polymer electrolyte film, utilize ultraviolet moment energy high temperature, MMA is made to become PMMA under the effect of crosslinking agent, uncrosslinked MMA monomer can play the effect of pore-creating because of its effumability, reduces the volatilization in operation of MMA monomer.Simultaneously easy and simple to handle, cost is lower, and the film pliability of preparation is good, can reach 2.76 × 10 for DEEYTFSI/PUA/PMMA type ion liquid polymer dielectric film room-temperature conductivity
-4scm
-1, the apparent activation energy E obtained
afor 9.174KJmol
-1; Py
13tFSI/PUA/PMMA type ion liquid polymer dielectric film room-temperature conductivity can reach 1.37 × 10
-3scm
-1, E
afor 7.907KJmol
-1.
Accompanying drawing explanation
Accompanying drawing explanation
Fig. 1 is DEEYTFSI/PUA/PMMA film macrograph;
Fig. 2 is the cyclic voltammogram of DEEYTFSI/PUA/PMMA battery;
Fig. 3 is the impedance diagram of DEEYTFSI/PUA/PMMA battery;
Fig. 4 is the activation energy of DEEYTFSI/PUA/PMMA film;
Fig. 5 is the cycle performance of DEEYTFSI/PUA/PMMA battery;
Fig. 6 is Py
13tFSI/PUA/PMMA film macrograph;
Fig. 7 is Py
13the cyclic voltammogram of TFSI/PUA/PMMA battery;
Fig. 8 is Py
13the impedance diagram of TFSI/PUA/PMMA battery;
Fig. 9 is Py
13the activation energy of TFSI/PUA/PMMA film;
Figure 10 is Py
13the charge and discharge electrograph of TFSI/PUA/PMMA battery;
Figure 11 is Py
13the cycle performance figure of TFSI/PUA/PMMA battery.
Embodiment
Embodiment one: the UV-crosslinked legal system described in present embodiment is for the method for lithium ionic cell polymer electrolyte film.
It comprises the steps:
Step one: by BPO, EDMA before using, dry process.
Step 2: by methyl methacrylate (MMA) monomer, BPO is according to certain mass than after mixing, and vigorous stirring 20-30min, until stir.
Step 3: by urethane acrylate (PUA), ionic liquid, EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir.
Step 4: liquid mixing step 2 and step 3 obtained, add appropriate solvent DMF (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
Step 5: by the solution casting that mixes on the glass plate of cleaning, utilize ultra-violet curing light irradiation 6-8min film forming, obtain DEEYTFSI/PUA/PMMA type ion liquid polymer dielectric film.
Step 6: by urethane acrylate (PUA), the two fluoroform sulfimide (Py of ionic liquid N-Methyl-N-propyl pyrrolidines
13tFSI), EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir.
Step 7: liquid mixing step 2 and step 6 obtained, add appropriate solvent DMF (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
Step 8: repeat step 5, obtain Py
13tFSI/PUA/PMMA type ion liquid polymer dielectric film.Step 9: to be become by the barrier film blunderbuss of preparation diameter to be the disk of 16mm with circular hole blunderbuss.
All stirring operations of present embodiment carry out in measuring cup, prevent from falling into the impurity effect experiment effects such as dust;
Adopt the battery electrochemical stable in properties that the film of step 6 is dressed up in present embodiment, cycle efficieny decay is little, and cyclic voltammetric is good, and DEEYTFSI/PUA/PMMA type ion liquid polymer dielectric film room-temperature conductivity can reach 2.76 × 10
-4scm
-1,, Py
13tFSI/PUA/PMMA type ion liquid polymer dielectric film room-temperature conductivity can reach 1.37 × 10
-3scm
-1.
Embodiment two: present embodiment is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film, described step 2 is: by methyl methacrylate (MMA) monomer, BPO is according to after the mixing of certain mass ratio, vigorous stirring 20-30min, until stir.
Embodiment three: present embodiment is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film, described step 3 is: by urethane acrylate (PUA), ionic liquid, EDMA and lithium salts press certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, vigorous stirring 1h, until stir.
Embodiment four: present embodiment is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film, described step 4 is: liquid mixing step 2 and step 3 obtained, add appropriate solvent N, dinethylformamide (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
Embodiment five: present embodiment is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film, described step 5 is: step 5: by the solution casting that mixes on the glass plate of cleaning, utilize ultra-violet curing light irradiation 6-8min film forming, obtain DEEYTFSI/PUA/PMMA type ion liquid polymer dielectric film.
Embodiment six: present embodiment is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film, described step 6 is: by urethane acrylate (PUA), the two fluoroform sulfimide (Py of ionic liquid N-Methyl-N-propyl pyrrolidines
13tFSI), EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir.
Embodiment seven: present embodiment is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film, described step 7 is: liquid mixing step 2 and step 6 obtained, add appropriate solvent N, dinethylformamide (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
Embodiment eight: present embodiment is that described step 8 is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film: repeat step 5, obtain Py
13tFSI/PUA/PMMA type ion liquid polymer dielectric film.
Embodiment nine: present embodiment is that described step 9 is to the further illustrating of method of the UV-crosslinked legal system described in embodiment one for lithium ionic cell polymer electrolyte film: to be become by the barrier film blunderbuss of preparation diameter to be the disk of 16mm with circular hole blunderbuss.
Claims (9)
1. UV-crosslinked legal system is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that,
Step one: by dibenzoyl peroxide (BPO) before using, ethylene glycol dimethacrylate (EDMA), dry process;
Step 2: by methyl methacrylate (MMA) monomer, BPO is according to certain mass than after mixing, and vigorous stirring 20-30min, until stir;
Step 3: by urethane acrylate (PUA), the two fluoroform sulfimide (DEEYTFSI) of ionic liquid diethyl methyl ether base first ammonium, EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir;
Step 4: the liquid mixing that step 2 and step 3 are obtained, add appropriate solvent DMF (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous;
Step 5: by the solution casting that mixes on the glass plate of cleaning, utilize ultra-violet curing light irradiation 6-8min film forming, obtain DEEYTFSI/PUA/PMMA type ion liquid polymer dielectric film;
Step 6: by urethane acrylate (PUA), the two fluoroform sulfimide (Py of ionic liquid N-Methyl-N-propyl pyrrolidines
13tFSI), EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C-70 DEG C, and vigorous stirring 1h, until stir;
Step 7: the liquid mixing that step 2 and step 6 are obtained, add appropriate solvent DMF (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous;
Step 8: repeat step 5, obtain Py
13tFSI/PUA/PMMA type ion liquid polymer dielectric film;
Step 9: to be become by the barrier film blunderbuss of preparation diameter to be the disk of 16mm with circular hole blunderbuss.
2. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 2 is: by methyl methacrylate (MMA) monomer, and BPO is according to after the mixing of certain mass ratio, vigorous stirring 20-30min, until stir.
3. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 3 is: by urethane acrylate (PUA), ionic liquid, EDMA and lithium salts press certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, vigorous stirring 1h, until stir.
4. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 4 is: liquid mixing step 2 and step 3 obtained, add appropriate solvent N, dinethylformamide (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
5. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 5 is: by the solution casting that mixes on the glass plate of cleaning, utilize ultra-violet curing light irradiation 6-8min film forming.
6. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 6 is: by urethane acrylate (PUA), the two fluoroform sulfimide (Py of ionic liquid N-Methyl-N-propyl pyrrolidines
13tFSI), EDMA and lithium salts are by certain quality than Hybrid Heating 60 DEG C ~ 70 DEG C, and vigorous stirring 1h, until stir.
7. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 7 is: liquid mixing step 2 and step 6 obtained, add appropriate solvent N, dinethylformamide (DMF), vigorous stirring 20-25min, obtains the liquid of transparent and homogeneous.
8. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 8 is: repeat step 5, obtain film 2.
9. UV-crosslinked legal system according to claim 1 is for the method for lithium ionic cell polymer electrolyte film, it is characterized in that, described step 9 is: to be become by the barrier film blunderbuss of preparation diameter to be the disk of 16mm with circular hole blunderbuss.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109216650A (en) * | 2017-06-30 | 2019-01-15 | 比亚迪股份有限公司 | Battery electrode and preparation method thereof and all-solid-state battery |
| CN111781781A (en) * | 2020-07-02 | 2020-10-16 | 深圳市诚德利科技有限公司 | Memory electrochromic film based on rare earth metal and preparation method and application thereof |
| CN113299987A (en) * | 2021-05-25 | 2021-08-24 | 哈尔滨工业大学 | Preparation method of solid polymer electrolyte of zinc ion battery |
| CN113701924A (en) * | 2021-08-24 | 2021-11-26 | 南京工业大学 | Porous solid-state ionic gel electrode and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109216650A (en) * | 2017-06-30 | 2019-01-15 | 比亚迪股份有限公司 | Battery electrode and preparation method thereof and all-solid-state battery |
| CN109216650B (en) * | 2017-06-30 | 2021-04-20 | 比亚迪股份有限公司 | Battery electrode, preparation method thereof and all-solid-state battery |
| CN111781781A (en) * | 2020-07-02 | 2020-10-16 | 深圳市诚德利科技有限公司 | Memory electrochromic film based on rare earth metal and preparation method and application thereof |
| CN111781781B (en) * | 2020-07-02 | 2023-03-21 | 深圳市诚德利科技有限公司 | Memory electrochromic film based on rare earth metal and preparation method and application thereof |
| CN113299987A (en) * | 2021-05-25 | 2021-08-24 | 哈尔滨工业大学 | Preparation method of solid polymer electrolyte of zinc ion battery |
| CN113299987B (en) * | 2021-05-25 | 2022-07-05 | 哈尔滨工业大学 | Preparation method of solid polymer electrolyte of zinc ion battery |
| CN113701924A (en) * | 2021-08-24 | 2021-11-26 | 南京工业大学 | Porous solid-state ionic gel electrode and preparation method and application thereof |
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Application publication date: 20160413 |