CN111900467A - Metal organic framework material modified PEO-based fire-safe solid polymer electrolyte and preparation method thereof - Google Patents
Metal organic framework material modified PEO-based fire-safe solid polymer electrolyte and preparation method thereof Download PDFInfo
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- CN111900467A CN111900467A CN202010650624.3A CN202010650624A CN111900467A CN 111900467 A CN111900467 A CN 111900467A CN 202010650624 A CN202010650624 A CN 202010650624A CN 111900467 A CN111900467 A CN 111900467A
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- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 34
- 239000005518 polymer electrolyte Substances 0.000 title claims abstract description 30
- 239000007787 solid Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 51
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 21
- 239000013148 Cu-BTC MOF Substances 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 11
- 229910003002 lithium salt Inorganic materials 0.000 claims description 11
- 159000000002 lithium salts Chemical class 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 5
- 239000013207 UiO-66 Substances 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 239000012456 homogeneous solution Substances 0.000 claims description 2
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052912 lithium silicate Inorganic materials 0.000 claims description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 10
- 239000003792 electrolyte Substances 0.000 abstract description 7
- 238000002485 combustion reaction Methods 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 description 17
- 239000003814 drug Substances 0.000 description 10
- 229920000307 polymer substrate Polymers 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- 239000004809 Teflon Substances 0.000 description 5
- 229920006362 Teflon® Polymers 0.000 description 5
- 239000003517 fume Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000004502 linear sweep voltammetry Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Classifications
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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
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62C—FIRE-FIGHTING
- A62C3/00—Fire prevention, containment or extinguishing specially adapted for particular objects or places
- A62C3/16—Fire prevention, containment or extinguishing specially adapted for particular objects or places in electrical installations, e.g. cableways
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2200/00—Safety devices for primary or secondary batteries
-
- 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
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
-
- 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 relates to a PEO-based fire-safe solid polymer electrolyte modified by a metal organic framework material and a preparation method thereof. The introduced metal organic framework material further releases more lithium ions capable of freely conducting, and has great contribution to improving the electrochemical performance of the electrolyte. Meanwhile, the metal organic framework material can catalyze and protect the formation of a carbon layer in the combustion process of the polymer due to the unique catalysis property, so that the further occurrence of combustion is inhibited, and the fire safety is improved. The modified solid polymer electrolyte prepared by the method has good ionic conductivity, electrochemical stability and thermal stability, is suitable for lithium ion batteries under certain conditions, and can greatly improve the safety performance.
Description
Technical Field
The invention belongs to the field of lithium battery electrolytes, and relates to a metal organic framework material modified PEO-based fire-safe solid polymer electrolyte and a preparation method thereof.
Background
The lithium ion battery has the characteristics of high energy ratio, long cycle life, cleanness, no pollution and the like, and gradually becomes a novel green energy system with the most development prospect and application prospect in the 21 st century. In daily life, due to the concern of safety problems of lithium ion batteries caused by the accidental occurrence of battery abuse and the accident of battery burning or explosion caused by severe impact, the development of all-solid-state batteries, which are necessary for the electrolyte material with fire safety, has become a necessary path for the development of lithium batteries in the future, wherein the solid-state polymer electrolyte is regarded as one of important development directions in the future. Solid polymer electrolytes composed of a polymer matrix and a lithium salt are considered to be the development direction of lithium battery electrolytes in the future. Among them, polyethylene oxide (PEO) has been widely studied because of its good complexing ability with lithium ions, but too high cost of modified fillers, poor electrochemical stability and low ionic conductivity have been a great obstacle to its large-scale application. On the other hand, PEO, which is one of flammable polymers, when it is applied as a polymer substrate in a solid polymer electrolyte, its flammability lowers fire safety of a lithium ion battery system, so that safety cannot be secured.
The application of metal organic framework Materials (MOFs) in the fields of gas storage and separation, catalysis, sensing, drug delivery, and the like has attracted wide attention. In general, MOFs are hybrid organic-inorganic materials with intramolecular pores formed by self-assembly of organic ligands and metal ions or clusters through coordination bonds, which have open metal sites capable of capturing anions, and release more freely conductive lithium ions after mixing with a metal lithium salt. Meanwhile, the metal sites can catalyze and protect the formation of a carbon layer in the combustion process of the polymer, so that the fire safety performance of the polymer is improved
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a PEO-based fire-safe solid polymer electrolyte modified by a metal organic framework material and a preparation method thereof. The solid electrolyte with good electrochemical stability and high ionic conductivity is obtained.
Technical scheme
A PEO-based fire-safe solid polymer electrolyte modified by a metal organic framework material is characterized in that the components are that the metal organic framework material is used as a modified filler, polyethylene oxide (PEO) is used as a matrix, and lithium bistrifluoromethanesulfonylimide (LiTFSI) is used as a lithium salt; wherein: the dosage of the metal organic framework material is 5-15 wt% of the total mass of the polymer matrix and the lithium salt; EO: Li+The molar ratio of the components is 15: 1-17: 1.
The EO: Li+The molar ratio of (A) to (B) is 15: 1.
The metal organic framework material includes but is not limited to HKUST-1, ZIF-67@ ZIF-8 or UiO-66.
The polyethylene oxide PEO has a molecular weight of 400000-900000.
The polyethylene oxide PEO has a molecular weight of 900000.
A preparation method of a PEO-based fire-safe solid polymer electrolyte modified by the metal organic framework material is characterized by comprising the following steps:
step 1: PEO, LiTFSI and metal organic framework material were dissolved in acetonitrile and magnetically stirred to a homogeneous solution. Stirring at 400-600 rpm, preferably 530rpm, for 6-18 h to form a solution; the using amount of the acetonitrile is 8-9 times of the total mass of the substances;
step 2: pouring the solution into a polytetrafluoroethylene culture dish, volatilizing at room temperature to remove the solvent, and drying to obtain the lithium silicate modified PEO-based solid polymer electrolyte; the drying time is 6-24 h, and the drying temperature is 40-70 ℃.
The amount of acetonitrile is 9 times of the total mass of the substance.
The stirring time of the step 1 is 12 hours.
The drying time of the step 2 is 12-18 h.
The temperature of the drying in step 2 was 60 ℃.
Advantageous effects
The invention provides a PEO-based fire-safe solid polymer electrolyte modified by a metal organic framework material and a preparation method thereof. The introduced metal organic framework material can further release more lithium ions capable of freely conducting, is used as a modified filler of the electrolyte, and has great contribution to improvement of the electrochemical performance of the electrolyte. Meanwhile, the metal organic framework material can catalyze and protect the formation of a carbon layer in the combustion process of the polymer due to the unique catalysis property, so that the further occurrence of combustion is inhibited, and the fire safety is improved. The modified solid polymer electrolyte prepared by the method has good ionic conductivity, electrochemical stability and thermal stability, is suitable for lithium ion batteries under certain conditions, and can greatly improve the safety performance.
Compared with the prior art, the invention improves the electrochemical stability and the ionic conductivity and the fire safety by introducing the metal organic framework material as the modified filler, so that the electrochemical performance and the use safety of the PEO-based solid polymer electrolyte are improved.
The results in FIG. 1 show that, after the addition of HKUST-1, it can be concluded that the modified filler was successfully added to the polymer substrate, while no unwanted diffraction peaks were observed, indicating that the properties of the other components were not affected.
The components of the obtained electrolyte membrane are uniformly dispersed without agglomeration, which can be seen from a scanning electron microscope image, and the uniform distribution of HKUST-1 in a polymer substrate is realized.
After HKUST-1 is added, the heat release rate is obviously reduced, and the reduction amplitude reaches about 42 percent, thereby showing that the fire safety performance is effectively improved.
DSC results showed the glass transition temperature point (T) of the solid polymer electrolyte membrane after the addition of ZIF-67@ ZIF-8g) And melting point (T)m) Respectively to-40.6 ℃ and 47.4 ℃, thereby increasing the mobility of the PEO polymer segments and reducing the nodules of the PEO substrateAnd the crystallinity improves the transmission capability of lithium ions.
LSV tests show that the electrochemical stability window of the ZIF-67@ ZIF-8 modified PEO-based fire-safe solid polymer electrolyte reaches 4.86V, and the electrolyte can be matched with almost all electrode materials in the current stage.
It can be seen that the ionic transport capacity of the uo-66 modified PEO-based fire-safe solid polymer electrolyte increases with increasing temperature.
Drawings
FIG. 1 is an XRD pattern of a sample of a product of an example of the invention.
FIG. 2 is a scanning electron micrograph of a sample of a product of an embodiment of the present invention.
FIG. 3 is a heat release rate test curve for a sample of a product of an example of the invention.
FIG. 4 is a graph showing the results of Differential Scanning Calorimetry (DSC) measurements on samples of products according to examples of the present invention.
FIG. 5 is a graph of the results of a linear sweep voltammetry test (LSV) on a sample of a product of an example of the invention.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
step 1: mixing LiTFSI, PEO (M)w=9×105g mol-1) And the HKUST-1 metal organic framework material is dried in a vacuum oven at 50 ℃ for 24 hours and is placed in a glove box for standby.
Step 2: weighing the PEO, the LiTFSI and the HKUST-1 obtained by drying in the step 1 in proportion, wherein the mass of the HKUST-1 is 5% wt of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the membrane, placing the membrane in a polytetrafluoroethylene culture dish, drying the membrane in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based fire-safe solid polymer electrolyte with HKUST-1 as a modified filler.
Example 2:
step 1: mixing LiTFSI, PEO (M)w=9×105g mol-1) And the HKUST-1 metal organic framework material is dried in a vacuum oven at 50 ℃ for 24 hours and is placed in a glove box for standby.
Step 2: weighing the PEO, the LiTFSI and the HKUST-1 obtained by drying in the step 1 in proportion, wherein the mass of the HKUST-1 is 10% wt of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the membrane, placing the membrane in a polytetrafluoroethylene culture dish, drying the membrane in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based fire-safe solid polymer electrolyte with HKUST-1 as a modified filler.
Example 3:
step 1: mixing LiTFSI, PEO (M)w=9×105g mol-1) And the HKUST-1 metal organic framework material is dried in a vacuum oven at 50 ℃ for 24 hours and is placed in a glove box for standby.
Step 2: weighing the PEO, the LiTFSI and the HKUST-1 obtained by drying in the step 1 in proportion, wherein the mass of the HKUST-1 is 15% wt of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the membrane, placing the membrane in a polytetrafluoroethylene culture dish, drying the membrane in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based fire-safe solid polymer electrolyte with HKUST-1 as a modified filler.
Example 4:
step 1: mixing LiTFSI, PEO (M)w=9×105g mol-1) And drying the ZIF-67@ ZIF-8 metal organic framework material in a vacuum oven at 50 ℃ for 24 hours, and placing the material in a glove box for later use.
Step 2: weighing PEO, LiTFSI and ZIF-67@ ZIF-8 obtained by drying in the step 1 in proportion, wherein the mass of the ZIF-67@ ZIF-8 is 15 wt% of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the membrane, placing the membrane in a polytetrafluoroethylene culture dish, drying the membrane in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based fire-safe solid polymer electrolyte taking ZIF-67@ ZIF-8 as the modified filler.
Example 5:
step 1: mixing LiTFSI, PEO (M)w=9×105g mol-1) And the UiO-66 metal organic framework material is dried in a vacuum oven at 50 ℃ for 24 hours and is placed in a glove box for standby.
Step 2: weighing PEO, LiTFSI and UiO-66 obtained by drying in the step 1 in proportion, wherein the mass of the UiO-66 is 15 wt% of the total mass of the polymer substrate and the lithium salt, and controlling the EO: li+In a molar ratio of 15: 1, placing the weighed medicine into a beaker, adding acetonitrile (the mass of the acetonitrile is 9 times of the total mass of the weighed medicine), and stirring strongly at room temperature for 12 hours.
And step 3: the resulting solution was poured onto a teflon plate, allowed to advect naturally, and the solvent was evaporated off at room temperature in a fume hood.
And 4, step 4: and tearing the membrane, placing the membrane in a polytetrafluoroethylene culture dish, drying the membrane in a vacuum oven at 60 ℃ for 12 hours, and further removing the solvent to obtain the PEO-based fire-safe solid polymer electrolyte taking ZIF-67@ ZIF-8 as the modified filler.
Claims (10)
1. A PEO-based fire-safe solid polymer electrolyte modified by a metal organic framework material is characterized in that the components are that the metal organic framework material is used as a modified filler, polyethylene oxide (PEO) is used as a matrix, and lithium bistrifluoromethanesulfonylimide (LiTFSI) is used as a lithium salt; wherein: the dosage of the metal organic framework material is 5-15 wt% of the total mass of the polymer matrix and the lithium salt; EO: Li+The molar ratio of the components is 15: 1-17: 1.
2. The metal organic framework material modified PEO-based fire safe solid polymer electrolyte of claim 1, wherein: the EO: Li+The molar ratio of (A) to (B) is 15: 1.
3. The metal organic framework material modified PEO-based fire safe solid polymer electrolyte of claim 1, wherein: the metal organic framework material includes but is not limited to HKUST-1, ZIF-67@ ZIF-8 or UiO-66.
4. The metal organic framework material modified PEO-based fire safe solid polymer electrolyte of claim 1, wherein: the polyethylene oxide PEO has a molecular weight of 400000-900000.
5. The metal organic framework material modified PEO-based fire safe solid polymer electrolyte of claim 1 or 4, wherein: the polyethylene oxide PEO has a molecular weight of 900000.
6. A process for the preparation of a PEO-based fire-safe solid polymer electrolyte modified with a metal-organic framework material according to any of claims 1 to 5, characterized by the following steps:
step 1: PEO, LiTFSI and metal organic framework material were dissolved in acetonitrile and magnetically stirred to a homogeneous solution. Stirring at 400-600 rpm, preferably 530rpm, for 6-18 h to form a solution; the using amount of the acetonitrile is 8-9 times of the total mass of the substances;
step 2: pouring the solution into a polytetrafluoroethylene culture dish, volatilizing at room temperature to remove the solvent, and drying to obtain the lithium silicate modified PEO-based solid polymer electrolyte; the drying time is 6-24 h, and the drying temperature is 40-70 ℃.
7. The method of claim 6, wherein: the amount of acetonitrile is 9 times of the total mass of the substance.
8. The method of claim 6, wherein: the stirring time of the step 1 is 12 hours.
9. The method of claim 6, wherein: the drying time of the step 2 is 12-18 h.
10. The method of claim 6, wherein: the temperature of the drying in step 2 was 60 ℃.
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