CN112786958A - Composite porous gel polymer electrolyte and preparation method thereof - Google Patents
Composite porous gel polymer electrolyte and preparation method thereof Download PDFInfo
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- CN112786958A CN112786958A CN202110119059.2A CN202110119059A CN112786958A CN 112786958 A CN112786958 A CN 112786958A CN 202110119059 A CN202110119059 A CN 202110119059A CN 112786958 A CN112786958 A CN 112786958A
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 239000005518 polymer electrolyte Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920000642 polymer Polymers 0.000 claims abstract description 23
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 17
- 239000012071 phase Substances 0.000 claims abstract description 16
- 239000002313 adhesive film Substances 0.000 claims abstract description 14
- 239000006255 coating slurry Substances 0.000 claims abstract description 14
- 229920000728 polyester Polymers 0.000 claims abstract description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- 229920003225 polyurethane elastomer Polymers 0.000 claims abstract description 12
- 230000004913 activation Effects 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000012808 vapor phase Substances 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 230000001112 coagulating effect Effects 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 230000015271 coagulation Effects 0.000 claims description 6
- 238000005345 coagulation Methods 0.000 claims description 6
- 239000000701 coagulant Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229920006254 polymer film Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 239000004809 Teflon Substances 0.000 claims 2
- 229920006362 Teflon® Polymers 0.000 claims 2
- 239000002002 slurry Substances 0.000 claims 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 10
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 10
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000012528 membrane Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000011245 gel electrolyte Substances 0.000 description 8
- 238000004080 punching Methods 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229920005597 polymer membrane Polymers 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000011244 liquid electrolyte Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 229920000831 ionic polymer Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
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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
-
- 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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Dispersion Chemistry (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a composite porous gel polymer electrolyte and a preparation method thereof, relating to the technical field of lithium ion batteries, wherein the preparation method comprises the following steps: dispersing vapor phase aluminum oxide into a solvent, then adding a polyester type polyurethane elastomer, heating and uniformly stirring to obtain coating slurry; coating the coating slurry on a polytetrafluoroethylene plate, standing until a nascent film is formed, then placing the nascent film in a coagulating bath for phase exchange to obtain a polymer adhesive film, and drying in vacuum to obtain a composite polymer dry film; and immersing the composite polymer dry film into an electrolyte under an inert atmosphere for activation, and taking out to obtain the composite porous gel polymer electrolyte. The composite porous polymer electrolyte adhesive film prepared by the invention has excellent mechanical property and electrochemical stability, high ionic conductivity, and the assembled button cell also shows good cycling stability.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a composite porous gel polymer electrolyte and a preparation method thereof.
Background
In recent years, with the shortage of conventional energy and the increasing environmental problem, the development and application of new clean energy are urgent. Lithium ion batteries have attracted attention because of their excellent characteristics of high operating voltage, high specific energy density, long cycle life, safety, reliability, and the like. Particularly, with the emergence of plastic lithium ion batteries, the research and development of ionic polymer electrolytes are in a new stage.
The gel polymer electrolyte has ion mobility and charge carrier concentration close to those of liquid electrolyte, and the ion conductivity can reach 10 at room temperature-4～10-3S/cm, and the gel polymer electrolyte adsorbing the electrolyte has safety not possessed by liquid electrolytes. Among the gel polymer electrolyte systems, the polyethylene oxide-based polymer electrolyte system is currently the most studied by scientists, but the higher crystallinity at room temperature leads to an ionic conductivity of only 10-7～10-8S/cm。
Disclosure of Invention
The invention provides a composite porous gel polymer electrolyte and a preparation method thereof, aiming at the problems of safety technology and low ionic conductivity of a solid polymer electrolyte of the traditional liquid lithium ion battery.
The invention provides a preparation method of a composite porous gel polymer electrolyte, which comprises the following steps:
s1, dispersing the vapor phase aluminum oxide into a solvent, then adding the polyester type polyurethane elastomer, heating and uniformly stirring to obtain coating slurry;
s2, coating the coating slurry on a polytetrafluoroethylene plate, standing until a primary film is formed, then placing the primary film in a coagulating bath for phase exchange to obtain a polymer adhesive film, and drying in vacuum to obtain a composite polymer dry film;
and S3, immersing the composite polymer dry film into an electrolyte under an inert atmosphere for activation, and taking out to obtain the composite porous gel polymer electrolyte.
Preferably, in S1, the mass percentage of the fumed alumina to the polyester polyurethane elastomer is 1-8: 92-99; preferably, the particle size D50 of the vapor phase alumina is 10-20 nm; preferably, the number average molecular weight of the polyester polyurethane elastomer is 1 × 105、2×105、5×105、1×106Preferably 2 × 10, and5。
preferably, in S1, the solvent is N, N-dimethylformamide; preferably, the mass ratio of the polyester polyurethane elastomer to the solvent is 1: 3 to 5.
Preferably, in S1, the fumed alumina is added into the solvent, magnetically stirred and dispersed for 2-6 hours at 40-80 ℃, then the polyester polyurethane elastomer is added, and the temperature is raised to 100-150 ℃ and stirred uniformly.
Preferably, in S2, the coagulant is deionized water.
Preferably, in S2, the coating slurry is applied to a polytetrafluoroethylene sheet with a 500 μm wet film doctor blade to conduct doctor blading until a primary film is formed on the polytetrafluoroethylene sheet, and then the sheet is placed in a coagulation bath to conduct phase exchange.
Preferably, in S2, the standing time for forming the primary film is controlled to be 80-100 min; preferably, the phase change time is 5-7 h.
Preferably, in S2, the composite dry polymer film has a thickness of 180 to 220 μm.
Preferably, in S3, the activation time is 5-10 min.
The invention also provides the composite porous gel polymer electrolyte prepared by the method.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
1. the coagulant in the preparation process of the invention adopts deionized water, is clean and pollution-free and is harmless to human body;
2. the polyester type polyurethane elastomer adopted by the invention has excellent mechanical property, so that the prepared polymer electrolyte has good interface stability and cycling stability in the use process of the lithium ion battery;
3. the added gas-phase alumina has a mechanical enhancement function on a polymer matrix, the existence of the alumina has a promotion effect on pore forming of the polymer matrix, the porosity is improved, and the ionic conductivity is increased.
Drawings
FIG. 1 is a graph showing a liquid absorption rate test of porous gel electrolyte membranes prepared in examples 1 to 3 of the present invention and a comparative example;
FIG. 2 is a graph showing mechanical property test curves of porous gel electrolyte membranes prepared in examples 1 to 3 of the present invention and a comparative example;
FIG. 3 is a graph showing the AC impedance of porous gel electrolyte membranes obtained in examples 1 to 3 of the present invention and a comparative example; wherein the lower right corner is an enlarged view.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
The specific preparation process of the composite porous gel polymer electrolyte comprises the following steps:
1. 0.063g of fumed alumina is added into 12g of DMF, magnetic stirring is carried out at 60 ℃ for 4 hours, 4g of polyester TPU is added, the temperature is increased to 135 ℃, and strong stirring is carried out until uniform coating slurry is formed.
2. The obtained uniform coating slurry was subjected to film scraping on a clean polytetrafluoroethylene plate having no surface scratches using a 500 μm wet film scraper at room temperature, allowed to stand for 90min until primary film formation, and placed in a coagulation bath together with the polytetrafluoroethylene plate for phase replacement for 6 hours. And (3) drying the polymer adhesive film subjected to phase replacement in a constant-temperature vacuum drying oven at 60 ℃ for 2h to obtain a polymer dry film with the thickness of about 200 mu m.
3. And punching the dried polymer adhesive film into a wafer with the radius of 8mm by using a punching machine, and transferring the wafer into a vacuum glove box filled with argon gas for storage and standby. And finally, immersing the porous polymer membrane into electrolyte (lithium hexafluorophosphate as solute) in a glove box for activation for 10min to obtain the composite porous gel electrolyte membrane.
Example 2
The specific preparation process of the composite porous gel polymer electrolyte comprises the following steps:
1. 0.063g of fumed alumina is added into 16g of DMF, magnetic stirring is carried out at 60 ℃ for 4 hours, 4g of TPU is added, the temperature is increased to 135 ℃, and strong stirring is carried out until uniform coating slurry is formed.
2. The obtained uniform coating slurry was subjected to film scraping on a clean polytetrafluoroethylene plate having no surface scratches using a 500 μm wet film scraper at room temperature, allowed to stand for 90min until primary film formation, and placed in a coagulation bath together with the polytetrafluoroethylene plate for phase replacement for 6 hours. And (3) drying the polymer adhesive film subjected to phase replacement in a constant-temperature vacuum drying oven at 60 ℃ for 2h to obtain a polymer dry film with the thickness of about 200 mu m.
3. And punching the dried polymer adhesive film into a wafer with the radius of 8mm by using a punching machine, and transferring the wafer into a vacuum glove box filled with argon gas for storage and standby. And finally, immersing the porous polymer membrane into electrolyte (lithium hexafluorophosphate as solute) in a glove box for activation for 10min to obtain the composite porous gel electrolyte membrane.
Example 3
The specific preparation process of the composite porous gel polymer electrolyte comprises the following steps:
1. 0.063g of fumed alumina is added into 20g of DMF, magnetic stirring is carried out at 60 ℃ for 4 hours, 4g of TPU is added, the temperature is increased to 135 ℃, and strong stirring is carried out until uniform coating slurry is formed.
2. The obtained uniform coating slurry was subjected to film scraping on a clean polytetrafluoroethylene plate having no surface scratches using a 500 μm wet film scraper at room temperature, allowed to stand for 90min until primary film formation, and placed in a coagulation bath together with the polytetrafluoroethylene plate for phase replacement for 6 hours. And (3) drying the polymer adhesive film subjected to phase replacement in a constant-temperature vacuum drying oven at 60 ℃ for 2h to obtain a polymer dry film with the thickness of about 200 mu m.
3. And punching the dried polymer adhesive film into a wafer with the radius of 8mm by using a punching machine, and transferring the wafer into a vacuum glove box filled with argon gas for storage and standby. And finally, immersing the porous polymer membrane into electrolyte (lithium hexafluorophosphate as solute) in a glove box for activation for 10min to obtain the composite porous gel electrolyte membrane.
Comparative example
The specific preparation process of the porous gel polymer electrolyte comprises the following steps:
1. 4g of TPU was added to 16g of DMF and the mixture was heated to 135 ℃ and stirred vigorously until a uniform coating paste was formed.
2. The obtained uniform coating slurry was subjected to film scraping on a clean polytetrafluoroethylene plate having no surface scratches using a 500 μm wet film scraper at room temperature, allowed to stand for 90min until primary film formation, and placed in a coagulation bath together with the polytetrafluoroethylene plate for phase replacement for 6 hours. And (3) drying the polymer adhesive film subjected to phase replacement in a constant-temperature vacuum drying oven at 60 ℃ for 2h to obtain a polymer dry film with the thickness of about 200 mu m.
3. And punching the dried polymer adhesive film into a wafer with the radius of 8mm by using a punching machine, and transferring the wafer into a vacuum glove box filled with argon gas for storage and standby. And finally, immersing the porous polymer membrane into electrolyte (lithium hexafluorophosphate as solute) in a glove box for activation for 10min to obtain the porous gel electrolyte membrane.
The porous gel electrolyte membranes prepared in examples 1 to 3 and comparative example were subjected to performance tests, and the results are shown in fig. 1 to 3.
Fig. 1 is a graph showing liquid absorption rate test curves of examples and comparative examples, and it can be seen from the test results of fig. 1 that the liquid absorption rates of examples 1 to 3 and comparative examples are 300.5%, 331.7%, 318.4%, and 290.8%, respectively, and the liquid absorption rate of the composite porous membrane is higher than that of the blank comparative example. The test result shows that the pores of the composite porous membrane for storing the electrolyte are increased after the nano-alumina is added, and the liquid absorption rate is increased.
FIG. 2 is the mechanical property test curves of examples and comparative examples, the tensile strengths of examples 1-3 and comparative examples are 25.1MPa, 18.8MPa, 19.6MPa and 27.4MPa, respectively, and the tensile strength of the blank sample is higher than that of the composite porous polymer film. The test result shows that the composite porous membrane has more gaps, the mechanical property is reduced due to stress concentration, and the mechanical strength is far more capable of meeting the requirement of the lithium ion battery.
FIG. 3 shows the AC impedance test of the examples and comparative examples. The impedance spectrum values of examples 1 to 3 and comparative example were 1.8. omega., 1.1. omega., 1.6. omega., and 2.4. omega., respectively. The room temperature ionic conductivity of the polymer electrolyte may be according to the formula
Calculating to obtain the ion conductivity of the sigma-polymer electrolyte adhesive film; l-the thickness of the corresponding polymer electrolyte membrane layer; r-the bulk resistance of the corresponding polymer electrolyte adhesive film; s-polymer electrolyte gelThe real contact area of the film and the stainless steel sheet. As a result of calculation, the lithium ion conductivities of examples 1 to 3 and comparative example were 4.77X 10, respectively-3s/cm、6.84×10-3s/cm、5.53×10-3s/cm、3.21×10-3s/cm. Test results show that the composite porous polymer electrolyte has more excellent lithium ion conductivity and is expected to be applied to lithium ion battery commercialization.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The preparation method of the composite porous gel polymer electrolyte is characterized by comprising the following steps of:
s1, dispersing the vapor phase aluminum oxide into a solvent, then adding the polyester type polyurethane elastomer, heating and uniformly stirring to obtain coating slurry;
s2, coating the coating slurry on a polytetrafluoroethylene plate, standing until a primary film is formed, then placing the primary film in a coagulating bath for phase exchange to obtain a polymer adhesive film, and drying in vacuum to obtain a composite polymer dry film;
and S3, immersing the composite polymer dry film into an electrolyte under an inert atmosphere for activation, and taking out to obtain the composite porous gel polymer electrolyte.
2. The preparation method of the composite porous gel polymer electrolyte according to claim 1, wherein in S1, the mass percentage of the fumed alumina to the polyester type polyurethane elastomer is 1-8: 92-99; preferably, the particle size D50 of the vapor phase alumina is 10-20 nm; preferably, the number average molecular weight of the polyester polyurethane elastomer is 1 × 105、2×105、5×105、1×106Preferably 2 × 10, and5。
3. the method for preparing a composite porous gel polymer electrolyte according to claim 1, wherein in S1, the solvent is N, N-dimethylformamide; preferably, the mass ratio of the polyester polyurethane elastomer to the solvent is 1: 3 to 5.
4. The preparation method of the composite porous gel polymer electrolyte according to claim 1, wherein in S1, fumed alumina is added into a solvent, magnetically stirred and dispersed for 2-6 hours at 40-80 ℃, then a polyester type polyurethane elastomer is added, and the temperature is raised to 100-150 ℃ and uniformly stirred.
5. The method of claim 1, wherein the coagulant is deionized water in S2.
6. The method of claim 1, wherein in S2, the slurry is applied to a teflon plate with a 500 μm wet film blade to form a primary film on the teflon plate, and the primary film is then placed in a coagulation bath to undergo phase exchange.
7. The method for preparing the composite porous gel polymer electrolyte according to claim 1, wherein in S2, the standing time for forming the primary film is controlled to be 80-100 min; preferably, the phase change time is 5-7 h.
8. The method of claim 1, wherein the composite dry polymer film has a thickness of 180 to 220 μm in S2.
9. The method for preparing the composite porous gel polymer electrolyte according to claim 1, wherein the activation time in S3 is 5-10 min.
10. A composite porous gel polymer electrolyte prepared by the method of any one of claims 1 to 9.
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| CN117855582A (en) * | 2024-03-08 | 2024-04-09 | 河南师范大学 | Flexible composite solid electrolyte and preparation and application thereof |
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| CN109326821A (en) * | 2018-09-14 | 2019-02-12 | 湘潭大学 | A kind of nanometer-material-modified rubber-gel electrolyte film and Preparation method and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109326821A (en) * | 2018-09-14 | 2019-02-12 | 湘潭大学 | A kind of nanometer-material-modified rubber-gel electrolyte film and Preparation method and use |
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| 高明昊等: ""聚氨酯／SiO2复合凝胶聚合物电解质的制备与性能"", 《高分子材料科学与工程》 * |
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| CN117855582A (en) * | 2024-03-08 | 2024-04-09 | 河南师范大学 | Flexible composite solid electrolyte and preparation and application thereof |
| CN117855582B (en) * | 2024-03-08 | 2024-05-24 | 河南师范大学 | Flexible composite solid electrolyte and preparation and application thereof |
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Application publication date: 20210511 |