CN113363563A - Composite solid electrolyte and preparation method and application thereof - Google Patents
Composite solid electrolyte and preparation method and application thereof Download PDFInfo
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- CN113363563A CN113363563A CN202110559155.9A CN202110559155A CN113363563A CN 113363563 A CN113363563 A CN 113363563A CN 202110559155 A CN202110559155 A CN 202110559155A CN 113363563 A CN113363563 A CN 113363563A
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- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 32
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- 239000000945 filler Substances 0.000 claims abstract description 14
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 13
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 13
- 239000012528 membrane Substances 0.000 claims abstract description 13
- 238000007731 hot pressing Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 5
- 239000002001 electrolyte material Substances 0.000 claims abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 6
- -1 lithium hexafluorophosphate Chemical compound 0.000 claims description 5
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims description 2
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 2
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 claims description 2
- 229910001486 lithium perchlorate Inorganic materials 0.000 claims description 2
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000013329 compounding Methods 0.000 abstract description 4
- 239000007787 solid Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 229920002239 polyacrylonitrile Polymers 0.000 description 4
- 239000005518 polymer electrolyte Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- VDVLPSWVDYJFRW-UHFFFAOYSA-N lithium;bis(fluorosulfonyl)azanide Chemical compound [Li+].FS(=O)(=O)[N-]S(F)(=O)=O VDVLPSWVDYJFRW-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 description 1
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
-
- 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
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- 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
- H01M2300/0068—Solid electrolytes inorganic
- H01M2300/0071—Oxides
-
- 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)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Conductive Materials (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to the technical field of lithium ion batteries, in particular to a composite solid electrolyte and a preparation method thereof, wherein the composite electrolyte material comprises a polymer, a lithium salt and a perovskite solid electrolyte filler; the preparation method comprises the following steps: (1) uniformly mixing a polymer, a lithium salt and a perovskite solid electrolyte filler, heating, melting and stirring to form an electrolyte composite solution; (2) and pouring the electrolyte composite solution on a substrate, carrying out hot pressing to a specified thickness to form a composite electrolyte membrane, and cooling to normal temperature to obtain the composite solid electrolyte. According to the invention, through the compounding of the polymer, the lithium salt and the high-conductivity perovskite solid electrolyte, the mechanical property of the composite solid electrolyte is improved, the electrochemical window is widened, and the interface impedance is reduced.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a composite solid electrolyte and a preparation method thereof.
Background
With the rapid development of industries such as electronic information, new energy automobiles and the like, the solid-state battery becomes a research hotspot of new energy materials due to the advantages of high energy density, safety, high working voltage, environmental friendliness and the like. The solid electrolyte is the most critical material in the solid battery, and is required to have the advantages of high thermal stability, negligible electronic conductance, wide electrochemical window, high ionic conductance and the like. Solid electrolytes are mainly classified into four main groups: organic-inorganic hybrid electrolyte, solid polymer electrolyte, solid sulfide electrolyte, and solid oxide electrolyte. The solid polymer electrolyte is an electrolyte material formed by compounding lithium salt and a polymer, and has the characteristics of easy assembly and good safety. The solid oxide electrolyte has better ion conductivity, wider electrochemical stability window and chemical stability.
The solid polymer electrolyte is easy to install and has good safety, but also has the problems of poor mechanical property, low conductivity and the like. The solid oxide electrolyte has good ion conductivity, a wide electrochemical stability window and chemical stability, but still has the problems of poor flexibility, large grain boundary resistance, large interface resistance between the solid oxide electrolyte and an electrode and the like.
Chinese patent literature discloses a preparation method of a polymer composite solid electrolyte and the polymer composite solid electrolyte, the application publication number of the preparation method is CN 112786951A, and the invention prepares polyacrylonitrile porous membrane matrix materials with different pore structures; performing alkali treatment reaction on polyacrylonitrile porous membrane base materials with different pore structures to obtain a functional polyacrylonitrile porous membrane base material; the polymer composite solid electrolyte for the all-solid-state lithium battery is obtained by compounding the functional polyacrylonitrile porous membrane substrate material and the inorganic component, and the prepared polymer composite solid electrolyte has high ionic conductivity, rich ionic conduction interfaces, good mechanical property, excellent structure and performance stability. However, the preparation process of the polymer composite solid electrolyte is complex and is not easy to industrialize.
The Chinese patent document discloses a composite solid electrolyte, a preparation method thereof and a solid battery, and the application publication number of the composite solid electrolyte is CN 112786950A. However, the invention is a three-layer structure composite membrane, the coating process requirement is high, the operation is complex, and the industrialization is not easy to realize.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides the composite solid electrolyte which can improve the ionic conductivity, widen the electrochemical window, enhance the mechanical property and improve the interface impedance.
The invention also provides a preparation method of the composite solid electrolyte, which is simple to operate, easy to control conditions and easy to industrialize.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composite solid electrolyte, the composite electrolyte material comprising a polymer, a lithium salt and a perovskite solid electrolyte filler.
The composite solid electrolyte design of the invention integrates the advantages of polymer electrolytes and solid oxide electrolytes, and can improve the ionic conductivity, widen the electrochemical window, enhance the mechanical property and improve the interface impedance.
Preferably, the chemical structural general formula of the perovskite solid electrolyte filler is Li0.5La0.5Ti1–xMxO3Wherein, M is a doping element,Xis the doping amount; m is selected from one or more of Sn, Al, Mn, Fe, Zr and Ge,Xthe range of (A) is 0.01 to 0.15. The ion conductivity of the solid oxide electrolyte can be obviously improved by doping the M element.
Preferably, the polymer is one or more selected from polyvinylidene fluoride, polyacrylic acid, polyvinyl cyanide, polyethylene oxide and polymethacrylic acid.
Preferably, the lithium salt is selected from one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium bistrifluoromethylsulfonyl imide, lithium bistrifluorosulfonimide, lithium bisoxalato borate, lithium perchlorate and lithium difluorooxalato borate.
Preferably, the mass ratio of the polymer to the lithium salt to the perovskite solid electrolyte filler is (4-6): (2-3): (2-3).
A method of preparing a composite solid electrolyte comprising the steps of:
(1) uniformly mixing a polymer, a lithium salt and a perovskite solid electrolyte filler, heating, melting and stirring to form an electrolyte composite solution; (2) and pouring the electrolyte composite solution on a substrate, carrying out hot pressing to a specified thickness to form a composite electrolyte membrane, and cooling to normal temperature to obtain the composite solid electrolyte.
Preferably, in the step (1), the heating and melting temperature is 200-300 ℃ and the time is 2-3 h. .
Preferably, in the step (2), the hot pressing temperature is 75-85 ℃ and the pressure is 15-25 Mpa.
Preferably, in the step (2), the thickness of the composite electrolyte membrane is 30 to 100 μm.
An application of a composite solid electrolyte in a lithium ion battery.
Therefore, the invention has the following beneficial effects:
(1) according to the invention, through the compounding of the polymer, the lithium salt and the high-conductivity perovskite solid electrolyte, the mechanical property of the composite solid electrolyte is improved, the electrochemical window is widened, and the interface impedance is reduced;
(2) the preparation method is simple to operate, easy to control conditions and easy to industrialize;
(3) the composite solid electrolyte has wide application prospect in lithium ion batteries.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) Mixing polyacrylic acid (PAA) and bisLithium trifluoromethanesulfonylimide (LiTFSI) and perovskite solid electrolyte filler Li0.5La0.5Ti0.95 Zr0.05O3Uniformly mixing the components in a glove box according to a mass ratio of 4:3:3, heating the mixture at 200 ℃ for 3 hours, and melting and stirring the mixture to form an electrolyte composite solution;
(2) and pouring the electrolyte composite solution on a substrate, hot-pressing to form a composite electrolyte membrane with the thickness of 80 microns, cooling to normal temperature at the hot-pressing temperature of 80 ℃ and the pressure of 20Mpa to obtain the composite solid electrolyte.
Example 2
(1) Polyethylene oxide (PEO), lithium bis-fluorosulfonimide (LiFSI) and perovskite solid electrolyte filler Li0.5La0.5Ti0.85Zr0.05 Al0.1O3Uniformly mixing the components in a glove box according to the mass ratio of 5:3:2, heating the mixture at 300 ℃ for 2 hours, and melting and stirring the mixture to form an electrolyte composite solution;
(2) and pouring the electrolyte composite solution on a substrate, hot-pressing to form a composite electrolyte membrane with the thickness of 100 mu m, cooling to normal temperature at the hot-pressing temperature of 85 ℃ and the pressure of 15Mpa to obtain the composite solid electrolyte.
Example 3
(1) Polytetrafluoroethylene (PVDF), lithium bis (fluorosulfonyl) imide (LiFSI) and perovskite solid electrolyte filler Li0.5La0.5Ti0.9Zr0.05 Mn0.05O3Uniformly mixing the components according to the mass ratio of 6:2:2, heating the mixture at 150 ℃ for 2.5 hours, and melting and stirring the mixture to form an electrolyte composite solution;
(2) and pouring the electrolyte composite solution on a substrate, hot-pressing to a specified thickness to form a composite electrolyte membrane with the thickness of 30 microns, cooling to normal temperature at the hot-pressing temperature of 75 ℃ and the pressure of 25Mpa to obtain the composite solid electrolyte.
Comparative example 1
Comparative example 1 differs from example 1 in that: the perovskite solid electrolyte filler is not added, and the rest processes are completely the same.
The composite solid electrolytes obtained in examples 1 to 3 and comparative example 1 were examined for their properties, and the results are shown in Table 1: watch (A)
1. The result of the detection
| Detecting the index | Decomposition voltage (V) | Bulk conductivity (S. cm-1) |
| Example 1 | 4.8 | 10-4～10-5 |
| Example 2 | 4.7 | 10-4～10-5 |
| Example 3 | 4.8 | 10-4～10-5 |
| Comparative example 1 | 4.2 | 10-6 |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. A composite solid electrolyte, characterized in that the composite electrolyte material comprises a polymer, a lithium salt and a perovskite solid electrolyte filler.
2. The composite solid-state electrolyte of claim 1, wherein the perovskite solid-state electrolyte filler has a general chemical structure formula of Li0.5La0.5Ti1–xMxO3Wherein, M is a doping element,Xis the doping amount; m is selected from one or more of Sn, Al, Mn, Fe, Zr and Ge,Xthe range of (A) is 0.01 to 0.15.
3. The composite solid electrolyte of claim 1, wherein said polymer is selected from one or more of polyvinylidene fluoride, polyacrylic acid, polyvinyl cyanide, polyethylene oxide, and polymethacrylic acid.
4. The composite solid-state electrolyte of claim 1, wherein the lithium salt is selected from one or more of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium bistrifluoromethylsulphonylimide, lithium bistrifluorosulphonylimide, lithium bisoxalato borate, lithium perchlorate and lithium difluorooxalato borate.
5. The composite solid electrolyte of claim 1, wherein the mass ratio of the polymer to the lithium salt to the perovskite solid electrolyte filler is (4-6): (2-3): (2-3).
6. A method of preparing a composite solid electrolyte according to any one of claims 1 to 5, comprising the steps of:
(1) uniformly mixing a polymer, a lithium salt and a perovskite solid electrolyte filler, heating, melting and stirring to form an electrolyte composite solution;
(2) and pouring the electrolyte composite solution on a substrate, carrying out hot pressing to a specified thickness to form a composite electrolyte membrane, and cooling to normal temperature to obtain the composite solid electrolyte.
7. The preparation method according to claim 1, wherein in the step (1), the heating and melting temperature is 200-300 ℃ and the time is 2-3 h.
8. The method according to claim 1, wherein the hot pressing temperature in step (2) is 75 to 85 ℃ and the pressure is 15 to 25 MPa.
9. The method according to claim 1, wherein in the step (2), the thickness of the composite electrolyte membrane is 30 to 100 μm.
10. Use of a composite solid-state electrolyte according to any one of claims 1 to 5 in a lithium ion battery.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110559155.9A CN113363563A (en) | 2021-05-21 | 2021-05-21 | Composite solid electrolyte and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110559155.9A CN113363563A (en) | 2021-05-21 | 2021-05-21 | Composite solid electrolyte and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114373972A (en) * | 2022-01-14 | 2022-04-19 | 东莞富瑟尔科技有限公司 | Molten salt diffusion compounding device and method |
| CN115566269A (en) * | 2022-11-04 | 2023-01-03 | 深圳市合壹新能技术有限公司 | Method for producing solid electrolyte, solid battery, and electricity-using device |
| CN118173879A (en) * | 2024-04-25 | 2024-06-11 | 浙江蓝德能源科技发展有限公司 | A phase-change solid electrolyte and preparation method thereof |
| CN119994156A (en) * | 2025-04-11 | 2025-05-13 | 昆宇电源股份有限公司 | A solid electrolyte for solid-state lithium battery |
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| CN115566269A (en) * | 2022-11-04 | 2023-01-03 | 深圳市合壹新能技术有限公司 | Method for producing solid electrolyte, solid battery, and electricity-using device |
| CN118173879A (en) * | 2024-04-25 | 2024-06-11 | 浙江蓝德能源科技发展有限公司 | A phase-change solid electrolyte and preparation method thereof |
| CN119994156A (en) * | 2025-04-11 | 2025-05-13 | 昆宇电源股份有限公司 | A solid electrolyte for solid-state lithium battery |
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