CN111326789B - Semi-interpenetrating network flame-retardant solid lithium ion electrolyte, solid lithium battery and preparation method - Google Patents
Semi-interpenetrating network flame-retardant solid lithium ion electrolyte, solid lithium battery and preparation method Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a semi-interpenetrating network flame-retardant solid lithium ion electrolyte, a solid lithium battery and a preparation method thereof, wherein the semi-interpenetrating network flame-retardant solid electrolyte is prepared by in-situ polymerization and mainly comprises a cross-linking agent, a comonomer, a high molecular compound, a lithium salt, an inorganic compound and an initiator thereof, and the solid electrolyte added with an oxide electrolyte can further improve the conductivity of the electrolyte and the safety performance of the battery; the corresponding solid-state battery is prepared by adopting a lamination process, the semi-interpenetrating network flame-retardant solid-state electrolyte is coated on the surface of the anode, and the prepared solid-state lithium battery has higher safety, can meet the requirement of the market on the safety performance of the lithium battery, has simple and convenient process and is beneficial to large-scale production and application.
Description
Technical Field
The invention belongs to the technical field of solid-state batteries, and particularly relates to a semi-interpenetrating network flame-retardant solid-state lithium ion electrolyte, a solid-state lithium battery and a preparation method thereof.
Background
The electrolyte is an important component of the lithium ion battery, the electrolyte used at present is all organic compounds, the problems of liquid leakage, combustion and the like can occur under the extreme use condition, and the energy which can be stored in a specific volume of the current mainstream lithium ion battery is limited. The solid electrolyte is adopted to replace organic electrolyte in the traditional lithium ion battery, so that the safety problem of the battery can be well relieved, and the glass ceiling with energy density can be broken through.
The solid electrolyte used at present mainly comprises a polymer solid electrolyte and an inorganic ceramic solid electrolyte, wherein the polymer solid electrolyte has good flexibility, a stable interface and easy operability, but the conductivity of a lithium ion battery is lower; the inorganic solid electrolyte has higher ionic conductivity and flame retardance, but the interface contact is poorer, and the defects of the solid electrolyte can be well solved by using the polymer solid electrolyte and the inorganic solid electrolyte in a combined way.
For example, in the existing patents, CN201710847995, CN201811397878 and CN201811345429 are developed mainly for the flame retardant direction of electrolytes, so that the safety performance of the battery in the use process is improved, and for the safety of the lithium ion battery, a large amount of phosphate compounds are adopted, which are embedded into the graphite cathode to a certain extent, damage the overall structure of the graphite, and have poor cycle stability for the high-nickel positive electrode and the lithium sheet, so that the high safety and the high cycle performance of the lithium ion battery cannot be well considered.
Disclosure of Invention
In order to solve the technical problems, the invention provides a semi-interpenetrating network flame-retardant solid lithium ion electrolyte, a solid lithium battery and a preparation method thereof, aiming at the problem of poor safety performance of the existing high-energy density battery, a network structure polymer is prepared by adopting an in-situ polymerization method, and a high molecule with low molecular weight shuttles in the network structure to form the semi-interpenetrating polymer network flame-retardant solid electrolyte; the method for preparing the solid lithium battery is simple in production process, and the oxide electrolyte is added into the solid electrolyte, so that the conductivity of the electrolyte and the safety performance of the battery can be further improved.
The technical scheme adopted by the invention is as follows: the semi-interpenetrating network flame-retardant solid lithium ion electrolyte belongs to the category of composite electrolytes and comprises a cross-linking agent, a comonomer, a macromolecular compound, a lithium salt, an inorganic compound and an initiator;
0.3-5% of cross-linking agent, 10-40% of comonomer, 5-30% of high molecular compound, 20-50% of lithium salt, 10-50% of inorganic compound and 0.15-3% of initiator.
Preferably, the crosslinking agent is a multi-double bond functional group monomer;
preferably, the crosslinking agent is one or more of polyethylene glycol diacrylate, trimethylolpropane trimethacrylate, pentaerythritol tetraacrylate, pentaerythritol triacrylate, ethoxylated trimethylolpropane triacrylate, polyether polyacrylate.
Preferably, the comonomer is one or more of 3- (methacryloyloxy) propyltrimethoxysilane, vinyl-tris (methyl ethyl ketoxime) silane, perfluoroalkylethyl acrylate, heptafluorobutyl methacrylate, hexafluorobutyl methacrylate, octafluoropentyl methacrylate, hexafluoroisopropyl methacrylate, ethyl acrylate, butyl acrylate, isooctyl acrylate.
Preferably, the high molecular compound is one or more of polyacrylonitrile, polyvinylidene fluoride, polypropylene carbonate, polyethylene carbonate and polyethylene terephthalate with low molecular weight; the preferred molecular weight of the high molecular compound is selected between 500-10000.
Preferably, the lithium salt is one or more of lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium bistrifluoromethanesulfonylimide, lithium bistrifluorosulfonylimide, lithium difluorooxalato borate and lithium dioxaoxalato borate;
preferably, the inorganic compound is one or more of LATP, LAGP, LLZO, LPS, LGPS;
preferably, the initiator is one of dibenzoyl peroxide, dilauroyl peroxide, tert-butyl peroxy-2-ethylhexanoate and azobisisobutyronitrile.
The method for preparing the semi-interpenetrating network flame-retardant solid lithium ion electrolyte adopts a blending and in-situ polymerization method.
A solid-state lithium battery includes a semi-interpenetrating network flame-retardant solid-state lithium-ion electrolyte.
Preferably, the positive electrode active material is NCA, NCM111, NCM523, NCM622, NCM811, CrxOy、LiFePO4One of a lithium rich manganese base and sulfur;
preferably, the negative electrode is one or more of graphite, silicon, lithium metal, lithium aluminum alloy, lithium silicon alloy, and lithium boron alloy;
the method for preparing the solid lithium battery adopts a lamination process to prepare, and the semi-interpenetrating network flame-retardant solid electrolyte is coated on the surface of the anode;
specifically, a lamination process for repeatedly overlapping a negative electrode and a positive electrode coated with a solid electrolyte;
preferably, the semi-interpenetrating network flame-retardant solid electrolyte is coated on the surface of the anode by a roll coating method, and the coating area is larger than that of the anode;
preferably, the surface of the semi-interpenetrating network flame-retardant solid electrolyte battery coated with the positive electrode is polymerized by adopting the temperature of 60-80 ℃;
preferably, the solid-state battery is allowed to stand in a 60-degree oven for 24 hours after assembly.
The invention has the advantages and positive effects that: the semi-interpenetrating network structure has branched chains and high molecular combination with low molecular weight can improve the conductivity of the solid electrolyte and can increase the flexibility of the solid electrolyte; the semi-interpenetrating network flame-retardant solid electrolyte can form a film spontaneously, the mechanical strength is good, the selected comonomer and the high molecular compound have certain flame retardance, the prepared solid lithium battery can be broken through, the safety is high, and the selected comonomer can improve the cycle performance of the battery;
the solid electrolyte with the semi-interpenetrating structure is simple to prepare and can be produced on the existing production equipment.
Drawings
Fig. 1 is a cycle curve at 0.2C rate for a pouch cell prepared using a semi-interpenetrating network flame retardant solid electrolyte.
Detailed Description
The invention provides a semi-interpenetrating network flame-retardant solid lithium ion electrolyte, which comprises a cross-linking agent, a comonomer, a macromolecular compound, a lithium salt, an inorganic compound and an initiator. 0.3-5% of cross-linking agent, 10-40% of comonomer, 5-30% of high molecular compound, 20-50% of lithium salt, 10-50% of inorganic compound and 0.15-3% of initiator.
Wherein the comonomer is one or more of 3- (methacryloyloxy) propyl trimethoxy silane, vinyl-tri (methyl ethyl ketoxime) silane, perfluoroalkyl ethyl acrylate, heptafluorobutyl methacrylate, hexafluorobutyl methacrylate, octafluoropentyl methacrylate, hexafluoroisopropyl methacrylate, ethyl acrylate, butyl acrylate and isooctyl acrylate.
The cross-linking agent is a multi-double-bond functional group monomer, and specifically is one or more of polyethylene glycol diacrylate, trihydroxy methyl propane trimethacrylate, pentaerythritol tetraacrylate, pentaerythritol triacrylate, ethoxylated trimethylolpropane triacrylate and polyether polyacrylate.
The high molecular compound is one or more of polyacrylonitrile, polyvinylidene fluoride, polypropylene carbonate, polyethylene carbonate and polyethylene terephthalate with low molecular weight, and the preferable molecular weight of the high molecular compound is selected from 500-10000.
The lithium salt is one or more of lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium bistrifluoromethylsulfonyl imide, lithium bistrifluorosulfonimide, lithium difluorooxalato borate and lithium dioxaoxalato borate;
the inorganic compound is one or more of LATP, LAGP, LLZO, LPS and LGPS;
the initiator is one of dibenzoyl peroxide, dilauroyl peroxide, tert-butyl peroxy-2-ethylhexanoate and azobisisobutyronitrile.
The method for preparing the semi-interpenetrating network flame-retardant solid lithium ion electrolyte comprises the steps of blending the raw material components in proportion, and preparing the semi-interpenetrating network flame-retardant solid lithium ion electrolyte by an in-situ polymerization method.
A solid lithium battery comprising semi-interpenetrating network flame-retardant solid lithium ion electrolyte, wherein the positive active material adopts NCA, NCM111, NCM523, NCM622, NCM811 and CrxOy、LiFePO4One of a lithium rich manganese base and sulfur; the negative electrode is one or more of graphite, silicon, lithium metal, lithium aluminum alloy, lithium silicon alloy and lithium boron alloy; the solid electrolyte membrane is a semi-interpenetrating network flame-retardant solid lithium ion electrolyte, specifically a composite membrane comprising the semi-interpenetrating network flame-retardant solid lithium ion electrolyte, or a solid electrolyte membrane formed by directly coating the semi-interpenetrating network flame-retardant solid lithium ion electrolyte on the surface of a positive electrode.
The preparation method of the solid-state lithium battery comprises the following steps: coating the semi-interpenetrating network flame-retardant solid electrolyte on the surface of the anode by a roll coating method, wherein the coating area is larger than that of the anode; and initiating polymerization at 60-80 deg.C; and then assembling the negative electrode and the positive electrode into a solid battery by adopting a lamination process, and pressurizing and standing the solid battery in a 60 ℃ oven for 24 hours after the solid battery is assembled.
The solid electrolyte with the semi-interpenetrating network structure can improve the conductivity of the solid electrolyte and the flexibility of the solid electrolyte, and the preparation process of the solid electrolyte with the semi-interpenetrating network structure is simple, does not need to change equipment, and can be produced on the existing production equipment. In addition, the semi-interpenetrating network flame-retardant solid electrolyte and the corresponding solid lithium battery are prepared by in-situ polymerization, the semi-interpenetrating network flame-retardant solid electrolyte prepared by the method has higher ionic conductivity and better flame retardance, the prepared solid lithium battery has higher safety, and the production process is easy to realize.
The present invention is further described in detail by the following specific embodiments, which are only for illustrating the technical concept and features of the present invention and not for limiting the technical scope of the present invention, and the purpose of the present invention is to make those skilled in the art understand the content of the present invention and to implement the same, and all equivalent changes or modifications made according to the spirit of the present invention are within the protection scope of the present invention.
Example 1 preparation of semi-interpenetrating network flame retardant solid electrolyte
Weighing 1g of LLZTO, 0.2g of polypropylene carbonate and 0.75g of LiPF60.05g of pentaerythritol tetraacrylate and 0.0016g of azobisisobutyronitrile to 0.3g of 3- (methacryloyloxy) propylThe preparation method comprises the following steps of stirring a trimethoxy silane and perfluoroalkyl ethyl acrylate mixed solution for 4 hours, coating the solution on a polytetrafluoroethylene film, heating the solution at 60 ℃ for 24 hours to prepare a semi-interpenetrating network flame-retardant solid electrolyte 1, measuring the impedance of the semi-interpenetrating network flame-retardant solid electrolyte 1 by adopting alternating current impedance, and calculating the ionic conductivity of the semi-interpenetrating network flame-retardant solid electrolyte according to a conductivity formula. The time of the semi-interpenetrating network flame-retardant solid electrolyte is 10 seconds, and the extinguishing time is observed.
Example 2 preparation of semi-interpenetrating network flame retardant solid electrolyte
Weighing 1g of LLZTO, 0.2g of polyvinylidene fluoride and 0.75g of LiPF60.05g of pentaerythritol tetraacrylate and 0.0016g of azobisisobutyronitrile are added into 0.3g of 3- (methacryloyloxy) propyltrimethoxysilane and isooctyl acrylate mixed solution, stirred for 4h, then coated on a polytetrafluoroethylene film, heated at 60 ℃ for 24h to prepare the semi-interpenetrating network flame-retardant solid electrolyte 2, then the impedance of the semi-interpenetrating network flame-retardant solid electrolyte 2 is measured by adopting alternating current impedance, and the ionic conductivity of the semi-interpenetrating network flame-retardant solid electrolyte is calculated according to a conductivity formula. The time of the semi-interpenetrating network flame-retardant solid electrolyte is 10 seconds, and the extinguishing time is observed.
Example 3 preparation of semi-interpenetrating network flame retardant solid electrolyte
Weighing 0.8g of LLZTO, 0.2g of polyethylene carbonate and 0.75g of LiPF60.05g of pentaerythritol tetraacrylate and 0.0016g of azobisisobutyronitrile are added into 0.3g of 3- (methacryloyloxy) propyl trimethoxy silane and perfluoroalkyl ethyl acrylate mixed solution, stirred for 4h, then coated on a polytetrafluoroethylene film, heated for 24h at 60 ℃ to prepare and obtain the semi-interpenetrating network flame-retardant solid electrolyte 3, then the impedance of the semi-interpenetrating network flame-retardant solid electrolyte 3 is measured by adopting alternating current impedance, and the ionic conductivity of the semi-interpenetrating network flame-retardant solid electrolyte is calculated according to a conductivity formula. The time of the semi-interpenetrating network flame-retardant solid electrolyte is 10 seconds, and the extinguishing time is observed.
Preparation of the positive electrode: adding 1.5% of lithium bistrifluoromethanesulfonimide and 3% of polyacrylonitrile and polypropylene carbonate mixture into an NMP solution of PVDF, then adding carbon nano tubes and graphene, uniformly mixing, then adding a positive electrode active substance NCM811 with the mass concentration of 94%, stirring the above materials for 2-8h, and fully mixing to prepare a slurry. And coating the slurry on two sides of the aluminum foil with the thickness of 12um, performing forced air drying at 85 ℃ for 20 hours, and then preparing the positive plate through a sheet punching process.
The positive plate is used as a positive electrode, the lithium plate is used as a negative electrode, the semi-interpenetrating network flame-retardant solid electrolyte in the implementation 3 is coated on the surface of the positive electrode, the coating thickness is 15 microns, then the semi-interpenetrating network flame-retardant solid electrolyte is heated for 0.5h at 60 ℃, the laminate process is adopted to assemble the soft package battery, the prepared soft package battery is heated for 24h at 60 ℃, and then the hot press is used for extruding, so that the compact pole group is ensured.
The ionic conductivities and extinguishing times of the different semi-interpenetrating network flame retardant solid electrolytes are shown in table 1:
TABLE 1
As can be seen from the results of table 1 and fig. 1, the adopted comonomer or polymer compound is a fluorine-containing or silicon-containing compound, and the prepared electrolyte has a certain flame retardance and can improve the ionic conductivity of the electric solid electrolyte by adding the electrodeless nanoparticles; the soft package battery prepared by adopting the semi-interpenetrating network flame-retardant solid electrolyte can be circulated under the multiplying power of 0.2C, the solid battery prepared by adopting the semi-interpenetrating network flame-retardant solid electrolyte 3 has the best cycle performance, the cycle lasts for 40 weeks, and the capacity retention rate can reach 97%.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (9)
1. A semi-interpenetrating network flame-retardant solid lithium ion electrolyte is characterized in that: blending a cross-linking agent, a comonomer, a high molecular compound, a lithium salt, an inorganic compound and an initiator, and heating at 60-80 ℃ for in-situ polymerization to prepare the semi-interpenetrating network flame-retardant solid lithium ion electrolyte;
0.3-5% of cross-linking agent, 10-40% of comonomer, 5-30% of high molecular compound, 20-50% of lithium salt and 10-50% of inorganic compound, wherein the initiator accounts for 0.15-3% of the mass of the cross-linking agent and the comonomer;
the comonomer is one or more of 3- (methacryloyloxy) propyl trimethoxy silane, vinyl-tri (methyl ethyl ketoxime) silane, perfluoroalkyl ethyl acrylate, heptafluorobutyl methacrylate, hexafluorobutyl methacrylate, octafluoropentyl methacrylate, hexafluoroisopropyl methacrylate, ethyl acrylate, butyl acrylate and isooctyl acrylate;
the high molecular compound is one or more of polyacrylonitrile, polyvinylidene fluoride, polypropylene carbonate, polyvinyl carbonate and polyethylene glycol terephthalate with branched chain and low molecular weight, the molecular weight of the high molecular compound is 500-10000, a network structure polymer is prepared by adopting an in-situ polymerization method, and the high molecular with low molecular weight shuttles in the network structure to form the semi-interpenetrating polymer network flame-retardant solid electrolyte.
2. The semi-interpenetrating network flame-retardant solid-state lithium ion electrolyte of claim 1, wherein: the cross-linking agent is a multi-double-bond functional group monomer; the cross-linking agent is one or more of polyethylene glycol diacrylate, trihydroxy methyl propane trimethacrylate, pentaerythritol tetraacrylate, pentaerythritol triacrylate, ethoxylated trimethylolpropane triacrylate and polyether polyacrylate.
3. The semi-interpenetrating network flame-retardant solid-state lithium ion electrolyte of claim 2, wherein: the lithium salt is one or more of lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium bistrifluoromethylsulfonyl imide, lithium bistrifluorosulfonyl imide, lithium difluorooxalato borate and lithium dioxaoxalato borate.
4. The semi-interpenetrating network flame-retardant solid-state lithium ion electrolyte of claim 2, wherein: the inorganic compound is one or more of LATP, LAGP, LLZO, LPS and LGPS;
the initiator is one of dibenzoyl peroxide, dilauroyl peroxide, tert-butyl peroxy-2-ethylhexanoate and azobisisobutyronitrile.
5. The method for preparing the semi-interpenetrating network flame-retardant solid lithium ion electrolyte of any one of claims 1 to 4, characterized in that: and (2) blending a crosslinking agent, a comonomer, a high molecular compound, a lithium salt, an inorganic compound and an initiator, and heating at 60-80 ℃ for in-situ polymerization to prepare the semi-interpenetrating network flame-retardant solid lithium ion electrolyte.
6. A solid state lithium battery comprising the semi-interpenetrating network flame retardant solid state lithium ion electrolyte of any of claims 1-4.
7. The lithium solid state battery of claim 6, wherein: the positive active material is NCA, NCM111, NCM523, NCM622, NCM811, CrxOy、LiFePO4One of a lithium rich manganese base and sulfur;
the negative electrode is one or more of graphite, silicon, lithium metal, lithium aluminum alloy, lithium silicon alloy and lithium boron alloy.
8. A method of manufacturing a lithium solid state battery as claimed in claim 6 or 7, characterized in that: the semi-interpenetrating network flame-retardant solid electrolyte is coated on the surface of the anode; the semi-interpenetrating network flame-retardant solid electrolyte battery is coated on the surface of the anode and polymerization is initiated at the temperature of 60-80 ℃.
9. The method of manufacturing a solid lithium battery according to claim 8, characterized in that: the semi-interpenetrating network flame-retardant solid electrolyte is coated on the surface of the anode by a roll coating method, and the coating area is larger than that of the anode; and standing the solid-state battery in an oven at 60 ℃ for 24 hours after the solid-state battery is assembled.
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| CN111916747B (en) * | 2020-08-11 | 2023-10-20 | 天津力神电池股份有限公司 | High-safety polymer battery positive plate, polymer battery and battery preparation method |
| CN111987373B (en) * | 2020-08-11 | 2023-07-25 | 天津力神电池股份有限公司 | Solid electrolyte coating based on positive electrode protection, positive electrode plate and preparation method |
| CN112701348B (en) * | 2020-12-28 | 2024-01-12 | 南方科技大学 | Polymer solid electrolyte, all-solid lithium battery and preparation method thereof |
| KR20230134521A (en) * | 2021-01-22 | 2023-09-21 | 글로벌 그래핀 그룹, 인크. | Flame-retardant quasi-solid and solid-state electrolytes, lithium batteries and manufacturing methods |
| CN113851730A (en) * | 2021-08-20 | 2021-12-28 | 佛山(华南)新材料研究院 | High-temperature-resistant polymer electrolyte membrane and preparation method thereof |
| CN114716775B (en) * | 2022-03-21 | 2023-09-12 | 惠州市豪鹏科技有限公司 | Material for electrolyte separator, preparation method and battery |
| CN115483436A (en) * | 2022-08-01 | 2022-12-16 | 四川新能源汽车创新中心有限公司 | Solid electrolyte, high-safety lithium ion battery and preparation method thereof |
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