CN112366292A - All-solid-state lithium battery and preparation method thereof - Google Patents
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Abstract
The invention discloses an all-solid-state lithium battery and a preparation method thereof, wherein the all-solid-state lithium battery comprises a lithium cathode, a lithium-containing anode, a high-voltage-resistant polymer electrolyte polymerized in situ, a low-voltage-resistant polymer electrolyte directly coated on the surface of metal lithium and an organic flame retardant dispersed in the polymer electrolyte. The design of the battery can effectively inhibit lithium dendrites, improve the interface stability between the solid electrolyte and the anode and cathode, and improve the chemical/electrochemical stability of the polymer electrolyte. The all-solid-state lithium battery disclosed by the invention simultaneously meets the requirements of high energy density, high safety and high cycle stability.
Description
Technical Field
The invention relates to the field of novel solid-state batteries, in particular to an all-solid-state lithium battery and a preparation method thereof.
Background
In view of the increasingly severe energy and environmental issues, the development of more environmentally friendly new energy vehicles has become a common consensus both at home and abroad. However, compared with the existing internal combustion engine automobiles, the driving mileage of the existing electric automobiles is still short, so that the development of lithium batteries with high energy density is imperative. The direct use of metallic lithium instead of graphite negative electrode is an important method for improving the energy density of lithium batteries, but the problems of dendrite and dead lithium are generated in the circulation process of the metallic lithium, so that the performance is reduced and the safety is improved.
Although the above problems can be solved to some extent by using a solid electrolyte, the solid electrolyte also has the problem of interfacial contact with the positive and negative electrodes, for example, the ceramic electrolyte generally has interfacial reaction when contacting with the positive and negative electrodes, which causes the increase of interfacial resistance. In addition, the higher density of the ceramic electrolyte causes a decrease in the energy density of the battery. The polymer electrolyte has certain flexibility, low density and good contact with metal lithium, but the polymer can generate oxidation and reduction reactions at high voltage and low voltage respectively to initiate the degradation of the polymer and the reduction of the battery performance. In addition, although the safety of solid polymer electrolytes is improved compared to liquid organic electrolytes, general polymers are also flammable.
Disclosure of Invention
The invention discloses an all-solid-state lithium battery and a preparation method thereof, aiming at the problems in the prior art, the all-solid-state lithium battery can solve the safety problem of a liquid electrolyte lithium battery and can also inhibit the interface reaction and the degradation problem of electrolyte, so that the lithium battery has both safety and excellent electrochemical performance.
The specific technical scheme is as follows:
an all-solid-state lithium battery comprising a metallic lithium negative electrode, a lithium-containing positive electrode, and a solid-state polymer electrolyte, wherein the polymer electrolyte comprises a low voltage-resistant polymer electrolyte and a high voltage-resistant polymer electrolyte.
The high-voltage-resistant polymer electrolyte consists of lithium salt and a high-voltage-resistant polymer, wherein the high-voltage-resistant polymer is formed on the surface of the positive electrode through in-situ polymerization of monomers and is dispersed in the positive electrode.
The low-voltage-resistant polymer electrolyte is composed of lithium salt and a low-voltage-resistant polymer, and is directly coated on the surface of a lithium negative electrode.
The preparation method of the all-solid-state lithium battery comprises the following steps:
1) uniformly mixing a low-voltage-resistant polymer and a lithium salt in an organic solvent, fully stirring and coating on the surface of the metal lithium, and then carrying out vacuum drying to obtain surface modified metal lithium for later use;
2) uniformly mixing a monomer of a high-voltage-resistant polymer and a lithium salt, and fully stirring to obtain a high-voltage-resistant polymer electrolyte precursor for later use;
3) and laminating the positive electrode and the modified lithium negative electrode, carrying out battery packaging on the high-voltage resistant polymer electrolyte precursor, and heating and polymerizing to obtain the all-solid-state lithium battery.
The invention uses the polymer electrolyte to assemble the all-solid-state lithium battery, and has the advantages of high safety, high energy density, high mechanical performance and excellent battery performance. In the all-solid-state battery, the polymer with low voltage resistance is used for modifying the metal lithium, so that the polymer can be inhibited from being reduced and degraded by the metal lithium; the polymer electrolyte of the positive electrode is polymerized by an in-situ method, so that the polymer electrolyte has good contact with low-voltage-resistant polymer interfaces on the surfaces of the positive electrode and the lithium negative electrode, can permeate into gaps of the positive electrode, and can remarkably reduce interface electrolysis and the bulk resistance of the positive electrode. In addition, the acrylic ester uses a monomer containing a ring, and the acrylic ester is easy to generate a crosslinking reaction with the low-voltage-resistant polymer during polymerization, so that the interface performance between the low-voltage-resistant polymer and the high-voltage-resistant polymer is improved, and the diffusion of lithium ions is promoted. Therefore, the all-solid-state battery design can effectively inhibit the interface reaction, prevent the degradation of the polymer and ensure the cycle performance of the battery. Preferably, the phosphate flame retardant is added into the solid polymer, so that the safety and the conductivity of the polymer electrolyte can be improved, and the phosphate organism also plays a role of a surfactant, namely the interface compatibility between the high-voltage-resistant polymer and the low-voltage-resistant polymer is improved, and the diffusion capacity of lithium ions on the interface is improved. Further preferably, a fluorine-containing phosphate organic substance such as trifluoroethyl phosphate is used, and lithium fluoride, which is a decomposition product thereof, can further coat the lithium negative electrode to suppress lithium dendrite.
In step 1):
preferably, the method comprises the following steps:
the low-voltage resistant polymer is selected from at least one of polyethylene oxide, polypropylene oxide and polybutylene oxide;
the lithium salt is selected from at least one of lithium perchlorate, lithium trifluoromethanesulfonate, lithium bis (fluorosulfonyl) imide, lithium hexafluorophosphate, lithium bis (trifluoromethanesulfonyl) imide, lithium tetrafluoroborate, lithium difluorooxalate borate and lithium bis (oxalate) borate;
the weight ratio of the lithium salt to the polymer is 1: 5-1: 20.
Preferably, the thickness of the surface modification layer is 10-50 μm, and under the condition, the polymer electrolyte can effectively modify the metal lithium, does not influence lithium ion-rapid conduction, and does not influence the rate capability of the all-solid-state lithium battery.
In step 2):
preferably, the method comprises the following steps:
the high-voltage resistant polymer monomer is a ring-containing monomer and is selected from at least one of 2-cyclohexyl methacrylate, cyclohexyl acrylate and 4-tert-butyl cyclohexyl acrylate;
the lithium salt is selected from at least one of lithium perchlorate, lithium trifluoromethanesulfonate, lithium bis (fluorosulfonyl) imide, lithium hexafluorophosphate, lithium hexafluoroarsenate, lithium bis (trifluoromethanesulfonyl) imide, lithium tetrafluoroborate, lithium difluoro (oxalato) borate and lithium bis (oxalato) borate;
the weight ratio of the lithium salt to the polymer is 1: 5-1: 20.
Further preferably, the polymer electrolyte membrane has a thickness of 10 to 100 μm, and under such conditions, the polymer electrolyte membrane has mechanical properties, high lithium ion conductivity, and high energy density of the battery.
In step 3):
preferably, the method comprises the following steps:
the positive electrode is composed of a positive active substance, a conductive agent and a polymer binder, and metal aluminum is used as a collector. The positive active material is selected from lithium-containing oxide, and can be selected from at least one of commercially available lithium manganate, lithium cobaltate, lithium iron phosphate, lithium nickel manganese, lithium manganese phosphate, nickel cobalt aluminum ternary material, nickel cobalt manganese ternary material and lithium-rich layered material;
the packaging can be aluminum-plastic packaging, aluminum shell packaging and steel shell packaging;
the temperature of the thermal polymerization is 60-80 ℃;
the organic flame retardant is selected from triethyl phosphate, trifluoroethyl phosphite and triphenyl phosphate, and the amount of the organic flame retardant is 1-10% of the total weight of the high-voltage resistant polymer and the low-voltage resistant polymer.
Compared with the prior art, the invention has the following advantages:
(1) the all-solid-state lithium battery disclosed by the invention uses the surface modified lithium cathode, and the surface modified layer can effectively inhibit lithium dendrite and lithium corrosion degradation;
(2) the all-solid-state lithium battery disclosed by the invention has the advantages that the high-voltage-resistant polymer and the low-voltage-resistant polymer are respectively contacted with the positive electrode and the negative electrode, the oxidation and reduction decomposition of the polymer can be effectively inhibited, and the safety performance and the conductivity of the solid electrolyte can be further improved by adding the flame retardant.
Drawings
Fig. 1 is a structural view of an all solid-state lithium battery prepared by the method of example 1.
Detailed Description
Example 1
Uniformly mixing polyethylene oxide and lithium hexafluorophosphate in N-methylpyrrolidone, fully stirring and coating on the surface of the metal lithium, and performing vacuum drying at 60 ℃ to obtain surface modified metal lithium, wherein the weight ratio of the lithium hexafluorophosphate to the polyethylene oxide is 1: 5; uniformly mixing the 2-cyclohexyl methacrylate monomer and the lithium perchlorate, and fully stirring to obtain the high-voltage-resistant polymer electrolyte precursor, wherein the lithium perchlorate and the 2-cyclohexyl methacrylate monomer areThe weight ratio is 1: 5; nickel cobalt manganese ternary positive electrode (LiNi)0.6Co0.2Mn0.2O2) The high-voltage-resistant polymer electrolyte precursor and the modified lithium cathode lamination are added, trifluoroethyl phosphate (the weight of the trifluoroethyl phosphate and the total weight ratio of the polyoxyethylene to the 2-cyclohexyl methacrylate monomer is 6%) is added, aluminum plastic packaging is carried out, and the all-solid-state lithium battery is obtained by heating and in-situ polymerization at 70 ℃. Fig. 1 is a schematic view of the resulting solid-state lithium battery, in which polymer electrolyte a is a high-voltage-resistant polymer electrolyte and polymer electrolyte B is a low-voltage-resistant polymer electrolyte.
Example 2
Uniformly mixing polypropylene oxide and lithium bis (trifluoromethanesulfonyl) imide in N-methylpyrrolidone, fully stirring, coating on the surface of metal lithium, and performing vacuum drying at 60 ℃ to obtain surface modified metal lithium, wherein the weight ratio of the bis (trifluoromethanesulfonyl) imide to the polypropylene oxide is 1: 7; uniformly mixing cyclohexyl acrylate monomers and lithium bis (fluorosulfonyl) imide, and fully stirring to obtain a high-voltage-resistant polymer electrolyte precursor, wherein the weight ratio of the lithium bis (fluorosulfonyl) imide to the cyclohexyl acrylate monomers is 1: 7; nickel cobalt aluminum ternary positive electrode (LiNi)0.85Co0.10Al0.05O2) The high-voltage-resistant polymer electrolyte precursor and the modified lithium cathode lamination are added with trifluoroethyl phosphite ester (the weight of the trifluoroethyl phosphite ester and the total weight ratio of the polyoxypropylene to the cyclohexyl acrylate monomer is 8 percent), aluminum-plastic packaging is carried out, and the all-solid-state lithium battery is obtained by heating and in-situ polymerization at 70 ℃.
Example 3
Uniformly mixing polyoxyethylene and polyoxypropylene (the weight ratio of the polyoxyethylene to the polyoxypropylene is 1: 1) and lithium bistrifluoromethanesulfonylimide in N-methylpyrrolidone, fully stirring and coating the mixture on the surface of the lithium metal, and performing vacuum drying at 60 ℃ to obtain surface modified lithium metal, wherein the weight ratio of the lithium bistrifluoromethanesulfonylimide to the total weight ratio of the polyoxyethylene to the polyoxypropylene is 1: 10; 4-tert-butyl cyclohexyl acrylate monomer and lithium tetrafluoroborate are evenly mixed byFully stirring to obtain a high-voltage-resistant polymer electrolyte precursor, wherein the weight ratio of the lithium tetrafluoroborate to the 4-tert-butyl cyclohexyl acrylate is 1: 10; lithium cobaltate positive electrode (LiCoO)2) The high-voltage-resistant polymer electrolyte precursor and the modified lithium cathode lamination are added with trifluoroethyl phosphite ester (the weight of the trifluoroethyl phosphite ester and the total weight ratio of polyoxyethylene and polyoxybutylene to 4-tert-butyl cyclohexyl acrylate monomer are 10%), aluminum plastic packaging is carried out, and the all-solid-state lithium battery is obtained by heating and in-situ polymerization at 70 ℃.
Claims (7)
1. An all-solid-state lithium battery comprising a metallic lithium negative electrode, a lithium-containing positive electrode, and a solid-state polymer electrolyte, wherein the polymer electrolyte comprises a low voltage-resistant polymer electrolyte and a high voltage-resistant polymer electrolyte.
2. The all solid-state lithium battery according to claim 1,
the high-voltage-resistant polymer electrolyte consists of lithium salt and a high-voltage-resistant polymer, wherein the high-voltage-resistant polymer is formed on the surface of the positive electrode through in-situ polymerization of monomers and is dispersed in the positive electrode.
3. The all solid-state lithium battery according to claim 1,
the low-voltage-resistant polymer electrolyte is composed of lithium salt and a low-voltage-resistant polymer, and is directly coated on the surface of a lithium negative electrode.
4. A method for producing an all-solid-state lithium battery according to any one of claims 1 to 3, comprising:
1) uniformly mixing a low-voltage-resistant polymer and a lithium salt in an organic solvent, fully stirring and coating on the surface of the metal lithium, and then carrying out vacuum drying to obtain surface modified metal lithium for later use;
2) uniformly mixing a monomer of a high-voltage-resistant polymer and a lithium salt, and fully stirring to obtain a high-voltage-resistant polymer electrolyte precursor for later use;
3) and (3) stacking the positive electrode, the modified lithium negative electrode, the high-voltage-resistant polymer electrolyte precursor and the organic flame retardant, packaging the battery, and heating and polymerizing to obtain the all-solid-state lithium battery.
5. The method for producing an all-solid-state lithium battery according to claim 4, wherein in step 1):
the low-voltage resistant polymer is selected from at least one of polyethylene oxide, polypropylene oxide and polybutylene oxide;
the lithium salt is selected from at least one of lithium perchlorate, lithium trifluoromethanesulfonate, lithium bis (fluorosulfonyl) imide, lithium hexafluorophosphate, lithium bis (trifluoromethanesulfonyl) imide, lithium tetrafluoroborate, lithium difluorooxalate borate and lithium bis (oxalate) borate;
the weight ratio of the lithium salt to the polymer is 1: 5-1: 20.
6. The method for producing an all-solid-state lithium battery according to claim 4, wherein in step 2):
the high-voltage resistant polymer monomer is a ring-containing monomer and is selected from at least one of 2-cyclohexyl methacrylate, cyclohexyl acrylate and 4-tert-butyl cyclohexyl acrylate;
the lithium salt is selected from at least one of lithium perchlorate, lithium trifluoromethanesulfonate, lithium bis (fluorosulfonyl) imide, lithium hexafluorophosphate, lithium hexafluoroarsenate, lithium bis (trifluoromethanesulfonyl) imide, lithium tetrafluoroborate, lithium difluoro (oxalato) borate and lithium bis (oxalato) borate;
the weight ratio of the lithium salt to the polymer monomer is 1: 5-1: 20.
7. The method for producing an all-solid-state lithium battery according to claim 4, wherein in step 3):
the organic flame retardant is selected from but not limited to triethyl phosphate, trifluoroethyl phosphite and triphenyl phosphate, and the amount of the organic flame retardant is 1 to 10 percent of the total weight of the high-voltage resistant polymer and the low-voltage resistant polymer;
the active material of the positive electrode is selected from lithium-containing oxides;
the positive electrode consists of a positive active material, a conductive agent and a polymer binder;
the temperature of the thermal polymerization is 60 ℃ to 80 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113140731A (en) * | 2021-03-29 | 2021-07-20 | 浙江大学 | All-solid-state lithium battery and preparation method thereof |
| CN113258132A (en) * | 2021-05-11 | 2021-08-13 | 合肥工业大学 | Solid electrolyte, preparation method thereof and solid battery |
| CN116169366A (en) * | 2022-12-27 | 2023-05-26 | 力神（青岛）新能源有限公司 | Solid-state lithium battery, preparation method thereof and electric equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113140731A (en) * | 2021-03-29 | 2021-07-20 | 浙江大学 | All-solid-state lithium battery and preparation method thereof |
| CN113140731B (en) * | 2021-03-29 | 2022-08-05 | 浙江大学 | All-solid-state lithium battery and preparation method thereof |
| CN113258132A (en) * | 2021-05-11 | 2021-08-13 | 合肥工业大学 | Solid electrolyte, preparation method thereof and solid battery |
| CN113258132B (en) * | 2021-05-11 | 2022-09-06 | 合肥工业大学 | Solid electrolyte, preparation method thereof and solid battery |
| CN116169366A (en) * | 2022-12-27 | 2023-05-26 | 力神（青岛）新能源有限公司 | Solid-state lithium battery, preparation method thereof and electric equipment |
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