CN112366293A - Solid metal lithium battery and preparation method thereof - Google Patents
Solid metal lithium battery and preparation method thereof Download PDFInfo
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
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Abstract
The invention discloses a solid-state metal lithium battery and a preparation method thereof, wherein the solid-state metal lithium battery comprises a negative electrode, a positive electrode, a high-voltage-resistant polymer electrolyte, a low-voltage-resistant polymer electrolyte coated on the surface of the metal lithium, and an organic flame retardant dispersed among the polymer electrolytes. The design of the battery can effectively inhibit lithium dendrites, improve the interface stability of the solid electrolyte and the positive and negative electrodes, and improve the chemical/electrochemical stability of the polymer electrolyte. Compared with the prior art, the invention has the following advantages: (1) the solid-state metal lithium battery disclosed by the invention uses the surface-modified lithium cathode, and the surface modification layer can effectively inhibit lithium dendrite and lithium corrosion degradation; (2) the solid-state metal lithium battery disclosed by the invention respectively uses the high-voltage-resistant and low-voltage-resistant polymers to be in contact with the positive electrode and the negative electrode, so that the oxidation and reduction decomposition of the polymers can be effectively inhibited, and meanwhile, the safety performance and the conductivity of the solid electrolyte can be further improved by adding the flame retardant.
Description
Technical Field
The invention relates to the field of novel solid-state batteries, in particular to a solid-state metal 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 a solid-state metal lithium battery and a preparation method thereof, aiming at the problems in the prior art, the solid-state metal lithium battery can solve the safety problem of a liquid electrolyte lithium battery and can also inhibit the interface reaction and the degradation of electrolyte, so that the lithium battery has both safety and excellent electrochemical performance.
The specific technical scheme is as follows:
a solid-state metal lithium battery comprises a metal lithium cathode, a positive electrode and a polymer electrolyte, and is characterized in that the metal lithium cathode is subjected to surface modification;
the polymer electrolyte is composed of lithium salt and polymer, and the polymer is selected from high-voltage-resistant polymer;
the surface modifier of the lithium negative electrode is composed of a polymer and a lithium salt, and the polymer is selected from low-voltage-resistant polymers.
The preparation method of the solid-state metal 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 high-voltage-resistant polymer and a lithium salt in an organic solvent, fully stirring and pouring the mixture on a glass matrix, and then drying the mixture in vacuum to obtain a polymer electrolyte membrane for later use;
3) and (3) laminating the positive electrode, the polymer electrolyte membrane and the modified lithium negative electrode, and rolling and packaging to obtain the solid metal lithium battery.
The invention uses the polymer electrolyte to assemble the all-solid-state metal 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; by using a high-voltage-resistant polymer electrolyte, the polymer can be inhibited from being oxidatively decomposed at a high voltage. Therefore, the interfacial reaction can be effectively inhibited, the degradation of the polymer can be prevented, and the cycle performance of the battery can be ensured. 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; preferably, the low voltage side polymer electrolyte contains 2 lithium salts, including a fluorine-containing lithium salt and a boron-containing lithium salt.
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 solid metal lithium battery.
In step 2):
preferably, the method comprises the following steps:
the high-voltage resistant polymer is selected from at least one of polycarbonate, polyimide, polytetrafluoroethylene, polyvinylidene fluoride and polyvinylidene fluoride-hexafluoropropylene;
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 organic flame retardant is selected from at least one of 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 solid-state metal lithium battery disclosed by the invention uses the surface-modified lithium cathode, and the surface modification layer can effectively inhibit lithium dendrite and lithium corrosion degradation;
(2) the solid-state metal lithium battery disclosed by the invention respectively uses the high-voltage-resistant and low-voltage-resistant polymers to be in contact with the positive electrode and the negative electrode, so that the oxidation and reduction decomposition of the polymers can be effectively inhibited, and meanwhile, 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 diagram of a solid-state lithium metal battery manufactured by the method of example 1.
Detailed Description
Example 1
Uniformly mixing polyethylene oxide, lithium hexafluorophosphate and lithium tetrafluoroborate in N-methyl pyrrolidone, 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 total weight of the lithium hexafluorophosphate and the lithium tetrafluoroborate to the weight of the polyethylene oxide is 1: 7; uniformly mixing polycarbonate and lithium perchlorate in N-methylpyrrolidone, fully stirring and pouring the mixture on a glass substrate, and performing vacuum drying at the temperature of 60 ℃ to obtain a polymer electrolyte membrane, wherein the weight ratio of the lithium perchlorate to the polycarbonate is 1: 7; lithium cobaltate positive electrode (LiCoO)2) Polymer electrolyte membrane, modified lithium negative electrode laminate, rolled, and then trifluoroethyl phosphate (weight of trifluoroethyl phosphate and total weight of polyethylene oxide and polycarbonate) was addedRatio of 5%), and aluminum-plastic packaging to obtain the solid-state metal lithium battery. 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, lithium bistrifluoromethanesulfonimide and lithium bisoxalateborate 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 total weight of the lithium bistrifluoromethanesulfonimide and the lithium bistrifluoromethanesulfonate to the polypropylene oxide is 1: 5; uniformly mixing polyimide and lithium bis (trifluoromethanesulfonyl) imide in N-methylpyrrolidone, fully stirring and pouring the mixture on a glass substrate, and performing vacuum drying at the temperature of 60 ℃ to obtain a polymer electrolyte membrane, wherein the weight ratio of the lithium bis (trifluoromethanesulfonyl) imide to the polyimide is 1: 5; nickel cobalt manganese ternary positive electrode (LiNi)0.6Co0.2Mn0.2O2) Rolling the polymer electrolyte membrane and the modified lithium cathode lamination, adding trifluoroethyl phosphite ester (the weight of the trifluoroethyl phosphite ester and the total weight ratio of polypropylene oxide to polyimide is 7 percent), and carrying out aluminum-plastic packaging to obtain the solid-state metal lithium battery.
Example 3
Uniformly mixing polyoxyethylene and polyoxybutylene (the weight ratio of the polyoxyethylene to the polyoxybutylene is 1: 1), lithium bis (fluorosulfonyl) imide and lithium difluoro (oxalato) borate in N-methylpyrrolidone, fully stirring and coating the mixture on the surface of metal lithium, and performing vacuum drying at 60 ℃ to obtain surface modified metal lithium, wherein the total weight ratio of the lithium bis (fluorosulfonyl) imide to the lithium difluoro (oxalato) borate to the total weight ratio of the polyoxyethylene to the polyoxypropylene is 1: 10; uniformly mixing polyvinylidene fluoride and lithium bis (oxalato) borate in N-methyl pyrrolidone, fully stirring and pouring the mixture on a glass substrate, and performing vacuum drying at 60 ℃ to obtain a polymer electrolyte membrane, wherein the weight ratio of the lithium bis (oxalato) borate to the polyvinylidene fluoride is 1: 10; nickel cobalt aluminum ternary positive electrode (LiNi)0.85Co0.10Al0.05O2) Rolling the polymer electrolyte membrane and the modified lithium cathode lamination, adding trifluoroethyl phosphite ester (the weight of the trifluoroethyl phosphite ester and the total weight ratio of polyoxyethylene, polyoxybutylene and polyvinylidene fluoride is 8%), and carrying out aluminum-plastic packaging to obtain the solid metal lithium battery.
Claims (7)
1. A solid-state lithium metal battery comprising a lithium metal anode, a cathode and a polymer electrolyte, wherein the lithium metal anode is surface modified.
2. The solid state lithium metal battery of claim 1,
the polymer electrolyte is composed of a lithium salt and a polymer selected from high voltage resistant polymers.
3. The solid state lithium metal battery of claim 1,
the surface modifier of the lithium negative electrode is composed of a polymer and a lithium salt, and the polymer is selected from low-voltage-resistant polymers.
4. A method of manufacturing a solid state lithium metal battery as claimed in 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 high-voltage-resistant polymer and a lithium salt in an organic solvent, fully stirring and pouring the mixture on a glass matrix, and then drying the mixture in vacuum to obtain a polymer electrolyte membrane for later use;
3) and (3) laminating the anode, the polymer electrolyte membrane and the modified lithium cathode, rolling, injecting an organic flame retardant, and packaging to obtain the solid metal lithium battery.
5. The method for preparing a solid-state lithium metal 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 preparing a solid-state lithium metal battery according to claim 4, wherein in step 2):
the high-voltage resistant polymer is selected from at least one of polycarbonate, polyimide, polytetrafluoroethylene, polyvinylidene fluoride and polyvinylidene fluoride-hexafluoropropylene;
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.
7. The method for preparing a solid-state lithium metal battery according to claim 4, wherein in step 3):
the organic flame retardant is selected from at least one of 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;
the active material of the positive electrode is selected from lithium-containing oxides;
the positive electrode is composed of a positive active material, a conductive agent and a polymer binder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113113667A (en) * | 2021-04-15 | 2021-07-13 | 浙江大学山东工业技术研究院 | High-voltage-resistant polyoxyethylene-based composite electrolyte and preparation method and application thereof |
| CN114512715A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Polyoxyethylene-based solid electrolyte, preparation method thereof and lithium ion battery |
| CN118017020A (en) * | 2024-04-02 | 2024-05-10 | 华南农业大学 | Preparation method of high-voltage-resistant solid polymer lithium metal battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113113667A (en) * | 2021-04-15 | 2021-07-13 | 浙江大学山东工业技术研究院 | High-voltage-resistant polyoxyethylene-based composite electrolyte and preparation method and application thereof |
| CN114512715A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Polyoxyethylene-based solid electrolyte, preparation method thereof and lithium ion battery |
| CN118017020A (en) * | 2024-04-02 | 2024-05-10 | 华南农业大学 | Preparation method of high-voltage-resistant solid polymer lithium metal battery |
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