CN114614097A - Electrolyte for ternary cathode material lithium ion battery and manufacturing method of lithium ion battery - Google Patents
Electrolyte for ternary cathode material lithium ion battery and manufacturing method of lithium ion battery Download PDFInfo
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- CN114614097A CN114614097A CN202210190687.4A CN202210190687A CN114614097A CN 114614097 A CN114614097 A CN 114614097A CN 202210190687 A CN202210190687 A CN 202210190687A CN 114614097 A CN114614097 A CN 114614097A
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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
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
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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
- 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
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- H01M10/05—Accumulators with non-aqueous electrolyte
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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
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- H01M2300/0017—Non-aqueous electrolytes
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Abstract
The invention discloses an electrolyte for a ternary anode material lithium ion battery, which comprises the following components in percentage by mass: 70-80% of double bond-containing monomer; 10-20% of lithium salt; 0-10% of organic solvent containing active hydrogen atoms, and is not 0. The invention also discloses a manufacturing method of the ternary cathode material lithium ion battery. The electrolyte provided by the invention can be subjected to polymerization reaction under the catalysis of residual alkali of a ternary positive electrode material, so that a polymer coating layer is formed on the surface of a positive electrode plate, the safety of a lithium ion battery is obviously improved, the polymerization condition is mild, the preparation method is simple, and the large-scale production is very easy to realize.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to electrolyte for a ternary cathode material lithium ion battery and a manufacturing method of the lithium ion battery.
Background
The lithium ion secondary battery gradually establishes a wide market by virtue of the advantages of high working voltage, long cycle life, high charging and discharging speed and the like, and plays an important role in the fields of small electronic products such as mobile phones, computers, electric tools and the like.
The development of electric vehicles and energy storage fields is more severe for the use conditions of lithium ion batteries, and particularly under extreme conditions (high temperature), the cycle performance of the batteries needs to be ensured. However, due to the existence of the liquid electrolyte in the lithium ion batteries widely used at present, the battery core is very easy to catch fire or even explode under the high-temperature condition or violent impact, and the safety performance is very high. In order to solve the problems, a polymer electrolyte or an electrodeless electrolyte is produced, but the electronic conductivity of the polymer electrolyte is low and cannot be compared with that of a liquid electrolyte, meanwhile, the preparation of the polymer electrolyte is relatively complicated, the requirement on polymerization conditions is high, and the current polymerization types of polymers and the polymerization types are various, so that the manufacturing process is complicated and the cost is overhigh, for example, Chinese patent 201810615609.8 relates to the preparation of a self-crosslinking composite solid electrolyte and an all-solid-state lithium ion battery formed by the self-crosslinking composite solid electrolyte, and the polymer electrolyte is obtained by crosslinking and curing with a nano inorganic substance, so that the manufacturing process is complicated; chinese patent 201710097194.5 relates to an electrochemical regulation atom transfer radical polymerization method under the action of alkali, which adopts an electrochemical method to carry out polymerization in the battery, and needs to change the formation process of the battery, thus increasing the electricity consumption cost. The methods improved by the patents need to change the existing lithium ion battery manufacturing process, and are not beneficial to the large-scale production of the polymer lithium ion battery. Meanwhile, a small amount of additive is generally required to be added during polymerization, but the addition of the additive has certain damage to the electrical property of the battery; on the other hand, the strong base exists in the positive electrode material of the ternary positive electrode material lithium ion battery, and the capacity exertion of the battery is damaged to a certain extent.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides electrolyte for a ternary cathode material lithium ion battery and a manufacturing method of the lithium ion battery, which can realize large-scale production of polymer lithium ion batteries and improve the high-temperature cycle life and safety of the batteries on the basis of not changing the existing lithium ion battery manufacturing process.
The invention provides an electrolyte for a ternary cathode material lithium ion battery, which comprises the following components in percentage by mass: 70-80% of double bond-containing monomer; 10-20% of lithium salt; 0-10% of organic solvent containing active hydrogen atoms, and is not 0.
Preferably, the double bond-containing monomer is at least one of acrylate and derivatives thereof, styrene, acrylic acid, acrylamide, acrylonitrile, trimethylene cyclic carbonate, 2-dimethyltrimethylene cyclic carbonate and lactide.
Preferably, the organic solvent containing active hydrogen atoms is at least one of ethylene glycol, diethylene glycol, polyethylene glycol, 1, 2-propylene glycol, polypropylene glycol, 1, 3-propylene glycol, 1, 4-butylene glycol, polybutylene glycol, 1, 5-pentanediol, 1, 6-hexanediol, 2, 4, 6-hexanetriol, 1, 1, 1-trimethylolpropane, pentaerythritol, sorbitol, polyepichlorohydrin, polyethylene glycol mono (meth) acrylate, polypropylene glycol mono (meth) acrylate, and methoxypolyethylene glycol mono (meth) acrylate.
Preferably, the lithium salt is at least one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium bis (oxalato) borate, lithium difluoro (oxalato) borate, lithium bis (fluorosulfonyl) imide and lithium bis (trifluoromethanesulfonyl) imide.
The preparation method of the electrolyte for the ternary cathode material lithium ion battery comprises the steps of uniformly mixing the double-bond-containing monomer and the organic solvent containing active hydrogen atoms to obtain a mixed solution, and then dissolving lithium salt in the mixed solution to obtain the ternary cathode material lithium ion battery electrolyte.
A method for manufacturing a ternary cathode material lithium ion battery comprises the following steps:
s1, assembling the diaphragm, the positive plate and the negative plate into a battery cell;
s2, injecting the electrolyte into the battery cell, firstly carrying out primary polymerization in an environment with dew point temperature less than or equal to-50 ℃, then sealing the battery cell, and continuing polymerization until the reaction is complete.
Preferably, in S2, the temperature of the preliminary polymerization is 30-50 ℃ and the polymerization time is 10-15 h.
Preferably, in S2, the polymerization is continued at a temperature of 40 to 50 ℃ for a time of 20 to 30 hours.
Preferably, the positive plate comprises a positive current collector and a positive active layer arranged on the positive current collector, the positive active layer comprises a positive material, and the positive material is at least one of lithium cobaltate, lithium nickelate, lithium manganese oxide, lithium manganate, lithium nickel manganese oxide, lithium rich manganese base, lithium manganese iron phosphate, lithium nickel cobalt aluminate, lithium nickel cobalt manganate, lithium iron phosphate and lithium vanadium phosphate.
Preferably, the negative electrode plate comprises a negative electrode current collector and a negative electrode active layer arranged on the negative electrode current collector, the negative electrode active layer comprises a negative electrode material, and the negative electrode material is at least one of metal lithium, metal lithium alloy, graphite, hard carbon, lithium metal nitride, antimony oxide, carbon germanium composite material, carbon silicon composite material, lithium titanate and lithium titanium oxide.
Preferably, the membrane is at least one of polyethylene, polypropylene and polyvinylidene fluoride.
In the present invention, both the preliminary polymerization and the continuous polymerization are carried out in an anhydrous and oxygen-free environment.
A ternary cathode material lithium ion battery is prepared by the preparation method.
The invention has the following beneficial effects:
the invention provides an electrolyte for a ternary anode material lithium ion battery, which comprises a double-bond monomer, a lithium salt and an organic solvent containing active hydrogen atoms, can be catalyzed by residual alkali on the surface of the ternary anode material, and can generate nucleophilic reaction in the presence of the active hydrogen atoms, so that double bonds are broken, the monomer is polymerized to form a polymer, and a polymer layer is gradually formed on the surface of an anode plate to play a role in protection, thereby obviously improving the safety of the lithium ion battery, and having the following advantages: (1) the in-situ polymerization inside the battery is simple; (2) the polymerization condition is mild, and no other initiator is added to influence the electrical property; (3) the catalyst used in the polymerization process is residual alkali on the surface of the ternary cathode material, so that part of the residual alkali can be consumed while the monomer is polymerized to form a polymer layer, and the improvement of the electrical property of the battery is facilitated; (4) the manufacturing process of the lithium ion battery is not required to be additionally added, and the large-scale production of the polymer lithium ion battery is facilitated.
Drawings
Fig. 1 is a DSC test curve of a full-current positive electrode of the ternary positive electrode material lithium ion battery of example 1 of the present invention and the ternary positive electrode material lithium ion battery of comparative example 1 using a conventional electrolyte.
Fig. 2 is a transmission electron microscope image of the surface of the positive electrode after the battery is disassembled after the polymerization in example 1 of the present invention is completed.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
Preparing an electrolyte:
uniformly mixing mono (meth) acrylic acid polypropylene glycol and lactide in an inert atmosphere glove box with the water content of less than 5ppm to obtain a mixed solution, and then dissolving lithium salt LiFSI in the mixed solution to obtain an electrolyte; wherein the mass percent of each component is as follows: 70% of lactide, 20% of lithium salt LiFSI and 10% of mono (methyl) acrylic acid polypropylene glycol.
Assembling a ternary cathode material lithium ion battery (a buckling battery):
adding a positive electrode material NMC (523), a binder PVDF and a conductive agent SuperP into an organic solvent NMP according to a mass ratio of 8:1:1 to mix into paste, uniformly coating the paste on an aluminum foil with the thickness of 15 mu m, and performing the procedures of drying, rolling and slicing to obtain a positive electrode sheet;
graphite, a binder CMC and deionized water are mixed according to a mass ratio of 8:1:1, then uniformly coating the mixture on a copper foil with the thickness of 15 mu m, and obtaining a negative plate through the procedures of drying, rolling and slicing;
and assembling the positive plate, the negative plate and the diaphragm Cellgard2400 into a charging battery, standing in a vacuum oven at 45 ℃ for 12 hours, sealing, and continuously placing in the oven for 24 hours to obtain the ternary positive material lithium ion battery.
Example 2
Preparing an electrolyte:
uniformly mixing mono (methyl) acrylic acid polyethylene glycol and acrylic acid in an inert atmosphere glove box with the water content of less than 5ppm to obtain a mixed solution, and then dissolving lithium hexafluorophosphate in the mixed solution to obtain an electrolyte; wherein the mass percent of each component is as follows: 70% of acrylic acid, 20% of lithium hexafluorophosphate and 10% of mono (methyl) acrylic acid polyethylene glycol.
The method for assembling the lithium ion battery with ternary cathode material is the same as that of example 1.
Example 3
In an inert atmosphere glove box with the moisture content of less than 5ppm, uniformly mixing ethylene glycol and acrylamide to obtain a mixed solution, and then dissolving lithium difluoro (oxalato) borate in the mixed solution to obtain an electrolyte; wherein the mass percent of each component is as follows: 80% of acrylamide, 10% of lithium difluoro (oxalato) borate and 10% of ethylene glycol.
The method for assembling the lithium ion battery with ternary cathode material is the same as that of example 1.
Comparative example 1
Comparative example 1 is a lithium ion battery using a ternary cathode material of a commercial electrolyte, as follows
Adding a positive electrode material NMC (523), a binder PVDF and a conductive agent SuperP into an organic solvent NMP according to a mass ratio of 8:1:1 to mix into paste, uniformly coating the paste on a 15-micron aluminum foil, and performing the procedures of drying, rolling and slicing to obtain a positive electrode sheet;
graphite, a binder CMC and deionized water are mixed according to a mass ratio of 8:1:1, then uniformly coating the mixture on a copper foil with the thickness of 15 mu m, and obtaining a negative plate through the procedures of drying, rolling and slicing;
and assembling the positive plate, the negative plate, a diaphragm Cellgard2400 and electrolyte into the buckling battery, wherein the model of the electrolyte is New Zezhou U20.
The assembled cells of example 1 and comparative example 1 were subjected to the following performance tests:
DSC test: and (3) performing constant current charging at 0.1 ℃, performing constant voltage charging at 0.1 ℃ to 4.3V, and performing DSC test for detecting full charge.
And (4) carrying out cycle testing, wherein the process steps are as follows: constant current of 0.1C, constant voltage charging of 0.1C to 4.3V, standing for 10min, constant current discharging of 0.1C to 3.0V; constant current of 0.2C, constant voltage charging of 0.2C to 4.3V, standing for 10min, constant current discharging of 0.2C to 3.0V; constant current of 0.33C, constant voltage charging of 0.33C to 4.3V, standing for 10min, constant current discharging of 0.33C to 3.0V; constant current of 0.5 deg.C, constant voltage charging of 0.5 deg.C to 4.3V, standing for 10min, constant current discharging of 0.5 deg.C to 3.0V; and (3) carrying out constant current at 1C, then carrying out constant voltage charging at 1C to 4.3V, standing for 10min, then carrying out constant current discharging at 1C to 3.0V, and finally carrying out charge-discharge at 0.1C until the cycle is completed for 100 circles, wherein the data are shown in the following table 1.
TABLE 1
As can be seen from table 1, the battery in which the positive electrode was coated by the polymerization of the electrolyte solution containing the polymer had no significant effect on the capacity development as compared with the conventional battery.
Fig. 1 is a DSC test curve for full charge for a lithium ion battery of example 1 of the present invention and a conventional electrolyte lithium ion battery of comparative example 1, wherein the curve labeled as a polymer-coated NCM positive electrode represents example 1 and the curve labeled as a conventional NCM positive electrode represents comparative example 1. The result shows that the full-charge electricity-detained battery prepared in the example 1 has better thermal stability than the electricity-detained battery prepared conventionally in the comparative example 1, the heat release is reduced by 153.8J/g and is reduced by about 43%, the peak temperature is also improved by 3.3 ℃, and the lithium ion battery of the invention has better safety.
FIG. 2 is a transmission electron microscope image of the surface of the anode after the battery is disassembled after the polymerization is completed in example 1 of the present invention, and the image shows that there is a layer of obvious coating on the surface of the anode.
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 electrolyte for the ternary cathode material lithium ion battery is characterized by comprising the following components in percentage by mass: 70-80% of double bond-containing monomer; 10-20% of lithium salt; 0-10% of organic solvent containing active hydrogen atoms, and is not 0.
2. The electrolyte for the ternary cathode material lithium ion battery according to claim 1, wherein the double bond-containing monomer is at least one of acrylates and derivatives thereof, styrene, acrylic acid, acrylamide, acrylonitrile, trimethylene cyclic carbonate, 2-dimethyltrimethylene cyclic carbonate, and lactide.
3. The electrolyte for a ternary positive electrode material lithium ion battery according to claim 1, wherein the organic solvent containing active hydrogen atoms is at least one of ethylene glycol, diethylene glycol, polyethylene glycol, 1, 2-propylene glycol, polypropylene glycol, 1, 3-propylene glycol, 1, 4-butylene glycol, polybutylene glycol, 1, 5-pentanediol, 1, 6-hexanediol, 2, 4, 6-hexanetriol, 1, 1, 1-trimethylolpropane, pentaerythritol, sorbitol, polyepichlorohydrin, polyethylene glycol mono (meth) acrylate, polypropylene glycol mono (meth) acrylate, and methoxypolyethylene glycol mono (meth) acrylate.
4. The electrolyte for a ternary positive electrode material lithium ion battery according to claim 1, wherein the lithium salt is at least one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium bis (oxalato) borate, lithium difluoro (oxalato) borate, lithium bis (fluorosulfonyl) imide and lithium bis (trifluoromethanesulfonyl) imide.
5. The preparation method of the electrolyte for the ternary cathode material lithium ion battery according to any one of claims 1 to 4, characterized in that the electrolyte is obtained by uniformly mixing the double bond-containing monomer and the organic solvent containing active hydrogen atoms to obtain a mixed solution, and then dissolving lithium salt in the mixed solution.
6. A method for manufacturing a ternary cathode material lithium ion battery is characterized by comprising the following steps:
s1, assembling the diaphragm, the positive plate and the negative plate into a battery cell;
s2, injecting the electrolyte of any claim 1-4 into the battery core, initially polymerizing in an environment with dew point temperature less than or equal to-50 ℃, sealing the battery core, and continuing to polymerize until the reaction is complete.
7. The method for manufacturing the ternary cathode material lithium ion battery according to claim 6, wherein in S2, the temperature of the preliminary polymerization is 30-50 ℃, and the polymerization time is 10-15 h.
8. The method for manufacturing the ternary cathode material lithium ion battery of claim 6, wherein in S2, the temperature for the continuous polymerization after the battery is sealed is 40-50 ℃ and the time is 20-30 h.
9. The method of claim 6, wherein the positive plate includes a positive current collector and a positive active layer disposed on the positive current collector, the positive active layer includes a positive material, and the positive material is at least one of lithium cobaltate, lithium nickelate, lithium manganese oxide, lithium manganate, lithium nickel manganate, lithium rich manganese base, lithium manganese phosphate, lithium nickel cobalt aluminate, lithium nickel cobalt manganate, lithium iron phosphate, and lithium vanadium phosphate;
the negative plate comprises a negative current collector and a negative active layer arranged on the negative current collector, the negative active layer comprises a negative material, and the negative material is at least one of metal lithium, metal lithium alloy, graphite, hard carbon, lithium metal nitride, antimony oxide, a carbon germanium composite material, a carbon silicon composite material, lithium titanate and lithium titanium oxide.
10. A lithium ion battery made of a ternary cathode material, characterized by being prepared by the preparation method of any one of claims 6 to 9.
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| CN111540948A (en) * | 2020-05-09 | 2020-08-14 | 中国乐凯集团有限公司 | Composite solid polymer electrolyte membrane and preparation method and application thereof |
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| CN113258132A (en) * | 2021-05-11 | 2021-08-13 | 合肥工业大学 | Solid electrolyte, preparation method thereof and solid battery |
| CN113346128A (en) * | 2020-07-30 | 2021-09-03 | 道克特斯(天津)新能源科技有限公司 | Semi-solid/solid battery prepared by electrochemical oxidation-reduction method and method |
| CN114069036A (en) * | 2020-08-07 | 2022-02-18 | 北京石墨烯研究院 | Gel electrolyte and composition thereof, flexible lithium ion battery and preparation method thereof |
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2022
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| JPH11345628A (en) * | 1998-06-03 | 1999-12-14 | Daiso Co Ltd | Lithium polymer battery |
| CN104752761A (en) * | 2013-12-31 | 2015-07-01 | 比亚迪股份有限公司 | Multihole self-crosslinking gel polymer electrolyte and application of multihole self-crosslinking gel polymer electrolyte in lithium ion battery |
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| CN114069036A (en) * | 2020-08-07 | 2022-02-18 | 北京石墨烯研究院 | Gel electrolyte and composition thereof, flexible lithium ion 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 |
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