CN111276747A - High-voltage lithium ion battery electrolyte and preparation method thereof - Google Patents
High-voltage lithium ion battery electrolyte and preparation method thereof Download PDFInfo
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- CN111276747A CN111276747A CN202010242947.9A CN202010242947A CN111276747A CN 111276747 A CN111276747 A CN 111276747A CN 202010242947 A CN202010242947 A CN 202010242947A CN 111276747 A CN111276747 A CN 111276747A
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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
- H01M10/0567—Liquid materials characterised by the additives
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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
- H01M10/052—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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- 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
Abstract
The invention relates to the technical field of lithium ion batteries, and particularly discloses a high-voltage lithium ion battery electrolyte and a preparation method thereof. The high-voltage lithium ion battery electrolyte is characterized in that: the electrolyte consists of an anhydrous organic solvent, lithium salt and a functional additive, wherein the functional additive is a mixture of cyano sulfate, fluoroethylene carbonate and 3-fluoro-1, 3-propane sultone, the content of the functional additive accounts for 5-15% of the total mass of the electrolyte, and the anhydrous organic solvent is linear carbonate and cyclic carbonate. The invention effectively improves the oxidation resistance of the SEI film of the electrolyte during the initial formation by combining various functional additives, further obviously improves the cycle first reflection of the lithium ion battery under high voltage, simultaneously has excellent charge and discharge performance, and is suitable for wide popularization and application.
Description
(I) technical field
The invention relates to the technical field of lithium ion batteries, in particular to a high-voltage lithium ion battery electrolyte and a preparation method thereof.
(II) background of the invention
Since their successful commercialization by sony corporation in 1991, lithium ion batteries have rapidly dominated the field of portable electronic devices such as mobile phones, notebook computers, video cameras, etc., with their advantages of high energy density, high operating voltage plateau, no memory effect, low self-discharge rate, etc. With the rapid development of the fields of hybrid electric vehicles and pure electric vehicles, lithium ion batteries, which are ideal power sources for power vehicles, face unprecedented opportunities and challenges. The development of lithium ion batteries with higher energy density has become a hot spot of research today. The development of high voltage positive electrode materials is one of the important approaches for the development of high energy density lithium ion batteries. However, the conventional electrolyte is likely to cause side reactions on the surface of the positive electrode material, which affects the performance of the high-voltage positive electrode material. Therefore, the development of high voltage electrolytes is imminent.
The traditional electrolyte is easy to oxidize and decompose under high voltage, and then can generate a large amount of gas, so that the internal pressure of the battery is increased, the battery swells, the use safety of the battery is influenced, and the service life of the battery is also shortened. In view of the above, it is important to provide a high voltage lithium ion battery electrolyte.
Disclosure of the invention
In order to make up for the defects of the prior art, the invention provides the high-voltage lithium ion battery electrolyte with long cycle life and excellent charge and discharge performance and the preparation method thereof.
The invention is realized by the following technical scheme:
a high voltage lithium ion battery electrolyte is characterized in that: the electrolyte consists of an anhydrous organic solvent, lithium salt and a functional additive, wherein the functional additive is one or more of cyano ester additives or fluoro ester additives, the content of the functional additive accounts for 5-15% of the total mass of the electrolyte, and the anhydrous organic solvent is linear carbonate and cyclic carbonate.
The functional additive cyano sulfate compound can form films on the surfaces of a positive electrode and a negative electrode, can generate better complexing action with metal atoms on the positive electrode, prevents the metal atoms from dissolving out, and can form an SRI film with lower impedance on the negative electrode, thereby reducing the oxidative decomposition of carbonate solvents on the surface of a motor; the 3-fluoro-1, 3-propane sultone has good negative film forming performance, can effectively coat a negative material, and can greatly improve the room temperature cycle performance under high voltage.
The more preferable technical scheme of the invention is as follows:
the anhydrous organic solvent is two or more of ethylene carbonate, propylene carbonate, butylene carbonate, dipropyl carbonate, vinylene carbonate, methyl propyl carbonate, dimethyl carbonate, diethyl carbonate and methyl ethyl carbonate.
The lithium salt is one or more of lithium hexafluorophosphate, lithium hexafluoroarsenate, lithium perchlorate, lithium tetrafluoroborate, lithium dioxalate borate, lithium difluorooxalate borate, lithium methylsulfonate, lithium trifluoromethylsulfonate and lithium bistrifluoromethylsulfonyl imide; preferably, the lithium salt is one or more of lithium hexafluorophosphate, lithium dioxalate borate and lithium bistrifluoromethylsulfonyl imide.
Wherein the concentration of lithium hexafluorophosphate is 1-1.5mol/L, and the concentrations of lithium dioxalate borate and lithium bistrifluoromethylsulfonyl imide are both 0.1-0.5 mol/L.
The functional additive is one or more of adiponitrile, glutaronitrile, 1, 2-difluoroethylene carbonate, 1-propenyl-1, 3-sultone, methylene methanedisulfonate, fluoroethylene carbonate, tris (trimethylsilane) phosphate, tris (trimethylsilane) borate, 3-fluoro-1, 3-propane sultone, cyano sulfate, sulfolane and phosphazene additives; preferably, the functional additive is one or more of cyano sulfate, fluoroethylene carbonate and 3-fluoro-1, 3-propane sultone.
According to the inventive concept, the preparation method of the high-voltage lithium ion battery electrolyte comprises the following steps:
(1) adding linear carbonate into a container, then adding cyclic carbonate melted into liquid, and uniformly mixing;
(2) cooling the mixed solution obtained in the step (1), slowly adding lithium salt, and continuously stirring until the solution is clear;
(3) adding the functional additive which is melted into liquid into the solution, continuously stirring until the solution is uniform and clear, and transferring the obtained product into a packaging bottle filled with inert gas for storage for later use.
Preferably, in the step (2), the temperature of the mixed solution is reduced to 5 ℃, and the lithium salt is added under the condition of lower than 5 ℃.
The invention effectively improves the oxidation resistance of the SEI film of the electrolyte during the initial formation by combining various functional additives, further obviously improves the cycle first reflection of the lithium ion battery under high voltage, simultaneously has excellent charge and discharge performance, and is suitable for wide popularization and application.
(IV) detailed description of the preferred embodiments
The following embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention are within the protection scope of the present invention.
Comparative example 1:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, when the temperature is reduced to 5 ℃, slowly adding lithium salt under the condition that the temperature is not higher than 10 ℃, preparing lithium hexafluorophosphate with the concentration of 1.2mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate according to the total mass of the electrolyte, fully stirring, and transferring to a packaging bottle filled with inert gas for storage for later use.
Comparative example 2:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, when the temperature is reduced to 5 ℃, slowly adding lithium salt under the condition that the temperature is not higher than 10 ℃, preparing electrolyte with the concentration of lithium hexafluorophosphate of 1.2mol/L and the concentration of lithium dioxalate borate of 0.2mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate according to the total mass of the electrolyte, fully stirring, and transferring into a packaging bottle filled with inert gas for storage.
Comparative example 3:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, when the temperature is reduced to 5 ℃, slowly adding lithium salt under the condition that the temperature is not higher than 10 ℃, preparing electrolyte with the concentration of lithium hexafluorophosphate of 1.2mol/L and the concentration of lithium bistrifluoromethylsulfonyl imide of 0.2mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate according to the total mass of the electrolyte, fully stirring, and transferring into a packaging bottle filled with inert gas for storage.
Example 1:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, slowly adding lithium salt when the temperature is reduced to 5 ℃, ensuring that the temperature is not higher than 10 ℃, preparing electrolyte with the lithium hexafluorophosphate concentration of 1.2mol/L, the lithium dioxalate borate of 0.1mol/L and the lithium bistrifluoromethylsulfonyl imide of 0.1mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate according to the total mass of the electrolyte, fully stirring, and transferring into a packaging bottle filled with inert gas for storage.
Example 2:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, when the temperature is reduced to 5 ℃, slowly adding lithium salt under the condition of ensuring that the temperature is not higher than 10 ℃, preparing electrolyte with the lithium hexafluorophosphate concentration of 1.2mol/L, the lithium dioxalate borate of 0.1mol/L and the lithium bistrifluoromethylsulfonyl imide of 0.1mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate and 2% cyano-sulfate according to the total mass of the electrolyte, fully stirring, and transferring into a packaging bottle filled with inert gas for storage.
Example 3:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, slowly adding lithium salt when the temperature is reduced to 5 ℃, ensuring that the temperature is not higher than 10 ℃, preparing electrolyte with the lithium hexafluorophosphate concentration of 1.2mol/L, the lithium dioxalate borate of 0.1mol/L and the lithium bistrifluoromethylsulfonyl imide of 0.1mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate and 2% 3-fluoro-1, 3-propane sultone according to the total mass of the electrolyte, fully stirring, and transferring into an inert gas filled packaging bottle for storage.
Example 4:
sequentially adding dimethyl carbonate (DMC), Ethylene Carbonate (EC) and Ethyl Methyl Carbonate (EMC) in a glove box (moisture is less than 10ppm and oxygen content is less than 1ppm) filled with nitrogen according to the mass ratio of 1:1:1, slowly adding lithium salt when the temperature is reduced to 5 ℃, ensuring that the temperature is not higher than 10 ℃, preparing electrolyte with the concentration of lithium hexafluorophosphate of 1.2mol/L, lithium dioxalate borate of 0.1mol/L and lithium bistrifluoromethylsulfonyl imide of 0.1mol/L, continuously stirring until the solution is clear, then adding 5% fluoroethylene carbonate, 2% 3-fluoro-1, 3-propane sultone and 2% cyano sulfate according to the total mass of the electrolyte, fully stirring, and transferring into an inert gas filled packaging bottle for storage for later use.
The electrolytes of the above three comparative examples and four examples were subjected to conductivity measurement at room temperature of 25 c, and the measurement results are shown in table 1. It can be seen from the following table that the electrolyte for a high voltage lithium battery of the present invention has good conductivity.
And respectively injecting the electrolytes of the three comparative examples and the four examples into a battery cell with a positive electrode material of lithium cobaltate, and carrying out chemical conversion and volume grading to obtain a 2Ah soft package battery cell. The cycling was performed at 1.0/1.0C charging and discharging current, the test voltage range was 3.0-4.45V, and the cycling performance of the battery after 500 weeks at room temperature (25 ℃) was recorded as shown in Table 2.
It can be seen from tables 1 and 2 that the addition of the novel lithium salt can significantly improve the conductivity and cycle performance of the electrolyte, and the comparison shows that the high-voltage lithium ion battery electrolyte prepared by the invention can significantly improve the cycle life of the lithium battery. The cyano sulfate compound can form films on the surfaces of a positive electrode and a negative electrode, can generate better complexing action with metal atoms on the positive electrode, prevents the metal atoms from dissolving out, and can form an SEI (solid electrolyte interphase) film with lower impedance on the negative electrode so as to reduce the oxidative decomposition of a carbonate solvent on the surface of the electrode; the 3-fluoro-1, 3-propane sultone has good negative film forming performance, can effectively coat a negative material, and can greatly improve the room temperature cycle performance under high voltage.
The present invention has been described above by way of example, but the present invention is not limited to the above-described specific embodiments, and any modification or variation made based on the present invention is within the scope of the present invention as claimed.
Claims (9)
1. A high voltage lithium ion battery electrolyte is characterized in that: the electrolyte consists of an anhydrous organic solvent, lithium salt and a functional additive, wherein the functional additive is one or more of cyano ester additives or fluoro ester additives, the content of the functional additive accounts for 5-15% of the total mass of the electrolyte, and the anhydrous organic solvent is linear carbonate and cyclic carbonate.
2. The high voltage lithium ion battery electrolyte of claim 1, wherein: the anhydrous organic solvent is two or more of ethylene carbonate, propylene carbonate, butylene carbonate, dipropyl carbonate, vinylene carbonate, methyl propyl carbonate, dimethyl carbonate, diethyl carbonate and methyl ethyl carbonate.
3. The high voltage lithium ion battery electrolyte of claim 1, wherein: the lithium salt is one or more of lithium hexafluorophosphate, lithium hexafluoroarsenate, lithium perchlorate, lithium tetrafluoroborate, lithium dioxalate borate, lithium difluorooxalate borate, lithium methylsulfonate, lithium trifluoromethylsulfonate and lithium bis (trifluoromethylsulfonyl) imide.
4. The high voltage lithium ion battery electrolyte of claim 1, wherein: the functional additive is one or more of adiponitrile, glutaronitrile, 1, 2-difluoroethylene carbonate, 1-propenyl-1, 3-sultone, methylene methanedisulfonate, fluoroethylene carbonate, tris (trimethylsilane) phosphate, tris (trimethylsilane) borate, 3-fluoro-1, 3-propane sultone, cyano sulfate, sulfolane and phosphazene additives.
5. The high voltage lithium ion battery electrolyte of claim 1 or 3, wherein: the lithium salt is one or more of lithium hexafluorophosphate, lithium dioxalate borate and lithium bistrifluoromethylsulfonyl imide.
6. The high voltage lithium ion battery electrolyte of claim 1 or 4, wherein: the functional additive is one or more of cyano sulfate, fluoroethylene carbonate and 3-fluoro-1, 3-propane sultone.
7. The high voltage lithium ion battery electrolyte of claim 5, wherein: the concentration of the lithium hexafluorophosphate is 1-1.5mol/L, and the concentrations of the lithium dioxalate borate and the lithium bistrifluoromethylsulfonyl imide are both 0.1-0.5 mol/L.
8. The method of claim 1, comprising the steps of: (1) adding linear carbonate into a container, then adding cyclic carbonate melted into liquid, and uniformly mixing; (2) cooling the mixed solution obtained in the step (1), slowly adding lithium salt, and continuously stirring until the solution is clear; (3) adding the functional additive which is melted into liquid into the solution, continuously stirring until the solution is uniform and clear, and transferring the obtained product into a packaging bottle filled with inert gas for storage for later use.
9. The method of claim 8, wherein the method comprises: in the step (2), the mixed solution is cooled to 5 ℃, and lithium salt is added under the condition that the temperature is lower than 5 ℃.
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| CN202010242947.9A CN111276747A (en) | 2020-03-31 | 2020-03-31 | High-voltage lithium ion battery electrolyte and preparation method thereof |
| PCT/CN2020/098713 WO2021196429A1 (en) | 2020-03-31 | 2020-06-29 | High-voltage lithium ion battery electrolyte and preparation method therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112838269A (en) * | 2021-01-11 | 2021-05-25 | 宁德新能源科技有限公司 | Electrolyte solution, electrochemical device and electronic apparatus including the same |
| WO2021196429A1 (en) * | 2020-03-31 | 2021-10-07 | 山东海容电源材料股份有限公司 | High-voltage lithium ion battery electrolyte and preparation method therefor |
| CN114865078A (en) * | 2022-06-24 | 2022-08-05 | 山东航盛新能源材料有限公司 | Electrolyte for lithium battery and preparation method thereof |
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| CN114221030B (en) * | 2021-11-05 | 2024-01-05 | 东方电气集团科学技术研究院有限公司 | Lithium ion battery electrolyte |
| CN114243108A (en) * | 2021-11-29 | 2022-03-25 | 惠州市豪鹏科技有限公司 | Electrolyte and battery thereof |
| CN114300750A (en) * | 2021-12-27 | 2022-04-08 | 清华大学 | Lithium ion battery electrolyte and lithium ion battery |
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| CN115189026A (en) * | 2022-07-26 | 2022-10-14 | 清华大学深圳国际研究生院 | High-voltage electrolyte and preparation method and application thereof |
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Application publication date: 20200612 |