CN108258308B - Lithium ion battery non-aqueous electrolyte and lithium ion battery - Google Patents
Lithium ion battery non-aqueous electrolyte and lithium ion battery Download PDFInfo
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- CN108258308B CN108258308B CN201611246392.5A CN201611246392A CN108258308B CN 108258308 B CN108258308 B CN 108258308B CN 201611246392 A CN201611246392 A CN 201611246392A CN 108258308 B CN108258308 B CN 108258308B
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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
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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
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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
- H01M10/05—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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a non-aqueous electrolyte of a lithium ion battery, aiming at solving the problem that the existing electrolyte of the lithium ion battery cannot give consideration to good high and low temperature performance and cycle performance. The lithium ion battery non-aqueous electrolyte comprises a compound A shown in a structural formula 1 and lithium difluorophosphate,wherein, in the formula 1, R1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a halogen atom or a C1-C5 group. The lithium ion battery non-aqueous electrolyte provided by the invention can endow the lithium ion battery using the non-aqueous electrolyte with excellent comprehensive performance, particularly including excellent cycle performance, high-temperature storage performance and low-temperature performance, by using the compound A and the lithium difluorophosphate in a combined manner.
Description
Technical Field
The invention belongs to the technical field of battery electrolyte, and particularly relates to a lithium ion battery non-aqueous electrolyte and a lithium ion battery.
Background
A lithium ion battery is a type of secondary battery that operates by movement of lithium ions between a positive electrode and a negative electrode. The lithium ion battery has the obvious advantages of high working voltage, high energy density, low self-discharge rate, no memory effect and the like, and is widely applied to energy storage power systems of hydraulic power, firepower, wind power, solar power stations and the like, and a plurality of fields of electric tools, electric bicycles, electric motorcycles, electric automobiles, military equipment, aerospace and the like. With the development of new energy automobiles and power energy storage, people have higher requirements on the performance of lithium ion power batteries, and the lithium ion batteries which can meet the requirements better need to be developed. The current lithium ion power battery has the defects of short high-temperature cycle life, and cannot give consideration to high-temperature and low-temperature performances and the like.
The non-aqueous electrolyte is a key factor influencing the cycle and high and low temperature performance of the battery, and particularly, an additive in the electrolyte plays a decisive role in the performance of the electrolyte.
The research finds that the lithium difluorophosphate can obviously improve the high-temperature storage and low-temperature discharge performance of the battery, but the researchers in the field find that the lithium difluorophosphate can improve the high-temperature storage and low-temperature discharge performance, but the improvement effect on the cycle performance is not obvious, and the cycle performance cannot meet the actual use requirement.
Disclosure of Invention
The invention aims to provide a lithium ion battery non-aqueous electrolyte simultaneously having good high and low temperature performance and cycle performance (namely good high temperature and cycle characteristics and low impedance), and aims to solve the problem that the existing lithium ion battery electrolyte cannot simultaneously have good high and low temperature performance and cycle performance, and particularly the cycle performance of the lithium difluorophosphate-containing non-aqueous electrolyte cannot meet the actual requirement.
The invention is realized in such a way that the lithium ion battery non-aqueous electrolyte comprises a compound A shown in the following structural formula 1 and lithium difluorophosphate,
wherein, in the formula 1, R1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a halogen atom or a C1-C5 group.
Preferably, the C1-C5 group includes C1-C5 hydrocarbon group, halogenated hydrocarbon group, oxygen-containing hydrocarbon group, silicon-containing hydrocarbon group and cyano-substituted hydrocarbon group.
Preferably, said R is1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a fluorine atom, a methyl group, an ethyl group, a methoxy group, an ethoxy group or a trifluoromethyl group.
Preferably, the compound A comprises the compounds shown in the following structural formulas 11-17,
preferably, the mass percentage of the compound A is 0.1-5% based on 100% of the total mass of the lithium ion battery nonaqueous electrolyte.
Preferably, the lithium difluorophosphate accounts for 0.1-2% of the total mass of the lithium ion battery nonaqueous electrolyte.
Preferably, the lithium ion battery nonaqueous electrolyte further comprises lithium bis (fluorosulfonyl) imide.
Preferably, the mass percentage of the lithium bis (fluorosulfonyl) imide is 0.1-10% based on 100% of the total mass of the lithium ion battery nonaqueous electrolyte.
And the lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm arranged between the positive electrode and the negative electrode, and electrolyte, wherein the electrolyte is the lithium ion battery non-aqueous electrolyte.
The lithium ion battery non-aqueous electrolyte provided by the invention contains the compound A and lithium difluorophosphate. The compound A forms an SEI with a compact structure after decomposition, so that the cycle and high-temperature storage performance of the battery are improved, the impedance is low, and the low-temperature performance of the battery cannot be degraded. After the lithium difluorophosphate and the compound A are mixed for use, the lithium difluorophosphate can participate in negative electrode film formation, so that the impedance of a passivation film formed by the compound A is further reduced, and the low-temperature performance of the lithium ion battery is improved. The lithium ion battery non-aqueous electrolyte, the lithium difluorophosphate and the compound A are used in combination, so that the lithium ion battery using the non-aqueous electrolyte can be endowed with excellent comprehensive performance, particularly including excellent cycle performance, high-temperature storage performance and low-temperature performance (low impedance).
The lithium ion battery provided by the invention contains the non-aqueous electrolyte, so that the lithium ion battery has good high and low temperature and cycle performance, and can meet the requirement of the lithium ion battery on the overall performance.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a lithium ion battery non-aqueous electrolyte, which comprises a compound A shown in the following structural formula 1 and lithium difluorophosphate,
wherein, in the formula 1, R1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a halogen atom or a C1-C5 group.
Among them, preferably, the C1-C5 group includes C1-C5 hydrocarbon group, halogenated hydrocarbon group, oxygen-containing hydrocarbon group, silicon-containing hydrocarbon group, cyano-substituted hydrocarbon group. Further preferably, R is1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a fluorine atom, a methyl group, an ethyl group, a methoxy group, an ethoxy group or a trifluoromethyl group. The preferable substituent group is more beneficial to the film formation of the compound A on the negative electrode, thereby effectively protecting the negative electrode and improving the cycle and high-temperature storage performance of the battery.
Particularly preferably, the compound A comprises the compounds shown in the following structural formulas 11-17,
the compound A with the structural characteristics forms an SEI with a denser structure after being decomposed, so that the cycle and high-temperature storage performance of the battery are improved, the impedance is low, and the low-temperature performance of the battery is not degraded. On the other hand, due to the existence of lithium difluorophosphate in the electrolyte, in the film forming process of the compound A, the lithium difluorophosphate and the compound A form a film together to generate a synergistic effect, so that a passivation film with lower impedance is formed, and the low-temperature performance of the lithium ion battery is further improved. Of course, it is to be understood that the specific type of the compound a is not limited thereto.
More preferably, the mass percentage of the compound A is 0.1-5% based on 100% of the total mass of the lithium ion battery nonaqueous electrolyte. When the mass percentage of the compound A is less than 0.1%, the film forming effect of the compound A on the negative electrode is reduced, and the improvement effect on the cycle performance is reduced; when the mass percentage of the compound A is more than 5%, the formed film on the negative electrode interface of the lithium ion battery is thick, the battery impedance is seriously increased, and the low-temperature performance of the battery is deteriorated.
In the embodiment of the invention, although the compound A can improve the cycle and high-temperature storage performance of the battery, the compound A can also ensure that the impedance of the battery is not influenced to a certain extent. However, the addition of the compound a still causes the battery to have insufficient low-temperature performance, and the low-temperature performance of the lithium ion battery needs to be improved. The lithium difluorophosphate cannot form a good SEI film, so that the circulation improvement effect is poor, and the application of the electrolyte under the high-temperature condition is inhibited. But after being compounded with the compound A, the compound A can participate in film formation at the negative electrode, thereby effectively complementing the compound A and simultaneously improving the high-low temperature and cycle performance of the lithium ion battery.
Preferably, the lithium difluorophosphate accounts for 0.1-2% of the total mass of the lithium ion battery nonaqueous electrolyte. When the content of the lithium difluorophosphate is less than 0.1%, the resistance reducing effect is reduced, and the low-temperature performance improving effect on the lithium ion battery is reduced; when the content of the lithium difluorophosphate is more than 2%, the solubility of the lithium difluorophosphate is poor, the lithium difluorophosphate cannot be uniformly dissolved in the electrolyte, the viscosity and the conductivity of the electrolyte are increased, and the performance of the lithium ion battery is reduced.
In the electrolyte system provided by the invention, the lithium bis (fluorosulfonyl) imide can further improve the high-temperature storage and low-temperature performance of the battery. Preferably, the mass percentage of the lithium bis (fluorosulfonyl) imide is 0.1-10%, and more preferably 0.1-5%, based on 100% of the total mass of the lithium ion battery nonaqueous electrolyte. When the content of the lithium bis (fluorosulfonyl) imide is less than 0.1%, the improvement effect is reduced, and when the content is more than 10%, the lithium bis (fluorosulfonyl) imide corrodes a current collector of a battery, which is not favorable for the performance of the battery.
The lithium ion battery non-aqueous electrolyte provided by the embodiment of the invention simultaneously contains the compound A and lithium difluorophosphate. After the lithium difluorophosphate is combined with the compound A, the low-temperature performance is improved, and the high-temperature performance and the high-temperature storage performance of the lithium ion battery are further improved. The lithium ion battery non-aqueous electrolyte, lithium difluorophosphate and the compound A are used in combination, so that the lithium ion battery using the non-aqueous electrolyte can be endowed with excellent comprehensive performance, specifically including excellent cycle performance, high-temperature storage performance and low-temperature performance (low impedance).
The embodiment of the invention also provides a lithium ion battery, which comprises a positive electrode, a negative electrode, a diaphragm arranged between the positive electrode and the negative electrode, and electrolyte, wherein the electrolyte is the lithium ion battery non-aqueous electrolyte.
In the embodiment of the present invention, the positive electrode, the negative electrode, and the separator are not specifically limited, and any one of the positive electrode, the negative electrode, and the separator that are conventional in the art may be used.
The lithium ion battery provided by the embodiment of the invention contains the nonaqueous electrolyte, so that the lithium ion battery has good high and low temperature and cycle performance, and can meet the requirement of the lithium ion battery on the overall performance.
The following description will be given with reference to specific examples.
Example 1
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprises a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte and comprises an additive, and the additive comprises the additive in the mass percentage shown in the example 1 in the table 1 based on the total weight of the nonaqueous electrolyte being 100%.
Example 2
LiNi0.5Co0.2Mn0.3ArtificialA graphite battery comprises a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte and comprises an additive, and the additive comprises the additive shown in the mass percentage in the example 2 in Table 1 based on the total weight of the nonaqueous electrolyte being 100%.
Example 3
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprises a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte and comprises an additive, and the additive comprises the additive in the mass percentage shown in the embodiment 3 in Table 1 based on the total weight of the nonaqueous electrolyte being 100%.
Example 4
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprises a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte and comprises an additive, and the additive comprises the additive shown in the embodiment 4 in Table 1 in percentage by mass based on the total weight of the nonaqueous electrolyte being 100%.
Example 5
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprises a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte and comprises an additive, and the additive comprises the additive shown in the embodiment 5 in Table 1 in percentage by mass based on the total weight of the nonaqueous electrolyte being 100%.
Example 6
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprises a positive electrode, a negative electrode, a separator arranged between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte and comprises an additive, and the additive comprises the additive shown in the mass percentage in the example 6 in Table 1 based on the total weight of the nonaqueous electrolyte being 100%.
Example 7
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprising a positive electrode, a negative electrode, a separator provided between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte containing an additive in a mass percentage shown in example 7 of Table 1, based on 100% by weight of the total weight of the nonaqueous electrolyte.
Example 8
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprising a positive electrode, a negative electrode, a separator provided between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte containing an additive in a mass percentage shown in example 8 of Table 1, based on 100% by weight of the total weight of the nonaqueous electrolyte.
Example 9
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprising a positive electrode, a negative electrode, a separator provided between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte containing an additive in a mass percentage shown in example 9 of Table 1, based on 100% by weight of the total weight of the nonaqueous electrolyte.
Comparative example 1
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprising a positive electrode, a negative electrode, a separator provided between the positive electrode and the negative electrode, and an electrolyte, wherein the electrolyte is a nonaqueous electrolyte containing an additive in a mass percentage shown in comparative example 1 of Table 1, based on 100% by weight of the total weight of the nonaqueous electrolyte.
Comparative example 2
LiNi0.5Co0.2Mn0.3An artificial graphite battery comprising a positive electrode, a negative electrode, a separator provided between the positive electrode and the negative electrode, and an electrolyte solution, wherein the electrolyte solution is a nonaqueous electrolyte solution containing an additive in an amount of 100% by weight based on the total weight of the nonaqueous electrolyte solution, and contains the following components in the following Table 1And (4) additives in percentage by mass as shown in comparative example 2.
LiNi of examples 1 to 9 of the present invention and comparative examples 1 to 2 were mixed0.5Co0.2Mn0.3The artificial graphite battery is subjected to performance test, and the test indexes and the test method are as follows:
(1) the high-temperature cycle performance is shown by testing the capacity retention rate of 500 cycles at 45 ℃ and 1C, and the specific method comprises the following steps: at 45 ℃, the formed battery is charged to 4.2V by a 1C constant current and constant voltage, the current is cut off to be 0.01C, and then the battery is discharged to 3.0V by a 1C constant current. After 500 cycles of such charge/discharge, the capacity retention rate after 500 cycles was calculated to evaluate the high temperature cycle performance.
The calculation formula of the capacity retention rate after 500 cycles of 1C at 45 ℃ is as follows:
the 500 th cycle capacity retention ratio (%) (500 th cycle discharge capacity/first cycle discharge capacity) × 100%.
(2) The low-temperature discharge performance is embodied by the discharge efficiency of 0.5C at the temperature of minus 20 ℃, and the specific method comprises the following steps: at 25 ℃, the formed battery is charged to 4.2V by using a 1C constant current and constant voltage, the cut-off current is 0.01C, then the battery is discharged to 3.0V by using a 1C constant current, and the discharge capacity is recorded. Then charging the battery to 4.2V at constant current and constant voltage of 1C until the current is 0.01C, placing the battery in an environment at the temperature of minus 20 ℃ for 12 hours, discharging the battery to 2.5V at constant current of 0.5C, and recording the discharge capacity.
-20 ℃ 0.5C discharge efficiency calculation formula as follows:
low-temperature discharge efficiency (%) at-20 ℃ of 0.5C discharge capacity (-20 ℃) per 1C discharge capacity (25 ℃).
(3) Method for testing capacity retention rate, capacity recovery rate and thickness expansion rate after 30 days of storage at 60 ℃: the formed battery is charged to 4.2V at constant current and constant voltage of 1C at normal temperature, the cut-off current is 0.01C, then the 1C constant current is used for discharging to 3.0V, the initial discharge capacity of the battery is measured, then the 1C constant current and constant voltage are used for charging to 4.2V, the cut-off current is 0.01C, the initial thickness of the battery is measured, then the battery is stored for 30 days at 60 ℃, the thickness of the battery is measured, then the 1C constant current is used for discharging to 3.0V, the retention capacity of the battery is measured, then the 1C constant current and constant voltage are used for charging to 4.2V, the cut-off current is 0.01C, then the 1C constant current is used for discharging to 3.0V, and the recovery. The calculation formulas of the capacity retention rate and the capacity recovery rate are as follows:
battery capacity retention (%) — retention capacity/initial capacity × 100%;
battery capacity recovery (%) — recovery capacity/initial capacity × 100%;
the battery thickness swelling ratio (%) (thickness after 30 days-initial thickness)/initial thickness × 100%.
The test results are shown in table 1 below.
TABLE 1
With reference to table 1, lithium difluorophosphate was added to each of the nonaqueous electrolytes of comparative examples 1 to 9, comparative example 1, examples 1 to 9 and comparative example 1, but compound a was added to the nonaqueous electrolytes of examples 1 to 9 and compound a was not added to the nonaqueous electrolyte of comparative example 1. The results show that examples 1-9, which contain both compound a and lithium difluorophosphate, have good cycle performance, high temperature storage performance and low temperature performance; while comparative example 1, which does not contain compound a, has better low temperature performance, but significantly poorer cycle performance and high temperature storage performance. Therefore, the addition of the compound A can obviously improve the cycle performance and the high-temperature storage property.
The nonaqueous electrolytic solutions of comparative examples 1 to 9, comparative example 2, examples 1 to 9 and comparative example 2 were all added with the compound a, but the nonaqueous electrolytic solutions of examples 1 to 9 were simultaneously added with lithium difluorophosphate, and the nonaqueous electrolytic solution of comparative example 2 was added with VC but without the compound a. The results show that examples 1-9, which contain both compound a and lithium difluorophosphate, have good cycle performance, high temperature storage performance and low temperature performance; while comparative example 2, which contained lithium difluorophosphate and VC, generally had lower cycle performance, low temperature performance and high temperature storage performance overall than examples 1 to 9. It can be seen that the combined use of the compound a and the lithium difluorophosphate can improve the cycle performance, high-temperature storage performance and low-temperature performance of the lithium ion battery.
In summary, the lithium ion batteries prepared by the nonaqueous electrolytic solution added with the compound a and the lithium difluorophosphate provided in embodiments 1 to 9 of the present invention all have good cycle performance, high temperature storage performance and low temperature performance.
In each of comparative examples 1 and 9, compound a and lithium difluorophosphate having the same structure were added to the nonaqueous electrolytic solution. Wherein the compound A is a compound shown in a structural formula 11, and the content of lithium difluorophosphate and the content of the compound A in each embodiment are both 1%. In example 9, 1% of lithium bis (fluorosulfonyl) imide was added. The results show that the cycle performance, the high-temperature storage performance and the low-temperature performance of example 9 added with lithium bis (fluorosulfonyl) imide are improved on the basis of example 1. Therefore, the lithium bis (fluorosulfonyl) imide can perform a synergistic effect with the compound A and lithium difluorophosphate, and further improve the overall performance (cycle performance, high-temperature storage performance and low-temperature performance) of the lithium ion battery.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A lithium ion battery non-aqueous electrolyte is characterized by comprising a compound A shown in a structural formula 1 and lithium difluorophosphate,
wherein, in the formula 1, R1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a fluorine atom or a C1-C5 group, and the C1-C5 group comprises trifluoromethyl, a C1-C5 hydrocarbyl group, an oxygen-containing hydrocarbyl group, a silicon-containing hydrocarbyl group and a cyano-substituted hydrocarbyl group.
2. The nonaqueous electrolyte solution for lithium ion batteries according to claim 1, wherein R is represented by formula1、R2、R3、R4、R5、R6Each independently is one of a hydrogen atom, a fluorine atom, a methyl group, an ethyl group, a methoxy group, an ethoxy group or a trifluoromethyl group.
4. the nonaqueous electrolyte solution for lithium ion batteries according to any one of claims 1 to 3, wherein the mass percentage of the compound A is 0.1 to 5% based on 100% by mass of the total mass of the nonaqueous electrolyte solution for lithium ion batteries.
5. The nonaqueous electrolyte solution for lithium ion batteries according to any one of claims 1 to 3, wherein the mass percentage of lithium difluorophosphate is 0.1 to 2% based on 100% by mass of the total mass of the nonaqueous electrolyte solution for lithium ion batteries.
6. The nonaqueous electrolyte solution for lithium ion batteries according to any one of claims 1 to 3, further comprising lithium bis (fluorosulfonyl) imide.
7. The nonaqueous electrolyte solution for lithium ion batteries according to claim 6, wherein the mass percentage of lithium bis (fluorosulfonyl) imide is 0.1 to 10% based on 100% by mass of the total mass of the nonaqueous electrolyte solution for lithium ion batteries.
8. A lithium ion battery comprising a positive electrode, a negative electrode, a separator provided between the positive electrode and the negative electrode, and an electrolytic solution, wherein the electrolytic solution is the lithium ion battery nonaqueous electrolytic solution according to any one of claims 1 to 7.
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