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CN113078355A - Ternary lithium ion battery electrolyte and ion battery thereof - Google Patents

Ternary lithium ion battery electrolyte and ion battery thereof Download PDF

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Publication number
CN113078355A
CN113078355A CN202110168815.0A CN202110168815A CN113078355A CN 113078355 A CN113078355 A CN 113078355A CN 202110168815 A CN202110168815 A CN 202110168815A CN 113078355 A CN113078355 A CN 113078355A
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ion battery
lithium ion
carbonate
battery electrolyte
lithium
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邱阳
朱学全
刘杨
王建斌
潘立宁
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Dongguan Shanshan Battery Materials Co Ltd
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Dongguan Shanshan Battery Materials Co Ltd
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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
    • 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
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Materials Engineering (AREA)
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Abstract

The invention discloses a ternary lithium ion battery electrolyte and an ion battery thereof, wherein the electrolyte comprises a non-aqueous organic solvent, lithium salt and a film forming additive, and the film forming additive with a specific structure can form a uniform and compact protective film on the surface of a ternary material, so that the reaction of the electrolyte and an electrode active material is reduced, and the electrochemical performance of the lithium ion battery is further improved.

Description

Ternary lithium ion battery electrolyte and ion battery thereof
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a ternary lithium ion battery electrolyte and an ion battery thereof.
Background
In recent years, as the demand for lithium ion batteries for large and medium-sized systems such as electric vehicles and energy storage systems has increased, further improvement in energy density of lithium ion batteries has been required. The common measure is to increase the charge cut-off voltage of the battery, but when the battery is under high voltage, the positive electrode material has certain defects, such as structure collapse, ion mixing and discharging, metal ion dissolution and the like; secondly, the cathode material with high energy density, such as NCM622 and NCM811, is adopted and simultaneously matched with the high energy densityAnd a negative electrode material such as a silicon-based negative electrode. However, the higher nickel content leads to a decrease in the cobalt and manganese content, resulting in structural instability of the NCM and severe capacity fade problems. The capacity attenuation of the nickel-rich NCM is caused by various factors such as irreversible phase change, side reaction of an electrode/electrolyte interface and the like, and the high-nickel ternary material is converted from a layered structure to an unordered spinel structure and a rock salt structure in the circulation process, namely, cation mixed discharge is realized, so that Li is blocked+Leading to an increase in interfacial resistance and a decrease in reversible capacity (Nano Letters,2017,17(6): 3946).
The technical difficulties of the high-nickel ternary material are that the high-temperature cycle performance is poor and the high-temperature storage gas is generated, and the conventional film-forming additive cannot well inhibit the dissolution of metal ions, the structural damage and the oxidation catalysis of the anode after the separation of the metal ions from the ternary anode material. In view of the above problems, the solution idea is generally as follows: forming a protective CEI film on the surface of a positive electrode, blocking the corrosion of HF to a structure and simultaneously inhibiting the dissolution of metal ions; secondly, adding a functional additive with complex metal ions to prevent Mn, Ni and other ions from depositing on the negative electrode, so that the reduction decomposition of the electrolyte and the insertion and removal of ions from a channel are prevented; and thirdly, adding a negative electrode film forming additive to improve the components and properties of a negative electrode interfacial film, so that the negative electrode is not negatively affected by the deposition of Mn, Ni and the like.
For example, chinese patent CN110380113A discloses an additive for a high voltage lithium ion battery electrolyte and an application thereof, the lithium ion battery electrolyte of the present invention comprises a lithium salt, an organic solvent and an additive, wherein the additive is an ester compound containing a dicyan group and other additives, and can generate a protective film on the surface of a high voltage positive electrode material, thereby further improving the cycle life and high temperature storage performance of the lithium ion battery on the basis of improving the energy density of the lithium ion battery. The disadvantage is that the film forming resistance of the additive is larger.
For example, chinese patent CN108336404A discloses a non-aqueous electrolyte for lithium ion battery and a lithium ion battery. The non-aqueous electrolyte comprises a lithium salt, an organic solvent and an additive, wherein the additive is selected from phosphate compounds. The electrolyte can play a good flame-retardant role, the safety performance of the battery is improved, the cycle performance of the battery is greatly improved, but the film forming resistance of the additive is larger.
Disclosure of Invention
In order to overcome the defects of the background art, the invention provides the ternary lithium ion battery electrolyte and the ion battery thereof, and the ternary lithium ion battery electrolyte can effectively solve the high-temperature storage performance and the rate cycling performance of the lithium ion battery under the synergistic action of multiple uniquely combined components by optimizing the formula, so that an electrolyte system has high energy density and high safety performance, the requirements of the electrolyte on the high-temperature storage performance, the rate cycling performance and the safety performance under high voltage are favorably met, and the electrochemical performance of the high-voltage lithium ion battery is further improved.
In order to achieve the purpose, the invention adopts the technical scheme that: a ternary lithium ion battery electrolyte comprises a non-aqueous organic solvent, a lithium salt and a film forming additive, wherein the structural formula of the film forming additive is shown as the following formula:
Figure BDA0002938258690000021
wherein R is1,R2,R3Each independently selected from hydrogen atom, fluorine atom, C1-C4 alkyl, alkenyl, alkynyl, nitrile, fluoroalkyl and aryl.
Preferably, the film-forming additive is selected from at least one of the compounds represented by the following structural formula:
Figure BDA0002938258690000022
preferably, the content of the film forming additive is 0.3-2.0% of the total mass of the ternary lithium ion battery electrolyte.
Preferably, the ternary lithium ion battery electrolyte further comprises other additives selected from at least one of Vinylene Carbonate (VC), vinyl sulfate (DTD), 1, 3-propane sultone (1,3-PS), 1, 3-propene sultone (1,3-PST), tris (trimethylsilyl) borate (TMSB), tris (trimethylsilyl) phosphate (TMSP), tris (trimethylsilyl) phosphite (TMSPi), citraconic anhydride.
Preferably, the content of the other additives is 1.0-5% of the total mass of the ternary lithium ion battery electrolyte.
Preferably, the lithium salt is selected from lithium hexafluorophosphate (LiPF)6) Lithium tetrafluoroborate (LiBF)4) Lithium difluorophosphate (LiPO)2F2) Lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (oxalato) borate (LiBOB), lithium tris (oxalato) phosphate, lithium difluoro (oxalato) borate (lidob), lithium tetrafluoro (oxalato) phosphate, and lithium difluoro (oxalato) phosphate.
Preferably, the content of the lithium salt is 10-15% of the total mass of the ternary lithium ion battery electrolyte.
The non-aqueous organic solvent in the present invention may be one or more selected from the group consisting of a chain carbonate, a cyclic carbonate, a carboxylic ester, a fluorocarbonate and a fluorocarboxylic ester. The cyclic carbonate is selected from ethylene carbonate and propylene carbonate; the chain carbonate is selected from methyl ethyl carbonate, dimethyl carbonate and diethyl carbonate; the carboxylic ester is selected from ethyl acetate, ethyl propionate, ethyl butyrate, methyl propionate, propyl butyrate and propyl acetate; the fluoro carbonate and fluoro carboxylic ester is selected from fluoro ethylene carbonate, 1, 2-difluoro ethylene carbonate, methyl trifluoroethyl carbonate, bis trifluoroethyl carbonate, ethyl difluoroacetate. Preferably, the non-aqueous organic solvent is selected from the group consisting of Ethylene Carbonate (EC), diethyl carbonate (DEC), a mixture of Ethyl Methyl Carbonate (EMC).
The invention also provides a ternary lithium ion battery which comprises a positive pole piece, a negative pole piece, an isolating membrane arranged between the positive pole piece and the negative pole piece and the ternary lithium ion battery electrolyte.
Preferably, the active material of the positive electrode plate may be LiNi1-x-y-zCoxMnyAlzO2(wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, and z is more than or equal to 0 and less than or equal to 1X + y + z is more than or equal to 1 and more than or equal to 0), lithium nickel manganese oxide, lithium cobaltate, lithium-rich manganese-based solid solution and lithium manganese oxide; the active material of the negative pole piece can be artificial graphite, lithium metal, coated natural graphite, a silicon-carbon negative pole and a silicon negative pole.
Preferably, the upper cut-off voltage of the ternary lithium ion battery is greater than or equal to 4.2V.
Compared with the prior art, the invention has the advantages that:
1. the film forming additive with a specific structure in the electrolyte of the ternary lithium ion battery has excellent electrochemical stability, can form a uniform and compact protective film on the surface of a ternary material, reduces the reaction of the electrolyte and an electrode active material, effectively inhibits the dissolution of metal ions, reduces impedance, and is beneficial to improving the electrochemical performance of the lithium ion battery;
2. the electrolyte lithium salt in the electrolyte of the ternary lithium ion battery has good film forming property, and can reduce the impedance of the anode and cathode passive films, thereby greatly improving the electrochemical performance of the lithium ion battery;
3. according to the high-voltage lithium ion battery non-aqueous electrolyte disclosed by the invention, through optimizing the formula, under the synergistic effect of multiple uniquely combined components, an electrolyte system has high energy density and high safety performance, the requirements of the electrolyte on high-temperature performance, low-temperature performance and safety performance under high voltage are favorably met, and the electrochemical performance of the high-voltage lithium ion battery is further improved.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail with reference to the following examples, which are only for the purpose of explaining the present invention and are not intended to limit the present invention.
The film-forming additives in the examples and comparative examples were characterized as follows:
the structural formula of the compound (1) is:
Figure BDA0002938258690000041
the structural formula of the compound (2) is:
Figure BDA0002938258690000042
the structural formula of the compound (3) is:
Figure BDA0002938258690000043
the structural formula of the compound (4) is:
Figure BDA0002938258690000044
the structural formula of the compound (5) is:
Figure BDA0002938258690000045
the structural formula of the compound (6) is:
Figure BDA0002938258690000051
example 1
The lithium ion battery electrolyte is prepared by the following method: ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) were mixed uniformly in a mass ratio of 30:20:50 in an argon-filled glove box (moisture < 0.1ppm, oxygen < 0.1ppm) to obtain a mixed solution, and lithium hexafluorophosphate (LiPF) was added to the mixed solution in an amount of 12.5% based on the total mass of the electrolyte6) Stirring until the lithium hexafluorophosphate is completely dissolved to obtain an electrolyte containing lithium hexafluorophosphate; then, 1% of the compound (1) based on the total mass of the electrolyte was added thereto and uniformly stirred to obtain the electrolyte for a lithium ion battery of example 1.
Examples 2 to 15
Examples 2 to 15 are also specific examples of the electrolyte preparation, and the parameters and preparation method are the same as those of example 1 except for the parameters shown in Table 1. The electrolyte formulation is shown in table 1.
Comparative examples 1 to 3
In comparative examples 1 to 3, the parameters and preparation method were the same as in example 1 except for the parameters shown in Table 1. The electrolyte formulation is shown in table 1.
TABLE 1 composition ratios of respective components of the electrolytes of examples 1 to 15 and comparative examples 1 to 3
Figure BDA0002938258690000052
Figure BDA0002938258690000061
Figure BDA0002938258690000071
Note: the concentration of the lithium salt is the mass percentage content in the electrolyte;
the content of the film forming additive is the mass percentage content in the electrolyte;
the content of each component in other additives is the mass percentage content in the electrolyte;
the proportion of each component in the solvent is mass ratio.
Lithium ion battery performance testing
Preparing a lithium ion battery:
in an Ar glove box, the electrolytes prepared in examples and comparative examples were respectively injected into fully dried artificial graphite material/LiNi0.6Co0.2Mn0.2O2The lithium ion battery is obtained after the conventional procedures of packaging, laying aside, formation, aging, secondary packaging, capacity grading and the like.
The lithium ion batteries of the examples and the comparative examples are respectively subjected to performance tests, and the test results are shown in table 2, wherein:
1) normal temperature cycle performance
Charging the lithium ion battery to 4.2V at a constant current and a constant voltage of 1C at the normal temperature (25 +/-2 ℃); standing for 5min, then discharging at constant current to 3.0V, standing for 5min, and repeating the steps for charging and discharging. And calculating the capacity retention rate of the 1000 th cycle after 1000 cycles of charge and discharge. The calculation formula is as follows:
the 1000 th cycle capacity retention rate (%) - (1000 th cycle discharge capacity/first discharge capacity) × 100%
2) High temperature cycle performance
Under the condition of high temperature (45 ℃), respectively charging the lithium ion batteries to 4.2V full charge at a constant current and a constant voltage of 1C; standing for 5min, discharging to 3.0V under 1C constant current condition, standing for 5min, and repeating the steps for charging and discharging. And calculating the capacity retention rate of the 500 th cycle after 500 cycles of charge and discharge. The calculation formula is as follows:
the 500 th cycle capacity retention rate (%) - (500 th cycle discharge capacity/first discharge capacity) × 100%
3) High temperature storage Properties
The lithium ion battery was charged and discharged at room temperature (25. + -. 2 ℃ C.) by 1C/1C once (discharge capacity is denoted as D)C0) Recording the initial thickness as D1, and then respectively charging the lithium ion batteries to 4.2V under the condition of 1C constant current and constant voltage; storing the fully charged lithium ion battery in a 60 ℃ high-temperature box for 7 days, immediately measuring the thickness D2 after taking out, and performing 1C discharge (discharge capacity D) at normal temperatureC1) (ii) a Then, 1C/1C charging and discharging (discharge capacity is denoted by D) were performed at ordinary temperatureC2). The thickness change rate, the capacity retention rate and the capacity recovery rate of the lithium ion battery were calculated using the following formulas.
The thickness change rate (%) on day seven was (D2-D1)/D1 × 100%;
capacity retention (%) at day seven ═ DC1/DC0×100％；
Capacity recovery (%) at day seven ═ DC2/DC0×100％；
Table 2 lithium ion battery performance test results of each comparative example and example
Figure BDA0002938258690000081
Figure BDA0002938258690000091
As can be seen from the performance data for comparative example 1 and examples 1-8 in Table 2: the film forming additive with a specific structure has excellent electrochemical stability, can form a uniform and compact protective film on the surface of a ternary material, reduces the reaction of electrolyte and an electrode active material, effectively inhibits the dissolution of metal ions, reduces the impedance, and obviously improves the cycle performance and the high-temperature storage performance of a battery.
As can be seen from the performance data for the cells of examples 1, 7, 8 and comparative example 3 in table 2: when the content of the film forming additive with a specific structure is 0.3-1.5% of the total mass of the electrolyte, the lithium ion battery has the best electrochemical performance. When the amount of the additive is less, the formed anode film is not compact, and the room temperature and high temperature cycle performance of the lithium ion battery is influenced; however, when the amount of the additive is large, the thickness of the lithium ion battery is greatly changed after 7 days of storage, and the capacity retention rate of the storage is also influenced.
As can be seen from the performance data of the lithium ion batteries in the embodiments 1 to 8 and the embodiments 9 to 15 in the table 2, the film-forming additive with a specific structure and other additives can play a synergistic effect when used in combination, so that the film-forming additive has a better effect, and further improves the cycle performance and the high-temperature storage performance of the lithium ion battery.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The ternary lithium ion battery electrolyte comprises a non-aqueous organic solvent, lithium salt and a film forming additive, and is characterized in that the structural formula of the film forming additive is shown as the following formula:
Figure FDA0002938258680000011
wherein R is1,R2,R3Each independently selected from hydrogen atom, fluorine atom, C1-C4 alkyl, alkenyl, alkynyl, nitrile, fluoroalkyl and aryl.
2. The ternary lithium ion battery electrolyte of claim 1, wherein the film forming additive is selected from at least one compound represented by the following structural formula:
Figure FDA0002938258680000012
3. the ternary lithium ion battery electrolyte of claim 1, wherein the content of the film forming additive is 0.3-2.0% of the total mass of the ternary lithium ion battery electrolyte.
4. The ternary lithium ion battery electrolyte of claim 1, further comprising other additives selected from at least one of vinylene carbonate, vinyl sulfate, 1,3 propane sultone, 1, 3-propene sultone, tris (trimethylsilyl) borate, tris (trimethylsilyl) phosphate, tris (trimethylsilyl) phosphite, and citraconic anhydride.
5. The ternary lithium ion battery electrolyte of claim 4, wherein the content of the other additives is 1.0-5% of the total mass of the ternary lithium ion battery electrolyte.
6. The ternary lithium ion battery electrolyte of claim 1, wherein the lithium salt is selected from at least one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium difluorophosphate, lithium difluorosulfonimide, lithium bis (oxalato) borate, lithium tris (oxalato) phosphate, lithium difluorooxalato borate, lithium tetrafluorooxalato phosphate, lithium difluorobis (oxalato) phosphate.
7. The ternary lithium ion battery electrolyte of claim 1, wherein the content of the lithium salt is 10-15% of the total mass of the ternary lithium ion battery electrolyte.
8. The ternary lithium ion battery electrolyte of claim 1, wherein the non-aqueous organic solvent is selected from at least one of ethylene carbonate, propylene carbonate, ethyl methyl carbonate, dimethyl carbonate, diethyl carbonate, ethyl acetate, ethyl propionate, ethyl butyrate, methyl propionate, propyl butyrate, propyl acetate, fluoroethylene carbonate, 1, 2-difluoroethylene carbonate, methyl trifluoroethyl carbonate, bistrifluoroethyl carbonate, and ethyl difluoroacetate.
9. The ternary lithium ion battery electrolyte of claim 8, wherein the non-aqueous organic solvent is selected from a mixture of ethylene carbonate, diethyl carbonate, ethyl methyl carbonate.
10. A ternary lithium ion battery is characterized by comprising a positive pole piece, a negative pole piece, a separation film arranged between the positive pole piece and the negative pole piece and the ternary lithium ion battery electrolyte of any one of claims 1 to 9.
CN202110168815.0A 2021-02-07 2021-02-07 Ternary lithium ion battery electrolyte and ion battery thereof Pending CN113078355A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108140888A (en) * 2015-09-25 2018-06-08 日清纺控股株式会社 Additive for electrolyte solution
CN110506358A (en) * 2017-03-30 2019-11-26 三井化学株式会社 Nonaqueous electrolyte for battery and lithium secondary battery
CN112310475A (en) * 2019-07-31 2021-02-02 杉杉新材料（衢州）有限公司 Lithium ion battery non-aqueous electrolyte and lithium ion battery

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108140888A (en) * 2015-09-25 2018-06-08 日清纺控股株式会社 Additive for electrolyte solution
CN110506358A (en) * 2017-03-30 2019-11-26 三井化学株式会社 Nonaqueous electrolyte for battery and lithium secondary battery
CN112310475A (en) * 2019-07-31 2021-02-02 杉杉新材料（衢州）有限公司 Lithium ion battery non-aqueous electrolyte and lithium ion battery

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