CN111430781A - Ternary high-voltage lithium ion battery electrolyte and lithium ion battery thereof - Google Patents
Ternary high-voltage lithium ion battery electrolyte and lithium ion battery thereof Download PDFInfo
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- CN111430781A CN111430781A CN202010371234.2A CN202010371234A CN111430781A CN 111430781 A CN111430781 A CN 111430781A CN 202010371234 A CN202010371234 A CN 202010371234A CN 111430781 A CN111430781 A CN 111430781A
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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
- 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
- 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 discloses a ternary high-voltage lithium ion battery non-aqueous electrolyte, which comprises a non-aqueous organic solvent, electrolyte lithium salt and an additive, wherein the additive comprises at least one fluophosphonic acid additive with a structure shown in a formula (I). The invention also discloses a lithium ion battery comprising the positive plate, the isolating membrane, the negative plate and the non-aqueous electrolyte of the ternary high-voltage lithium ion battery. The fluorophosphonic acid additive in the ternary high-voltage lithium ion battery electrolyte has the functions of removing water and acid, and prevents the lithium hexafluorophosphate from generating HF and PF by water or thermal reaction5、HPO2F2，H2PO3F and H3PO4And the like, affect battery performance; meanwhile, the intermediate of the substance reacting with hydrofluoric acid and water has good film-forming property, and the invention can effectively solve the problem of ternary high-voltage lithium by the synergistic effect of the conventional additive and the fluophosphonic acid additiveCycle performance, high temperature storage performance and low temperature discharge performance of the ion battery.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a ternary high-voltage lithium ion battery electrolyte and a lithium ion battery thereof.
Background
The lithium ion battery has the advantages of high working voltage, high energy density, long service life, wide working temperature range, environmental friendliness and the like, and is widely applied to the fields of 3C digital products, electric tools, electric automobiles, aerospace and the like. Especially in the 3C digital field, mobile electronic devices, especially smart phones, have been rapidly developed in recent years toward lighter and thinner, and higher requirements are put forward on the energy density of lithium ion batteries.
In order to increase the energy density of lithium ion batteries, a common measure is to increase the charge medium voltage of the positive electrode material, such as the voltage of the commercialized ternary material battery from 4.2V → 4.35V → 4.4V → 4.5V → 4.6V. However, the positive electrode material has certain defects under high voltage, for example, the high-voltage positive electrode active material has strong oxidizability in a lithium-deficient state, so that the electrolyte is easily oxidized and decomposed to generate a large amount of gas; in addition, the high-voltage positive active material is unstable in a lithium-deficient state, and is prone to side reactions, such as release of oxygen, dissolution of transition metal ions and the like, so that the transition metal ions are separated from crystals along with the reaction and enter the electrolyte to catalyze the decomposition of the electrolyte and damage the passivation film of the active material, and meanwhile, the transition metal ions can occupy the lithium ion migration channel of the passivation film on the surface of the negative electrode material to block the migration of the lithium ions, thereby affecting the service life of the battery, and when the lithium ion battery is used in a high-temperature and high-pressure state, the negative effects are more obvious.
When the electrolyte contains a trace amount of water or under high temperature conditions, the reaction of an electrolyte lithium salt such as lithium hexafluorophosphate with water or the thermal decomposition of lithium hexafluorophosphate generates a series of by-products such as HF, PF5、HPO2F2，H2PO3F and H3PO4Etc. which cause irreversible damage to lithium ion batteries, such as PF5The Lewis acid is used for catalyzing the oxidative decomposition of the carbonate solvent, and HF can dissolve the passive film of the positive and negative electrode interfaces, so that the solvent is oxidized and decomposed on the surfaces of the positive and negative electrodes.
At present, the main method for solving the problems is to develop a new film forming additive, but the currently developed additive can not remove water and acid, or a reaction intermediate can not form a passivation film on the interface of a positive electrode material and a negative electrode material through oxidation reduction, so as to protect the positive electrode material and the negative electrode material and avoid excessive reaction of a solvent and an electrolyte solvent. Therefore, there is a need to develop new additives to better improve the electrochemical performance of ternary high voltage lithium ion batteries.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a ternary high-voltage lithium ion battery electrolyte and a lithium ion battery thereof, wherein an additive in the ternary high-voltage lithium ion battery electrolyte has the functions of removing water and acid, and prevents lithium hexafluorophosphate from generating HF and PF by water or thermal reaction5、HPO2F2，H2PO3F and H3PO4And the like, affecting battery performance. Meanwhile, the intermediate of the additive reacting with hydrofluoric acid and water has good film-forming property, and can effectively solve the problems of cycle performance, high-temperature storage performance and low-temperature discharge performance of the ternary high-voltage lithium ion battery.
In order to achieve the purpose, the invention adopts the technical scheme that: a ternary high-voltage lithium ion battery electrolyte comprises a non-aqueous organic solvent, an electrolyte lithium salt and an additive, wherein the additive comprises at least one fluophosphonic acid additive with a structure shown in a formula (I):
wherein R is1And R2Each independently selected from any one of linear or non-linear alkyl group having less than 4 carbon atoms, fluoroalkyl group, methoxy group, ethoxy group, fluorine atom, hydrogen atom, phenyl group and cyclohexyl group.
Preferably, the fluorophosphonic acid additive is selected from dimethyl fluorophosphonate or diethyl fluorophosphonate, and the structural formula is as follows:
preferably, the mass percentage of the fluorophosphonic acid additive in the electrolyte of the ternary high-voltage lithium ion battery is 0.1-1.0%.
Preferably, the ternary high-voltage lithium ion battery electrolyte further comprises conventional additives, wherein the conventional additives are one or more of vinylene carbonate, fluoroethylene carbonate, vinyl ethylene carbonate, 1, 3-propane sultone, 1, 3-propylene sultone, methylene methane disulfonate, tris (trimethylsilane) borate, tris (trimethylsilane) phosphate, citral anhydride, 1-propyl phosphoric anhydride, triacrylate and nitrile additives.
Preferably, the nitrile additive is one or more of succinonitrile, adiponitrile, ethylene glycol bis (propionitrile) ether, and 1, 4-dicyano-2-butene; the addition amount of the nitrile additive accounts for 0.1-1.0% of the total mass of the electrolyte.
Preferably, the conventional additive is a mixture of 1, 3-Propane Sultone (PS), ethylene carbonate (DTD), 1, 3-Propylene Sultone (PST), Adiponitrile (ADN), fluoroethylene carbonate (FEC).
Preferably, the mass percentage of the conventional additive in the electrolyte of the ternary high-voltage lithium ion battery is 0.5-10.0%.
Preferably, the electrolyte lithium salt is a mixed lithium salt of lithium hexafluorophosphate and lithium difluorophosphate.
Preferably, the mass percentage of the electrolyte lithium salt in the electrolyte of the ternary high-voltage lithium ion battery is 10.5-15.0%.
In the invention, the non-aqueous organic solvent comprises a carbonate and a carboxylic ester solvent, wherein the carbonate solvent comprises a cyclic carbonate solvent and a chain carbonate solvent, the cyclic carbonate solvent is selected from at least one of ethylene carbonate and propylene carbonate, and the chain carbonate solvent is selected from one or more of diethyl carbonate, ethyl methyl carbonate, 1, 2-difluoroethylene carbonate and bis (2,2, 2-trifluoroethyl) carbonate; the carboxylic ester solvent is selected from ethyl acetate, propyl propionate, ethyl propionate, n-propyl acetate and the like. More preferably, the non-aqueous organic solvent is a mixture of Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC), Ethyl Propionate (EP) and Propyl Propionate (PP). Furthermore, the mass ratio of the ethylene carbonate to the propylene carbonate to the diethyl carbonate to the ethyl propionate to the propyl propionate is (10-20): (5-10): (20-35): (25-35): (25-35).
The invention also discloses a ternary high-voltage lithium ion battery which comprises a positive plate, an isolating membrane, a negative plate and the ternary high-voltage lithium ion battery electrolyte.
Preferably, the positive active material of the positive electrode sheet is L iNi1-x-y-zCoxMnyAlzO2Or L iAmBnPO4Wherein: 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, z is more than or equal to 0 and less than or equal to 1, x + y + z is more than or equal to 0 and less than or equal to 1, A, B are respectively Fe, Mn, Co or V, m is more than or equal to 0 and less than or equal to 1, and n is more than or equal to.
Preferably, the negative active material of the negative electrode sheet is artificial graphite, natural graphite, or SiOwThe silicon-carbon composite material is compounded with graphite, wherein w is more than 1 and less than 2.
Preferably, the positive plate is prepared by mixing L iNi positive active material0.5Co0.2Mn0.3O2The conductive agent acetylene black and the binder polyvinylidene fluoride (PVDF) are mixed according to the mass ratio of 94: 3: and 3, fully stirring and uniformly mixing in an N-methyl pyrrolidone solvent system, coating on an aluminum foil, drying, and performing cold pressing to obtain the positive plate.
Preferably, the method for preparing the negative active material comprises: preparing negative active material artificial graphite, conductive agent acetylene black, binder Styrene Butadiene Rubber (SBR), and thickener carboxymethylcellulose sodium (CMC) according to a mass ratio of 96: 1.5: 1.5: 1, fully stirring and uniformly mixing in a deionized water solvent system, coating on a copper foil, drying, and cold pressing to obtain the negative plate.
Preferably, the charge cut-off voltage of the ternary high voltage lithium ion battery of the present invention is greater than or equal to 4.4V.
Compared with the prior art, the invention has the beneficial effects that:
1. the fluorophosphonic acid additive can react with trace amount of water in electrolyte to avoid reaction of lithium hexafluorophosphate with water to produce HF and HPO2F2，H2PO3F and H3PO4Impurities cause the dissolution and damage of the anode and cathode passive films;
2. the fluorophosphonic acid additive of the invention can be decomposed with lithium hexafluorophosphate at high temperature to generate Lewis acid PF5Combined, avoiding PF5Catalyzing the solvent to perform decomposition reaction;
3. the intermediate of the reaction of the fluophosphonic acid additive and hydrofluoric acid and water has a certain anode film forming effect and plays a crucial role in protecting anode materials, the moisture content in the electrolyte is below 11ppm, and the acidity is below 6.9 ppm;
4. the fluorophosphoric acid additive and the conventional additive have a synergistic effect, so that the film forming quality of the negative electrode is better, the reaction activity of the electrode material and the electrolyte is reduced, the microstructure of the electrode material is stabilized, and the cycle performance and the high-temperature performance of the high-voltage lithium ion battery are improved; meanwhile, the formed solid electrolyte membrane has low impedance, which is beneficial to improving the internal dynamic characteristics of the lithium ion battery and reducing the interface impedance, thereby effectively improving the cycle performance, the high-temperature storage performance and the low-temperature performance of the ternary high-voltage lithium ion battery.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
Example 1
Preparing electrolyte: in a glove box filled with argon, Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC), Ethyl Propionate (EP) and Propyl Propionate (PP) were mixed in a mass ratio EC: PC: DEC: EP: PP 20: 10: 20: 30: 20 to obtain a mixed non-aqueous organic solvent, and then slowly adding 12.5 percent of the mixed non-aqueous organic solvent based on the total mass of the electrolyteLithium hexafluorophosphate (L iPF) as the conductive lithium salt6) And 0.8% of lithium difluorophosphate (L iPO) based on the total mass of the electrolyte2F2) And finally, adding 0.5 percent of dimethyl fluorophosphate additive based on the total mass of the electrolyte, and uniformly stirring to obtain the lithium ion battery electrolyte of the embodiment 1.
Examples 2 to 9
Examples 2 to 9
Examples 2 to 9 are also specific examples of the preparation of the electrolyte, and the parameters and preparation method are the same as those of example 1 except that the composition ratios of the components of the electrolyte are added as shown in Table 1.
Comparative examples 1 to 6
In comparative examples 1 to 6, the parameters and preparation method were the same as in example 1 except that the composition ratios of the respective components of the electrolyte were changed as shown in Table 1.
TABLE 1 composition ratios of the components of the electrolytes of examples 1-9 and comparative examples 1-6
Note: the concentration of the lithium salt is the mass percentage content in the electrolyte;
the content of the fluophosphonic acid 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 nonaqueous organic solvent is mass ratio.
Performance testing
Preparing a lithium ion battery:
mixing the positive electrode active material L iNi0.5Co0.2Mn0.3O2Acetylene black as conductive agent and polyvinylidene fluoride as binderVinyl fluoride (PVDF) in a mass ratio of 94: 3: 3, fully stirring and uniformly mixing in an N-methylpyrrolidone solvent system, coating the mixture on an aluminum foil, drying and cold-pressing the mixture to obtain the positive plate, wherein the preparation method of the negative active material comprises the following steps: preparing negative active material artificial graphite, conductive agent acetylene black, binder Styrene Butadiene Rubber (SBR), and thickener carboxymethylcellulose sodium (CMC) according to a mass ratio of 96: 1.5: 1.5: 1, fully stirring and uniformly mixing in a deionized water solvent system, coating on a copper foil, drying, and cold pressing to obtain the negative plate.
Polyethylene (PE) is used as a base film, and a nano aluminum oxide coating is coated on the base film to be used as an isolating film.
And sequentially laminating the positive plate, the isolating membrane and the negative plate, winding the positive plate, the isolating membrane and the negative plate along the same direction to obtain a bare cell, placing the bare cell in an outer package, injecting the electrolyte prepared in the examples 1-9 and the comparative examples 1-6, and carrying out the procedures of packaging, standing at 45 ℃, high-temperature clamp formation, secondary packaging, capacity grading and the like to obtain the ternary high-voltage lithium ion battery.
The following performance tests were performed on the batteries of examples 1-9 and comparative examples 1-6, respectively, and the test results are shown in tables 2 and 3, wherein:
(1) and (3) testing the normal-temperature cycle performance of the ternary high-voltage battery: and (3) charging the battery after capacity grading to 4.4V at a constant current and a constant voltage of 1C and stopping the current to 0.02C at 25 ℃, then discharging to 3.0V at a constant current of 1C, and calculating the capacity retention rate of the 500 th cycle after the battery is cycled according to the cycle and is charged/discharged for 500 cycles. The calculation formula is as follows:
the 500 th-cycle capacity retention ratio (%) (500 th-cycle discharge capacity/first-cycle discharge capacity) × 100% was 100%.
(2) And (3) testing the constant-temperature storage gas production rate and the capacity residual rate of the ternary high-voltage battery at 60 ℃: firstly, the battery is circularly charged and discharged for 1 time (4.4V-3.0V) at the normal temperature at 0.5C, and the discharge capacity C of the battery before storage is recorded0Then charging the battery to 4.4V full-voltage state at constant current and constant voltage, and testing the thickness V of the battery before high-temperature storage by using a drainage method1Then the battery is put into a thermostat with the temperature of 60 ℃ for storage for 7 days, the battery is taken out after the storage is finished, and the volume V of the battery after the storage is tested after the battery is cooled for 8 hours2And calculating the battery after the battery is stored for 7 days at the constant temperature of 60 DEG CGas production; after the battery is cooled for 24H at room temperature, the constant current discharge is carried out on the battery to 3.0V at 0.5C again, and the discharge capacity C after the battery is stored is recorded1And calculating the capacity residual rate of the battery after 7 days of constant-temperature storage at 60 ℃, wherein the calculation formula is as follows:
the gas production of the battery is V after 7 days of storage at 60 DEG C2-V1；
The residual capacity rate after 7 days of constant temperature storage at 60 ℃ is C1/C0*100％。
(3) And (3) testing the 45 ℃ cycle performance of the ternary high-voltage battery: and (3) charging the battery after capacity grading to 4.4V at a constant current and a constant voltage of 1C at 45 ℃, stopping the current to 0.02C, then discharging to 3.0V at a constant current of 1C, and calculating the capacity retention rate of the 300 th cycle after the cycle is repeated and the charge/discharge is performed for 300 times. The calculation formula is as follows:
the 300 th cycle capacity retention (%) — × 100% (300 th cycle discharge capacity/first cycle discharge capacity).
(4) Testing the water acidity after the electrolyte is stored for 24 hours at 60 ℃: performed as SJ/T11723-2018, the free acid content, calculated as HF, is calculated according to the following formula:
CHF＝C*V*MHF*1000/m
in the formula:
CHFfree acid content (calculated as HF), mg/kg;
c- -concentration of sodium methoxide standard titration solution, mol/L;
v- - - -titration of the volume of sodium methoxide standard titration solution consumed, m L;
m-sample mass, g;
MHF-molar mass of hydrofluoric acid (20.006), g/mol.
The arithmetic mean of the two test values was taken as the test result.
TABLE 2 test results of water acidity after 24-hour storage at 45 ℃ for electrolytes of examples and comparative examples
Remarking: the lithium ion battery electrolyte is specified in the standard, after the electrolyte is prepared, the water content is less than or equal to 20ppm, and the acidity is less than or equal to 50 ppm.
TABLE 3 results of testing cycle characteristics and high-temperature storage characteristics of batteries of examples and comparative examples
As can be seen from the comparison of the results of the cell performance test of comparative example 1 and examples 1-6 in Table 2: the fluorophosphonic acid additive can remove water and acid, and inhibit the increase of water and acidity after the electrolyte is stored, because the substances react with water and hydrofluoric acid to avoid the dissolution of a positive and negative electrode passive film caused by excessive hydrofluoric acid, and meanwhile, the fluorophosphonic acid additive can be thermally decomposed with a product PF of lithium hexafluorophosphate5Binding to avoid Lewis acid type substance PF5Catalytic dissolution and decomposition of additives.
As can be seen from the comparison of the results of the cell performance test of comparative example 1 and examples 1-6 in Table 3: the addition of the fluophosphonic acid can improve the electrochemical performance of the high-voltage ternary lithium ion battery.
As can be seen from a comparison of the results of the battery performance tests of examples 7-9 in Table 3: the intermediate of the reaction of the fluophosphonic acid additive and hydrofluoric acid and water participates in the film forming action of the anode, thereby avoiding the generation of cracks in NCM particles in the circulating process, reducing the dissolution of transition metal elements at high temperature and further improving the electrochemical performance of the lithium ion battery; meanwhile, the fluorophosphoric acid additive and other additives have synergistic effect, and the electrochemical performance of the lithium ion battery can be greatly improved.
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 electrolyte of the ternary high-voltage lithium ion battery is characterized by comprising a non-aqueous organic solvent, an electrolyte lithium salt and an additive, wherein the additive comprises at least one fluophosphonic acid additive with a structure shown in a formula (I):
wherein R is1And R2Each independently selected from any one of linear or non-linear alkyl group having less than 4 carbon atoms, fluoroalkyl group, methoxy group, ethoxy group, fluorine atom, hydrogen atom, phenyl group and cyclohexyl group.
2. The ternary high voltage lithium ion battery electrolyte of claim 1 wherein the fluorophosphonic acid based additive is selected from dimethyl fluorophosphonate or diethyl fluorophosphonate.
3. The ternary high voltage lithium ion battery electrolyte of claim 1, wherein the mass percentage of the fluorophosphonic acid additive in the ternary high voltage lithium ion battery electrolyte is 0.1-1.0%.
4. The ternary high voltage lithium ion battery electrolyte of claim 1 further comprising conventional additives, wherein the conventional additives are one or more of vinylene carbonate, fluoroethylene carbonate, vinyl ethylene carbonate, 1, 3-propane sultone, 1, 3-propene sultone, methylene methanedisulfonate, tris (trimethylsilane) borate, tris (trimethylsilane) phosphate, citrakoanhydride, 1-propylphosphoric anhydride, triacrylate, and nitrile additives.
5. The ternary high voltage lithium ion battery electrolyte of claim 4 wherein the conventional additive is a mixture of 1, 3-propane sultone, ethylene carbonate, 1, 3-propylene sultone, adiponitrile, fluoroethylene carbonate.
6. The electrolyte of a ternary high-voltage lithium ion battery according to claim 1, wherein the conventional additive is contained in the electrolyte of a ternary high-voltage lithium ion battery in an amount of 0.5 to 10.0% by mass.
7. The ternary high voltage lithium ion battery electrolyte of claim 1 wherein the electrolyte lithium salt is a mixed lithium salt of lithium hexafluorophosphate and lithium difluorophosphate.
8. The ternary high voltage lithium ion battery electrolyte of claim 1, wherein the mass percentage of the electrolyte lithium salt in the ternary high voltage lithium ion battery electrolyte is 10.5-15.0%.
9. The ternary high voltage lithium ion battery electrolyte of claim 1 wherein the non-aqueous organic solvent is a mixture of ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl propionate and propyl propionate.
10. A ternary high voltage lithium ion battery, characterized in that, the ternary high voltage lithium ion battery comprises a positive plate, a separation film, a negative plate and the electrolyte of the ternary high voltage lithium ion battery of any one of claims 1 to 9.
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| CN114006042A (en) * | 2021-10-21 | 2022-02-01 | 湖南立方新能源科技有限责任公司 | Electrolyte for sodium ion battery and sodium ion battery |
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