CN110838595A - Lithium ion battery electrolyte and application thereof - Google Patents
Lithium ion battery electrolyte and application thereof Download PDFInfo
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- CN110838595A CN110838595A CN201810926898.3A CN201810926898A CN110838595A CN 110838595 A CN110838595 A CN 110838595A CN 201810926898 A CN201810926898 A CN 201810926898A CN 110838595 A CN110838595 A CN 110838595A
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
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- 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
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Abstract
The invention relates to a lithium ion battery electrolyte, which comprises a solvent, lithium salt and an additive, wherein the additive comprises a fluorine-containing nonionic surfactant shown as a structural formula (1),wherein R is1、R3Independently selected from one of fluoroalkyl, fluoroalkoxy, fluorophenyl, fluorophenoxy and fluoro group consisting of O, S, N and P, wherein fluoro is fully or partially substituted; r2Independently selected from alkyl, alkoxy, O, S, N and P, and n is an integer of 3-12. The electrolyte of the lithium ion battery has high wettability, and the lithium ion battery using the electrolyte has good high-temperature output characteristic, multiplying power and cyclicityCan be used.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a lithium ion battery electrolyte and application thereof.
Background
Lithium ion batteries are more and more widely inserted into the production and life of people, which makes the safety problem of the lithium ion batteries become the key point of attention, and the solution of the safety problem of the lithium ion batteries in the aspect of electrolytes is as follows: the first way is as follows: the research on the electrolyte of the all-solid-state lithium ion battery is still in the research and development stage at present, is not mature, and the industrialization route is long; and (2) a second way: the improvement of the existing lithium ion battery electrolyte system, namely using a flame-retardant even non-combustible solvent (fluorine-containing solvent) or a flame retardant is one of the most promising approaches for solving the flammability problem of the existing lithium ion battery electrolyte, and the flame-retardant, non-combustible and non-combustible solvent has little damage to the battery performance and obvious effect of inhibiting the electrolyte from burning. However, the flame-retardant and even non-combustible solvents generally have high viscosity, the battery is difficult to absorb liquid, and a certain amount of surfactant, namely wetting agent, needs to be added.
Disclosure of Invention
The invention aims to provide a lithium ion battery electrolyte with improved wettability and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides an electrolyte of a lithium ion battery, which comprises a solvent, lithium salt and an additive, wherein the additive comprises a fluorine-containing nonionic surfactant shown as a structural formula (1),
wherein R is1、R3Independently selected from one of fluoroalkyl, fluoroalkoxy, fluorophenyl, fluorophenoxy and fluoro group consisting of O, S, N and P, wherein fluoro is fully or partially substituted; r2Independently selected from alkyl, alkoxy, O, S, N and P, and n is an integer of 3-12.
Preferably, the fluorine-containing nonionic surfactant is perfluoroalkyl alcohol polyoxyethylene ether and/or oleic acid polyethylene glycol phosphate.
Preferably, the addition amount of the fluorine-containing nonionic surfactant is 0.001 to 2%, more preferably 0.05 to 1%, and still more preferably 0.1 to 0.5% of the total mass of the lithium ion battery electrolyte.
Preferably, the additive also comprises other additives accounting for 0.01-20% of the total mass of the lithium ion battery electrolyte, and further preferably, the addition amount of the other additives is 0.1-10% of the total mass of the lithium ion battery electrolyte, and more preferably 0.1-5%.
Further preferably, the other additive is one or more of Vinylene Carbonate (VC), 1, 3-Propane Sultone (PS), ethylene carbonate (VEC), Biphenyl (BP), Cyclohexylbenzene (CHB), propylene sulfate (TSA), trioctyl phosphate (TOP), vinyl sulfate, vinyl 4-methylsulfate, vinyl sulfite, and lithium difluorophosphate.
Preferably, the lithium salt is lithium hexafluorophosphate (LiPF)6) Lithium tetrafluoroborate (LiBF)4) Lithium hexafluoroarsenate (LiAsF)6) Anhydrous lithium perchlorate (LiClO)4) Lithium bis (trifluoromethanesulfonate imide) (LiN (SO)2CF3)2) Lithium difluorooxalate phosphate (LiPF)2(C2O4)2) Lithium difluorophosphate (LiPO)2F2) Lithium trifluoromethanesulfonate (LiSO)3CF3) Lithium bis (oxalato) borate (LiC)2O4BC2O4) Lithium monooxalyldifluoroborate (LiF)2BC2O4) Lithium bis (fluorosulfonylimide) (LiN (SO)2F)2) One or more of them.
Preferably, the concentration of the lithium salt is 1-5 mol/L, and more preferably 1-3 mol/L.
Preferably, the solvent is one or more of gamma-butyrolactone (GBL), Ethylene Carbonate (EC), Propylene Carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carbonate (DMC), Ethyl Methyl Carbonate (EMC), diethyl carbonate (DEC), Methyl Propyl Carbonate (MPC), Methyl Propionate (MP), Ethyl Propionate (EP), Propyl Propionate (PP), Methyl Acetate (MA), Ethyl Acetate (EA), Propyl Acetate (PA), Methyl Butyrate (MB), butyl ethyl Ester (EB), Propyl Butyrate (PB), fluoroethyl acetate (FEA), methyl Fluoropropionate (FMP), propyl fluoropropionate, and ethyl fluoropropionate.
More preferably, the solvent is a mixed solvent of gamma-butyrolactone, propylene carbonate and dimethyl carbonate in a volume ratio of 1: 0.9-1.1, or a mixed solvent of ethylene carbonate and ethyl methyl carbonate in a volume ratio of 1: 0.9-1.1, or a mixed solvent of dimethyl carbonate, ethylene carbonate and ethyl methyl carbonate in a volume ratio of 1: 0.9-1.1, or a mixed solvent of fluoroethylene carbonate, propylene carbonate and methyl fluoropropionate in a volume ratio of 1: 0.9-1.1.
The invention also aims to provide a lithium ion battery, which comprises a positive electrode, a negative electrode and the electrolyte, wherein the electrolyte is the lithium ion battery electrolyte.
Preferably, the negative electrode is one or a combination of several selected from lithium titanate, artificial graphite and natural graphite, and the positive electrode is one or a combination of several selected from lithium cobaltate, ternary materials and lithium nickel manganese oxide.
The inventor finds that the fluorine-containing nonionic surfactant has the advantages of high surface activity, high heat-resistant stability, low flammability, high chemical stability and the like. The fluorine-containing nonionic surface active agent is one of all the surfactants with highest activity so far, which is the most important property of the fluorine-containing nonionic surface active agent and can obviously reduce the surface tension of a solution when the concentration is very low; the non-ionic surfactant is not in ionic state in solution, so that it has high stability, less influence of strong electrolyte and acid and alkali, good compatibility, high solubility in various solvents and no strong adsorption on solid surface, and may be used in lithium ion cell with non-aqueous electrolyte.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the electrolyte of the lithium ion battery has high wettability, and the lithium ion battery using the electrolyte has good high-temperature output characteristic, multiplying power and cycle performance.
Drawings
Fig. 1 is a contact angle of an electrolyte of example 1 on an artificial graphite anode material, a separator, and a ternary cathode material, respectively;
FIG. 2 is an ordinary temperature cycle performance of the battery of example 1;
FIG. 3 is a contact angle of the electrolyte of example 2 on an artificial graphite anode material;
FIG. 4 is a graph showing the results of high-temperature cycles at 45 ℃ of the batteries of example 3, example 4 and comparative example 2;
FIG. 5 is a graph showing the results of high temperature cycles at 45 ℃ of the batteries of example 5, example 6, comparative example 3 and comparative example 4;
FIG. 6 is a graph showing the results of high-temperature cycles at 45 ℃ of the batteries of example 7, example 8 and comparative example 5.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The perfluoroalkyl alcohol polyoxyethylene ether used in the present invention can be perfluoroalkyl alcohol polyoxyethylene ether available from the fluorination technology, and the perfluoroalkyl alcohol polyoxyethylene ethers used in the following examples are all perfluoroalkyl alcohol polyoxyethylene ethers (FEO-500) obtained from the fluorination technology.
The oleic acid polyethylene glycol phosphate ester adopted in the invention can be oleic acid polyethylene glycol phosphate ester purchased from sanderian chemical industry, and the oleic acid polyethylene glycol phosphate ester adopted in the following examples is oleic acid polyethylene glycol phosphate ester (PEG400MO phosphate ester) of sanderian chemical industry.
Example 1:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a GBL/PC/DMC ratio of 1/1/1 by volume, and 1.0mol/L of lithium hexafluorophosphate (LiPF) was dissolved6) Therein is provided withThen, perfluoroalkyl alcohol polyoxyethylene ether in an amount of 0%, 0.01%, 0.05%, 0.1%, 0.5% of the total amount of the electrolyte is added to the electrolyte.
And testing contact angles of the electrolytes on the artificial graphite cathode material, the diaphragm and the ternary anode material respectively, forming the battery by selecting the ternary graphite battery and charging and discharging at 0.1 ℃, and testing the normal-temperature cycle performance of the battery. The test results are shown in fig. 1 and 2.
Example 2:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in an EC/EMC (1/1 vol), and then 3.0mol/L of lithium hexafluorophosphate (LiPF) was dissolved6) Then, perfluoroalkyl alcohol polyoxyethylene ether with the total amount of 0%, 0.1% and 0.5% of the electrolyte is respectively added into the electrolyte.
The contact angle of each electrolyte on the artificial graphite anode material was tested as shown in fig. 3.
Example 3:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of DMC/EC/EMC 1/1/1, and then 1mol/L of lithium bis (fluorosulfonyl) imide (LiN (SO)2F)2) Wherein, perfluoroalkyl alcohol polyoxyethylene ether accounting for 0.1 percent of the total amount of the electrolyte, vinylene carbonate accounting for 1 percent of the total amount of the electrolyte and lithium difluorophosphate accounting for 1 percent of the total amount of the electrolyte are added into the electrolyte.
A nickel-cobalt-aluminum graphite battery is selected, the battery is formed by 0.1C charging and discharging, the first charging and discharging efficiency is measured, and high-temperature circulation is carried out at 45 ℃. The test results are shown in table 1 and fig. 4.
Example 4:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of DMC/EC/EMC 1/1/1, and then 3mol/L of lithium bis (fluorosulfonyl) imide (LiN (SO)2F)2) Wherein, perfluoroalkyl alcohol polyoxyethylene ether accounting for 0.5 percent of the total amount of the electrolyte, vinylene carbonate accounting for 1 percent of the total amount of the electrolyte and lithium difluorophosphate accounting for 1 percent of the total amount of the electrolyte are added into the electrolyte.
A nickel-cobalt-aluminum graphite battery is selected, the battery is formed by 0.1C charging and discharging, the first charging and discharging efficiency is measured, and high-temperature circulation is carried out at 45 ℃. The test results are shown in table 1 and fig. 4.
Comparative example 1
In an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of DMC/EC/EMC 1/1/1, and then 3mol/L of lithium bis (fluorosulfonyl) imide (LiN (SO)2F)2) To this electrolyte, vinylene carbonate and lithium difluorophosphate were added in an amount of 1% of the total electrolyte.
A nickel-cobalt-aluminum graphite battery is selected, the battery is formed by 0.1C charging and discharging, the first charging and discharging efficiency is measured, and high-temperature circulation is carried out at 45 ℃. The test results are shown in table 1 and fig. 4.
Comparative example 2
In an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of DMC/EC/EMC 1/1/1, and then 3mol/L of lithium bis (fluorosulfonyl) imide (LiN (SO)2F)2) To the electrolyte, 0.1% of trioctyl phosphate, 1% of vinylene carbonate and 1% of lithium difluorophosphate were added.
A nickel-cobalt-aluminum graphite battery is selected, the battery is formed by 0.1C charging and discharging, the first charging and discharging efficiency is measured, and high-temperature circulation is carried out at 45 ℃. The test structures are shown in table 1 and fig. 4.
TABLE 1
Example 5:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a DMC/EC/EMC ratio of 1/1/1 volume ratio, and then 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved6) Wherein, perfluoroalkyl alcohol polyoxyethylene ether accounting for 0.1 percent of the total amount of the electrolyte and vinylene carbonate accounting for 0.5 percent of the total amount of the electrolyte are added into the electrolyte.
A ternary graphite battery is selected, the battery is formed by 0.1C charge-discharge, the first charge-discharge efficiency is measured, and high-temperature circulation at 45 ℃ is carried out. The test results are shown in table 2 and fig. 5.
Example 6:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a DMC/EC/EMC ratio of 1/1/1 volume ratio, and then 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved6) Wherein, perfluoroalkyl alcohol polyoxyethylene ether accounting for 0.5 percent of the total amount of the electrolyte and vinylene carbonate accounting for 0.5 percent of the total amount of the electrolyte are added into the electrolyte.
A ternary graphite battery is selected, the battery is formed by 0.1C charge-discharge, the first charge-discharge efficiency is measured, and high-temperature circulation at 45 ℃ is carried out. The test results are shown in table 2 and fig. 5.
Comparative example 3
In an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a DMC/EC/EMC ratio of 1/1/1 volume ratio, and then 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved6) To this electrolyte, vinylene carbonate was added in an amount of 0.5% of the total amount of the electrolyte.
A ternary graphite battery is selected, the battery is formed by 0.1C charge-discharge, the first charge-discharge efficiency is measured, and high-temperature circulation at 45 ℃ is carried out. The test results are shown in table 2 and fig. 5.
Comparative example 4
In an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a DMC/EC/EMC ratio of 1/1/1 volume ratio, and then 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved6) To the electrolyte, trioctyl phosphate was added in an amount of 0.1% by weight based on the total amount of the electrolyte, and vinylene carbonate was added in an amount of 0.5% by weight based on the total amount of the electrolyte.
A ternary graphite battery is selected, the battery is formed by 0.1C charge-discharge, the first charge-discharge efficiency is measured, and high-temperature circulation at 45 ℃ is carried out. The test results are shown in table 2 and fig. 5.
TABLE 2
Battery numbering | Charging capacity (mAh) | Discharge capacity (mAh) | First charge-discharge efficiency (%) |
Comparative example 3 | 1479.6 | 1202.9 | 81.3 |
Comparative example 4 | 1489.7 | 1230.5 | 82.6 |
Example 5 | 1451.7 | 1290.6 | 88.9 |
Example 6 | 1495.7 | 1289.3 | 86.2 |
Example 7:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of FEC/PC/FMP 1/1/1, and 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved therein6) Wherein, oleic acid polyethylene glycol phosphate with the total amount of 0.1 percent of the electrolyte is added into the electrolyte.
The method comprises the steps of selecting a nickel-manganese anode material half cell, forming the cell by 0.1C charge-discharge, measuring the first charge-discharge efficiency, and performing normal-temperature circulation. The test results are shown in table 3 and fig. 6.
Example 8:
in an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of FEC/PC/FMP 1/1/1, and 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved therein6) Wherein, oleic acid polyethylene glycol phosphate with the total amount of 0.5 percent of the electrolyte is added into the electrolyte.
The method comprises the steps of selecting a nickel-manganese anode material half cell, forming the cell by 0.1C charge-discharge, measuring the first charge-discharge efficiency, and performing normal-temperature circulation. The test results are shown in table 3 and fig. 6.
Comparative example 5
In an argon-filled glove box (H)2O<10ppm) was mixed uniformly in a volume ratio of FEC/PC/FMP 1/1/1, and 1mol/L of lithium hexafluorophosphate (LiPF) was dissolved therein6) Wherein the process is carried out.
The method comprises the steps of selecting a nickel-manganese anode material half cell, forming the cell by 0.1C charge-discharge, measuring the first charge-discharge efficiency, and performing normal-temperature circulation. The test results are shown in table 3 and fig. 6.
TABLE 3
Battery numbering | Charging capacity (mAh/g) | Discharge capacity (mAh/g) | First charge-discharge efficiency (%) |
Comparative example 5 | 168.3 | 127.2 | 75.6 |
Example 7 | 174.6 | 144.7 | 82.9 |
Example 8 | 174.4 | 138.1 | 79.2 |
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (9)
1. The lithium ion battery electrolyte comprises a solvent, lithium salt and an additive, and is characterized in that: the additive comprises fluorine-containing nonionic surfactant shown as a structural formula (1),
wherein R is1、R3Independently selected from one of fluoroalkyl, fluoroalkoxy, fluorophenyl, fluorophenoxy and fluoro group consisting of O, S, N and P, wherein fluoro is fully or partially substituted; r2Independently selected from alkyl, alkoxy, O, S, N and P, and n is an integer of 3-12.
2. The lithium ion battery electrolyte of claim 1, wherein: the fluorine-containing nonionic surfactant is perfluoroalkyl alcohol polyoxyethylene ether and/or oleic acid polyethylene glycol phosphate.
3. The lithium ion battery electrolyte of claim 1 or 2, wherein: the addition amount of the fluorine-containing nonionic surfactant is 0.001-2% of the total mass of the lithium ion battery electrolyte.
4. The lithium ion battery electrolyte of claim 1, wherein: the additive also comprises other additives accounting for 0.01-20% of the total mass of the lithium ion battery electrolyte, wherein the other additives are one or more of Vinylene Carbonate (VC), 1, 3-Propane Sultone (PS), ethylene carbonate (VEC), Biphenyl (BP), Cyclohexylbenzene (CHB), propylene sulfate (TSA), trioctyl phosphate (TOP), vinyl sulfate, 4-methyl vinyl sulfate, vinyl sulfite and lithium difluorophosphate.
5. The lithium ion battery electrolyte of claim 1, wherein: the lithium salt is lithium hexafluorophosphate (LiPF)6) Lithium tetrafluoroborate (LiBF)4) Lithium hexafluoroarsenate (LiAsF)6) Anhydrous lithium perchlorate (LiClO)4) Lithium bis (trifluoromethanesulfonate imide) (LiN (SO)2CF3)2) Lithium difluorooxalate phosphate (LiPF)2(C2O4)2) Lithium difluorophosphate (LiPO)2F2) Lithium trifluoromethanesulfonate (LiSO)3CF3) Lithium bis (oxalato) borate (LiC)2O4BC2O4) Lithium monooxalyldifluoroborate (LiF)2BC2O4) Lithium bis (fluorosulfonylimide) (LiN (SO)2F)2) One or more of them.
6. The lithium ion battery electrolyte of claim 1 or 5, wherein: the concentration of the lithium salt is 1-5 mol/L.
7. The lithium ion battery electrolyte of claim 1, wherein: the solvent is one or more of gamma-butyrolactone (GBL), Ethylene Carbonate (EC), Propylene Carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC), diethyl carbonate (DEC), Methyl Propyl Carbonate (MPC), Methyl Propionate (MP), Ethyl Propionate (EP), Propyl Propionate (PP), Methyl Acetate (MA), Ethyl Acetate (EA), Propyl Acetate (PA), Methyl Butyrate (MB), butyl ethyl Ester (EB), Propyl Butyrate (PB), ethyl Fluoroacetate (FEA), methyl Fluoropropionate (FMP), propyl fluoropropionate and ethyl fluoropropionate.
8. A lithium ion battery comprises a positive electrode, a negative electrode and electrolyte, and is characterized in that: the electrolyte is the lithium ion battery electrolyte as defined in any one of claims 1 to 7.
9. The lithium ion battery of claim 8, wherein: the negative electrode is one or a combination of more of lithium titanate, artificial graphite and natural graphite, and the positive electrode is one or a combination of more of lithium cobaltate, ternary material and lithium nickel manganese oxide.
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