CN115064769A - Electrolyte compatible with graphite cathode and application thereof - Google Patents
Electrolyte compatible with graphite cathode and application thereof Download PDFInfo
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- CN115064769A CN115064769A CN202210887104.3A CN202210887104A CN115064769A CN 115064769 A CN115064769 A CN 115064769A CN 202210887104 A CN202210887104 A CN 202210887104A CN 115064769 A CN115064769 A CN 115064769A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M10/0568—Liquid materials characterised by the solutes
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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
- H01M10/0569—Liquid materials characterised by the solvents
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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 provides an electrolyte compatible with a graphite cathode and application thereof. The electrolyte can solve the problem of incompatibility with a graphite cathode, further broadens the liquid range and improves the high-voltage stability.
Description
Technical Field
The invention relates to the field of alkali metal ion batteries, in particular to an electrolyte compatible with a graphite cathode and application thereof.
Background
At present, most of electrolytes have the characteristic of being difficult to be compatible with a graphite cathode, and the high-voltage oxidation stability is poor. For example, patent document CN201811464756.6 discloses that trifluorobenzene is used as an additive in the electrolyte, but the addition amount of trifluorobenzene is only 0.5 wt% to 2 wt%, which is too high to be miscible with the electrolyte, and thus the wide application and effect of trifluorobenzene are limited to be fully exerted. In addition, the halogenated benzene in the electrolyte has a narrow liquid range and relatively poor high-pressure stability.
Disclosure of Invention
Based on this, it is necessary to provide an electrolyte compatible with a graphite negative electrode, which can improve the temperature resistance and high-voltage stability of the battery, and applications thereof.
The invention adopts the following technical scheme:
the invention provides an electrolyte compatible with a graphite cathode, which is prepared by mixing the following raw materials in molar ratio: 1-1.5 moL of electrolyte salt, 3-10 moL of organic solvent, 1-10 moL of halogenated benzene and 1-10 moL of halomethylbenzene; wherein the organic solvent is at least one of propylene carbonate, ethylene glycol dimethyl ether, trimethyl phosphate, diethyl carbonate and dimethyl sulfoxide.
In some embodiments, the electrolyte compatible with the graphite negative electrode is prepared by mixing the following raw materials in a molar ratio: 1-1.2 moL of electrolyte salt, 4-6 moL of organic solvent, 4-6 moL of halogenated benzene and 1-5 moL of halogenated methylbenzene.
In some of these embodiments, the electrolyte salt is selected from at least one of lithium hexafluorophosphate, lithium difluorophosphate, lithium bistrifluoromethylsulfonyl imide, lithium tetrafluoroborate, lithium bisoxalato borate, potassium hexafluorophosphate, potassium perchlorate, potassium trifluoromethane sulfonate.
In some of these embodiments, the halogenated benzene is selected from at least one of chlorobenzene, fluorobenzene, bromobenzene, iodobenzene.
In some of these embodiments, the halomethylbenzene is selected from at least one of trifluorotoluene, trifluoromethoxybenzene, trichlorotoluene, trichloromethoxybenzene, tribromotoluene, tribromomethoxybenzene, triiodotoluene, triiodomethoxybenzene.
Preferably, the electrolyte compatible with the graphite negative electrode is prepared by mixing the following raw materials in molar ratio: 1moL of lithium hexafluorophosphate, 0.2 moL of lithium bis (oxalato) borate, 4 moL of propylene carbonate, 6moL of fluorobenzene and 1moL of trifluoromethoxybenzene.
Preferably, the electrolyte compatible with the graphite negative electrode is prepared by mixing the following raw materials in molar ratio: 1moL of lithium bis (fluorosulfonyl) imide, 0.2 moL of lithium bis (oxalato) borate, 5moL of propylene carbonate, 6moL of bromobenzene and 1moL of trifluoromethyl benzene.
The invention also provides the application of the electrolyte compatible with the graphite cathode in the preparation of the alkali metal ion battery with high pressure oxidation resistance and stability.
The invention also provides an alkali metal ion battery which comprises a positive electrode, a graphite negative electrode, a diaphragm and the electrolyte compatible with the graphite negative electrode.
In some of these embodiments, the positive electrode is selected from one of a lithium iron phosphate positive electrode, a lithium cobaltate positive electrode, a lithium manganate positive electrode, a lithium nickel manganese oxide positive electrode, a lithium rich manganese based positive electrode, and a layered ternary positive electrode.
Compared with the prior art, the invention has the beneficial effects that:
the electrolyte obtained by screening through a large number of tests and prepared by mixing electrolyte salt, organic solvent, halogenated benzene and halomethylbenzene in specific types and proportions can solve the problem of incompatibility with a graphite cathode, further broaden the liquid range and improve the high-voltage stability.
Drawings
Fig. 1 is a charge and discharge graph at 0.1C for a lithium ion battery using the electrolytes of example 1 and comparative example 1.
Fig. 2 is a graph of the cycle performance at 1C for a lithium ion battery using the electrolyte of example 2.
Fig. 3 is a charge and discharge graph at 0.1C for a lithium ion battery using the electrolytes of example 3 and comparative example 2.
Fig. 4 is a charge and discharge graph at 0.1C for a lithium ion battery using the electrolytes of example 4 and comparative example 3.
Detailed Description
The present invention is further described in detail below with reference to specific examples so that those skilled in the art can more clearly understand the present invention.
The following examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention. All other embodiments obtained by a person skilled in the art based on the specific embodiments of the present invention without any inventive step are within the scope of the present invention.
In the examples of the present invention, all the raw material components are commercially available products well known to those skilled in the art, unless otherwise specified; in the examples of the present invention, unless otherwise specified, all technical means used are conventional means well known to those skilled in the art.
Example 1
This example provides an electrolyte comprising lithium bis-fluorosulfonylimide, propylene carbonate, fluorobenzene, and trifluorotoluene in a molar ratio of 1:5:7: 3.
The preparation method of the electrolyte comprises the following steps: dissolving lithium bis (fluorosulfonyl) imide in propylene carbonate in a glove box, stirring and mixing uniformly at room temperature, adding fluorobenzene and mixing uniformly, and adding benzotrifluoride and mixing uniformly.
Example 2
This example provides an electrolyte comprising lithium hexafluorophosphate, propylene carbonate, fluorobenzene and trifluoromethoxybenzene in a molar ratio of 1:5:7: 10.
The preparation method of the electrolyte comprises the following steps: in a glove box, firstly dissolving lithium hexafluorophosphate in propylene carbonate, stirring and mixing uniformly at room temperature, then adding fluorobenzene and mixing uniformly, and then adding trifluoromethoxybenzene and mixing uniformly.
Example 3
This example provides an electrolyte comprising lithium bis-fluorosulfonylimide, ethylene glycol dimethyl ether, fluorobenzene, and trichloromethoxybenzene in a molar ratio of 1:3:1: 10.
The preparation method of the electrolyte comprises the following steps: dissolving lithium bis (fluorosulfonyl) imide in ethylene glycol dimethyl ether in a glove box, stirring and mixing uniformly at room temperature, adding fluorobenzene and mixing uniformly, adding trichloromethoxybenzene and mixing uniformly.
Example 4
This example provides an electrolyte comprising lithium tetrafluoroborate, trimethyl phosphate, bromobenzene, and tribromomethoxybenzene in a molar ratio of 1:3:7: 1.
The preparation method of the electrolyte comprises the following steps: in a glove box, firstly, dissolving lithium tetrafluoroborate in trimethyl phosphate, stirring and mixing uniformly at room temperature, then adding fluorobenzene and mixing uniformly, then adding tribromomethoxybenzene and mixing uniformly.
Example 5
This example provides an electrolyte comprising lithium bis-fluorosulfonylimide, diethyl carbonate, iodobenzene, and tribromomethoxybenzene in a molar ratio of 1.2:3:3: 1.
The preparation method of the electrolyte comprises the following steps: dissolving lithium bis (fluorosulfonyl) imide in diethyl carbonate in a glove box, stirring and mixing uniformly at room temperature, adding iodobenzene and mixing uniformly, adding tribromomethoxybenzene and mixing uniformly.
Example 6
This example provides an electrolyte comprising lithium bis (oxalato) borate, dimethyl sulfoxide, iodobenzene, and trichloromethoxybenzene in a molar ratio of 1.2:10:10: 1.
The preparation method of the electrolyte comprises the following steps: in a glove box, firstly dissolving lithium bis (oxalato) borate in dimethyl sulfoxide, stirring and mixing uniformly at room temperature, then adding iodobenzene and mixing uniformly, and then adding trichloromethoxybenzene and mixing uniformly.
Example 7
This example provides an electrolyte comprising lithium bis-fluorosulfonylimide, dimethyl sulfoxide, iodobenzene, and triiodomethoxybenzene in a molar ratio of 1:7:5: 3.
The preparation method of the electrolyte comprises the following steps: dissolving lithium bis (fluorosulfonyl) imide in dimethyl sulfoxide in a glove box, stirring and uniformly mixing at room temperature, adding iodobenzene, uniformly mixing, adding triiodomethoxybenzene, and uniformly mixing.
Example 8
This example provides an electrolyte comprising lithium hexafluorophosphate, lithium bis (oxalato) borate, propylene carbonate, fluorobenzene and trifluoromethoxybenzene in a molar ratio of 1:0.2:4:6: 1.
The preparation method of the electrolyte comprises the following steps: in a glove box, firstly dissolving lithium hexafluorophosphate in propylene carbonate, stirring and mixing uniformly at room temperature, then adding fluorobenzene and mixing uniformly, then adding trifluoromethoxybenzene and mixing uniformly, and adding 0.2 mol of lithium bis (oxalate) borate.
Example 9
This example provides an electrolyte comprising lithium bis (fluorosulfonylimide), lithium bis (oxalato) borate, propylene carbonate, bromobenzene, and trifluoromethylbenzene in a molar ratio of 1:0.2:5:6: 1.
The preparation method of the electrolyte comprises the following steps: dissolving lithium bis (fluorosulfonyl) imide in propylene carbonate in a glove box, stirring and mixing uniformly at room temperature, adding bromobenzene and mixing uniformly, adding trifluoromethylbenzene and mixing uniformly, and adding 0.2 mol of lithium bis (oxalato) borate.
Comparative example 1
The comparative example provides an electrolyte comprising lithium bis (fluorosulfonyl) imide and propylene carbonate in a molar ratio of 1: 5.
Comparative example 2
This comparative example provides an electrolyte comprising lithium bis-fluorosulfonylimide and ethylene glycol dimethyl ether in a molar ratio of 1: 3.
Comparative example 3
This comparative example provides an electrolyte comprising lithium bis-fluorosulfonylimide and trimethyl phosphate in a molar ratio of 1: 3.
Comparative example 4
This comparative example provides an electrolyte comprising lithium bis-fluorosulfonylimide, propylene carbonate, and fluorobenzene in a molar ratio of 1:5: 7.
Comparative example 5
This comparative example provides an electrolyte comprising lithium bis-fluorosulfonylimide, propylene carbonate, and trifluorotoluene in a molar ratio of 1:3: 7.
Comparative example 6
This comparative example provides an electrolyte comprising lithium hexafluorophosphate, propylene carbonate and trichloromethoxybenzene in a molar ratio of 1:5: 7.
Comparative example 7
This comparative example provides an electrolyte comprising lithium perchlorate, ethylene glycol dimethyl ether, and iodobenzene in a molar ratio of 1:5: 5.
Comparative example 8
This comparative example provides an electrolyte comprising lithium bis fluorosulfonylimide, diethyl carbonate, and tribromomethoxybenzene in a molar ratio of 1:7: 9.
Comparative example 9
The present comparative example provides an electrolyte comprising lithium bis (fluorosulfonyl) imide, lithium bis (oxalato) borate, propylene carbonate, and trifluoromethylbenzene at a ratio of 1:0.2:5: 1.
The electrolytes prepared in examples 1 to 9 and comparative examples 1 to 9 were tested for electrical conductivity and contact angle with the separator, respectively. Higher conductivity indicates faster electron transmission efficiency, smaller contact angle indicates better electrolyte wettability, and the two are beneficial to improving the rate capability. In the conductivity test, the electrolyte is placed in a constant temperature bath, and the conductivity at that temperature is measured with a conductivity meter. In the contact angle test, 40 μ L of electrolyte is vertically dropped on the surface of a PP diaphragm, and a contact angle formed by the electrolyte and the diaphragm at the dropping moment is recorded by a contact angle meter. The results are shown in the following table:
further, electrochemical performance tests were performed on the electrolytes prepared in examples 1 to 9 and comparative examples 1 to 9, in a graphite/Li half cell, a button cell was assembled using graphite and metallic lithium as positive and negative electrodes, the electrolyte was 40 μ L, a PP separator was used, and after the assembled cell was left to stand for 24 hours, charge and discharge tests were performed at a current of 0.1C, and the first coulomb efficiency was recorded. In the NCM 811/graphite all-cell, button cell batteries were assembled with the NCM811 and graphite as positive and negative electrodes, respectively. The electrolyte is 40 mu L, a PP diaphragm is adopted, the packed battery is statically placed for 24 h and then is charged and discharged at a constant current of 0.5C, and the capacity retention rate after circulation is recorded. Impedance of the NCM 811/graphite full cell after 10 turns of 0.1C activation is performed on a CHI Chen Hua test system, and the test interval is 100KHz-100 Mhz. The results are shown in the following table:
the higher conductivity at low temperature indicates better low temperature resistance of the electrolyte. Meanwhile, the electrolyte prepared by the embodiment is subjected to low-temperature and high-temperature storage experiments to represent the temperature resistance. The test mode is as follows: 2ml of electrolyte (pH 7) is taken out and sealed in a reagent bottle, the reagent bottle is respectively placed in the environment of 60 ℃ below zero and 60 ℃, the storage is carried out for 10 days, and the state and the characteristics of the electrolyte are observed. The electrolyte solidified at low temperature is difficult to use, and lithium salt is precipitated to destroy the electrolyte. The ideal electrolyte should be clear and transparent, no discoloration occurs, and deeper colors indicate more severe decomposition. The lower the pH, the more acidic the electrolyte, the more severe the property change. In combination with the low-temperature conductivity, the low-temperature and high-temperature storage, it can be seen that the electrolyte prepared in the above example generally has more excellent wide-temperature characteristics.
The high-voltage stability can be judged by the 4.5V voltage capacity retention ratio in the NCM 811/graphite full cell. The better the cycle performance is, the better the high-voltage stability of the electrolyte and the compatibility of the anode and cathode materials are. Further, the application also tested the LSV curve of the electrolyte of the examples: the copper foil and the metal lithium sheet are assembled into a battery, the battery is scanned from the open-circuit voltage in the positive direction at the scanning speed of 1mVs-1, the voltage value when the current reaches 10 milliamperes is recorded, and the higher the voltage value is, the better the high-voltage stability is.
It should be noted that the above examples are only for further illustration and description of the technical solution of the present invention, and are not intended to further limit the technical solution of the present invention, and the method of the present invention is only a preferred embodiment, and is not intended to limit the protection scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The electrolyte compatible with the graphite cathode is characterized by being prepared by mixing the following raw materials in molar ratio: 1-1.5 moL of electrolyte salt, 3-10 moL of organic solvent, 1-10 moL of halogenated benzene and 1-10 moL of halomethylbenzene;
wherein the organic solvent is at least one of propylene carbonate, ethylene glycol dimethyl ether, trimethyl phosphate, diethyl carbonate and dimethyl sulfoxide.
2. The electrolyte compatible with the graphite negative electrode according to claim 1, which is prepared by mixing the following raw materials in a molar ratio: 1-1.2 moL of electrolyte salt, 4-6 moL of organic solvent, 4-6 moL of halogenated benzene and 1-5 moL of halogenated methylbenzene.
3. The electrolyte compatible with the graphite negative electrode according to claim 1 or 2, wherein the electrolyte salt is selected from at least one of lithium hexafluorophosphate, lithium difluorophosphate, lithium bistrifluoromethylsulfonyl imide, lithium bistrifluorosulfonimide, lithium tetrafluoroborate, lithium bisoxalato borate, potassium hexafluorophosphate, potassium perchlorate, and potassium trifluoromethanesulfonate.
4. The electrolyte compatible with the graphite negative electrode according to claim 1 or 2, wherein the halogenated benzene is at least one selected from chlorobenzene, fluorobenzene, bromobenzene and iodobenzene.
5. The electrolyte compatible with the graphite anode according to claim 1 or 2, wherein the halomethylbenzene is selected from at least one of trifluorotoluene, trifluoromethoxybenzene, trichlorotoluene, trichloromethoxybenzene, tribromotoluene, tribromomethoxybenzene, triiodotoluene, and triiodomethoxybenzene.
6. The electrolyte compatible with the graphite negative electrode according to claim 1 or 2, which is prepared by mixing the following raw materials in a molar ratio:
1moL of lithium hexafluorophosphate, 0.2 moL of lithium bis (oxalato) borate, 4 moL of propylene carbonate, 6moL of fluorobenzene and 1moL of trifluoromethoxybenzene.
7. The electrolyte compatible with the graphite negative electrode according to claim 1 or 2, which is prepared by mixing the following raw materials in a molar ratio:
1moL of lithium bis (fluorosulfonyl) imide, 0.2 moL of lithium bis (oxalato) borate, 5moL of propylene carbonate, 6moL of bromobenzene and 1moL of trifluoromethyl benzene.
8. Use of an electrolyte compatible with a graphite negative electrode according to any one of claims 1 to 7 for the preparation of an alkali metal ion battery having high oxidative stability under high pressure.
9. An alkali metal ion battery comprising a positive electrode, a graphite negative electrode, a separator, and the electrolyte solution compatible with the graphite negative electrode according to any one of claims 1 to 7.
10. The alkali metal ion battery of claim 9, wherein the positive electrode is selected from one of a lithium iron phosphate positive electrode, a lithium cobaltate positive electrode, a lithium manganate positive electrode, a lithium nickel manganese oxide positive electrode, a lithium rich manganese based positive electrode, and a layered ternary positive electrode.
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Cited By (2)
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| CN116231090A (en) * | 2023-05-06 | 2023-06-06 | 华中科技大学 | High-pressure-resistant flame-retardant electrolyte compatible with graphite and lithium ion battery |
| CN116565324A (en) * | 2023-07-05 | 2023-08-08 | 华中科技大学 | Lithium ion battery electrolyte and lithium ion battery comprising same |
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