CN115360428A - Ionic liquid modified electrolyte and preparation method and application thereof - Google Patents

Ionic liquid modified electrolyte and preparation method and application thereof Download PDF

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CN115360428A
CN115360428A CN202211044026.7A CN202211044026A CN115360428A CN 115360428 A CN115360428 A CN 115360428A CN 202211044026 A CN202211044026 A CN 202211044026A CN 115360428 A CN115360428 A CN 115360428A
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ionic liquid
lithium
stachydrine
electrolyte
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李宣
陈正件
刘凌雯
徐林
孔晶
陈晓欣
费玉清
杨岳
李江南
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Zhuhai Institute Of Advanced Technology Chinese Academy Of Sciences 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
    • H01M10/056—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
    • 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
    • H01M10/42—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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract

The invention belongs to the technical field of battery electrolyte, and discloses an ionic liquid modified electrolyte and a preparation method and application thereof. The ionic liquid modified electrolyte comprises a solvent and lithium salt, wherein the solvent comprises an organic solvent and stachydrine base ionic liquid, and the mass percent of the stachydrine base ionic liquid in the solvent is 1% -50%. According to the ionic liquid modified electrolyte provided by the invention, the stachydrine base ionic liquid is added into the traditional electrolyte, and the interaction of the ester bond in the stachydrine base ionic liquid and the carbonate electrolyte is utilized, so that the transference number of lithium ions can be increased, the charge-discharge capacity of the lithium iron phosphate electrode can be obviously increased, and after the lithium iron phosphate electrode is operated under different multiplying powers, especially when the lithium iron phosphate electrode is operated under a high multiplying power and enters a low multiplying power, the good charge-discharge capacity can still be maintained, and the circulation stability is strong.

Description

Ionic liquid modified electrolyte and preparation method and application thereof
Technical Field
The invention belongs to the technical field of battery electrolyte, and particularly relates to ionic liquid modified electrolyte and a preparation method and application thereof.
Background
The electrolyte plays an important role in the stable operation of the lithium ion battery. In recent years, with the increasing demand for high energy batteries, developers have attempted to expand the electrochemical window of the electrolyte to enable it to operate in lithium metal anodes with very low reduction potentials (LMA, -3.040V vs. standard hydrogen electrode) and cathodes with high oxidation potentials (> 4.5V vs Li/Li +). However, conventional electrolytes in lithium ion batteries are not suitable for Lithium Metal Batteries (LMB) because they lead to the growth of Li dendrites and the Coulombic Efficiency (CE) of the LMA is low. In the prior art, an electrolyte containing high-concentration lithium salt (4-6 mol/L) is researched, and the formation of lithium dendrite and the corrosion of a positive current collector are inhibited by adopting the synergistic effect of double anions, so that the cycle performance of the battery is improved.
In addition, the conventional carbonate solvent has high volatility and inflammability, presents a serious safety risk, and LiPF 6 The chemical nature is unstable, which makes the electrolyte highly sensitive to moisture and temperature variations. Even in combination with additives, the electrochemical window of the electrolyte can only be within 4.4V. The next generation of batteries requires higher energy density (higher voltage orCapacity) and wider operating temperatures, and must meet the requirements for smart phones, electric vehicles, smart grids and higher safety standards, etc., these shortcomings of conventional electrolytes have hindered the development of next generation batteries. Therefore, research on electrolytes, such as ionic liquids, polymer electrolytes, inorganic solid electrolytes, and salt-concentrated electrolytes, is increasingly important over conventional lithium ion electrolytes.
Therefore, it is highly desirable to provide an electrolyte solution that can significantly improve the charge and discharge capacity of a lithium iron phosphate electrode and maintain good charge and discharge capacity after the lithium iron phosphate electrode is operated at different multiplying factors.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides an ionic liquid modified electrolyte and a preparation method and application thereof. The ionic liquid modified electrolyte provided by the invention can obviously improve the charge and discharge capacity of the lithium iron phosphate electrode, and can still maintain good charge and discharge capacity after the lithium iron phosphate electrode is operated under different multiplying powers, particularly when the lithium iron phosphate electrode is operated under a high multiplying power and enters a low multiplying power.
The invention provides an ionic liquid modified electrolyte in a first aspect.
Specifically, the ionic liquid modified electrolyte comprises a solvent and lithium salt, wherein the solvent comprises an organic solvent and stachydrine base ionic liquid, the mass percent of the stachydrine base ionic liquid in the solvent is 1% -50%, and the cation structure of the stachydrine base ionic liquid is as shown in the formula (1):
Figure BDA0003819914770000021
in the formula (1), R 1 、R 2 、R 3 Represents a C1-C6 alkyl group.
Preferably, in formula (1), R 1 、R 2 、R 3 Are each independently selected from-CH 3 、-CH 2 CH 3 、-CH 2 CH 2 CH 3 、-CH 2 CH 2 CH 2 CH 3 、-CH 2 CH 2 CH 2 CH 2 CH 3 To (3) is provided.
Preferably, the anion of the stachydrine-based ionic liquid is selected from hexafluorophosphate (PF) 6 - ) Tetrafluoroborate (BF) 4 - ) Perchlorate (ClO) 4 - ) Bis (oxalato) borate (BOB) - ) Difluoro oxalato borate (DFOB) - ) Bis (fluorosulfonyl) imide (FSI) - ) Bis (trifluoromethyl) sulfonimide (TFSI) - ) At least one of (a).
Preferably, the stachydrine base ionic liquid is selected from the group consisting of lithium stachydrine butyl bistrifluoromethylsulfonyl imide (P) 1,1- 4 TFSI), stachydrine ethyl ester bis (trifluoromethyl) sulfonimide lithium (P) 1,1-2 TFSI), stachydrine propyl ester lithium bis (trifluoromethylsulfonyl) imide (P) 1,1-3 TFSI), stachydrine pentyl ester lithium bistrifluoromethylsulfonyl imide (P) 1,1-5 TFSI), stachydrine ethyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-2 FSI), stachydrine propyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-3 FSI), stachydrine butyl ester lithium bis (fluorosulfonyl) imide (P) 1,1- 4 FSI), stachydrine pentyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-5 FSI).
Further preferably, the stachydrine-based ionic liquid is selected from the group consisting of lithium stachydrine butyl bistrifluoromethylsulfonyl imide (P) 1,1-4 TFSI), stachydrine pentyl ester lithium bistrifluoromethylsulfonyl imide (P) 1,1-5 TFSI), stachydrine butyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-4 FSI), stachydrine pentyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-5 FSI).
More preferably, the stachydrine base ionic liquid is stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) 1,1- 4 TFSI)。
Preferably, the content of lithium salt in the ionic liquid modified electrolyte is 0.1-4.0mol/Kg; further preferably, the content of lithium salt in the ionic liquid modified electrolyte is 0.2-2.0mol/Kg; preferably, the content of the lithium salt in the ionic liquid modified electrolyte is 0.2-1.0mol/Kg.
Preferably, the stachydrine-based ionic liquid accounts for 5-30% of the solvent by mass percent; further preferably, the mass percentage of the stachydrine-based ionic liquid in the solvent is 5% -20%.
Preferably, the lithium salt is selected from at least one of lithium hexafluorophosphate, lithium tetrafluoroborate, lithium perchlorate, lithium bis (oxalate) borate, lithium difluoro (oxalate) borate, lithium bis (fluorosulfonyl) imide, and lithium bis (trifluoromethylsulfonyl) imide. The anion in the lithium salt may be the same as or different from the anion in the ionic liquid.
Preferably, the organic solvent accounts for 95-30% of the solvent by mass; further preferably, the organic solvent accounts for 70-95% of the solvent by mass.
Preferably, the organic solvent is at least one selected from the group consisting of carboxylic acid esters, carbonic acid esters, aromatic acid esters, lactones, sulfites and sulfoxides.
Preferably, the organic solvent is selected from at least one of methyl formate, methyl acetate, ethyl acetate, propyl acetate, ethyl propionate, ethyl butyrate, vinyl acetate, cyclobutyrolactone, methyl benzoate, ethylene carbonate, propylene carbonate, diethyl carbonate, dimethyl carbonate, ethyl methyl carbonate, vinylene carbonate, ethylene sulfite, propylene sulfite, butylene sulfite, dimethyl sulfite, diethyl sulfite, dimethyl sulfoxide, ethylmethyl sulfoxide, 1,3-sultone, 1,4-butyrolactone, and organic esters containing fluorine, sulfur and unsaturated bonds.
Preferably, the organic solvent is a carbonate; further preferably, the organic solvent is at least one selected from the group consisting of Ethylene Carbonate (EC), diethyl carbonate (DEC), ethyl Methyl Carbonate (EMC), propylene carbonate, dimethyl carbonate, vinylene carbonate.
Preferably, the ionic liquid modified electrolyte further comprises at least one of imidazole, pyrrolidine, pyridine, piperidine and amide ionic liquids. The ionic liquid can be mixed with the stachydrine ionic liquid in any proportion.
The invention provides a preparation method of an ionic liquid modified electrolyte.
Specifically, the preparation method of the ionic liquid modified electrolyte comprises the following steps:
and mixing an organic solvent, the stachydrine base ionic liquid and the lithium salt to obtain the ionic liquid modified electrolyte.
The invention provides application of an ionic liquid modified electrolyte in a third aspect.
A battery comprises the ionic liquid modified electrolyte.
A lithium battery comprises the ionic liquid modified electrolyte, a negative plate and a positive plate; the negative active substance on the negative plate is selected from at least one of metallic lithium, artificial graphite, natural graphite, mesocarbon microbeads, soft carbon, hard carbon, mesocarbon fibers, lithium titanate and metallic lithium alloy; the positive active material on the positive plate is lithium iron phosphate.
The invention adopts the stachydrine base ionic liquid to modify the traditional electrolyte, in particular to the carbonate electrolyte, and the molecular structure of the stachydrine base ionic liquid contains an ester bond which can interact with the carbonate electrolyte. The transference number of lithium ions can be improved by adding a small amount of stachydrine-based ionic liquid (the mass ratio is not more than 50%), because the stachydrine-based ionic liquid can change the traditional organic solvent (especially carbonate solvents) to form a solvation shell layer with the lithium ions, so that the thickness of the lithium ion shell layer is reduced, and the lithium ions are easier to solvate and desolvate. The stachydrine base ionic liquid modified electrolyte can also obviously improve the activity and the charge-discharge capacity of the lithium iron phosphate electrode, and can still keep good charge-discharge capacity and cycle stability after the lithium iron phosphate electrode runs under different multiplying powers, particularly when the lithium iron phosphate electrode runs under a high multiplying power and then enters a low multiplying power.
Compared with the prior art, the invention has the following beneficial effects:
according to the ionic liquid modified electrolyte provided by the invention, stachydrine base ionic liquid is added into the traditional electrolyte (especially carbonate electrolyte), and the interaction of the ester bond in the stachydrine base ionic liquid and the carbonate electrolyte is utilized, so that the transference number of lithium ions can be increased, the charge-discharge capacity of the lithium iron phosphate electrode is obviously increased, and after the lithium iron phosphate electrode is operated under different multiplying powers, especially when the lithium iron phosphate electrode is operated under a high multiplying power and enters a low multiplying power, the good charge-discharge capacity can still be maintained, and the circulation stability is strong.
Drawings
Fig. 1 is a graph comparing the charge and discharge capacities at different rates of the ferric lithium phosphate electrodes of examples 1-7.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-4 TFSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine butyl ester 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain a sample A1 of the ionic liquid modified electrolyte.
Sample A1 is used as electrolyte, a lithium piece is used as a battery cathode, lithium iron phosphate is used as a battery anode, and a half-cell is assembled to test the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is to divide the battery intoThe charge and discharge capacity at each rate was tested by cycling at 0.1C, 0.2C, 0.5C, 1.0C, 2.0C, 5.0C, respectively, and then at 0.1C. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode at a rate of 0.1C is improved by 21mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running at a high rate and then enters a low rate again, and is basically consistent with the first charge and discharge capacity.
Example 2
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine ethyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-2 TFSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine ethyl ester 1,1- 2 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain a sample A2 of the ionic liquid modified electrolyte.
And (3) testing the charge and discharge capacity of the lithium iron phosphate electrode by using the sample A2 as electrolyte, a lithium sheet as a battery cathode and lithium iron phosphate as a battery anode and assembling a half battery. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, then circulated under the multiplying power of 0.1C, and the charging under each multiplying power is testedAnd (4) discharge capacity. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 7mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 3
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine propyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-3 TFSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium bistrifluoromethylsulfonimide (P) as a stachydrine propyl ester 1,1- 3 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A3 of the ionic liquid modified electrolyte.
And (3) testing the charge and discharge capacity of the lithium iron phosphate electrode by using the sample A3 as electrolyte, a lithium sheet as a battery cathode and lithium iron phosphate as a battery anode and assembling a half battery. Specifically, the battery is cycled at the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then cycled at the multiplying power of 0.1C, and the charge and discharge capacity at each multiplying power is tested. Mixing a conventional electrolyte (a solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1And 1vol% of Vinylene Carbonate (VC) is added as an additive, and lithium salt is lithium hexafluorophosphate (LiPF) 6 ) 1.0 mol/Kg) was used as a blank control. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode at a rate of 0.1C is improved by 6mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running at a high rate and then enters a low rate again, and is basically consistent with the first charge and discharge capacity.
Example 4
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of lithium bistrifluoromethylsulfonyl imide (P) of stachydrine amyl ester 1,1-5 TFSI) and 95% by mass of an organic solvent, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) in a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine pentyl ester 1,1- 5 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain a sample A4 of the ionic liquid modified electrolyte.
Sample A4 is used as electrolyte, a lithium piece is used as a battery cathode, lithium iron phosphate is used as a battery anode, and the assembled half-cell is used for testing the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) as a blankAnd (4) a control group. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 12mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 5
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine ethyl ester lithium bis (fluorosulfonyl) imide (P) by mass 1,1-2 FSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium stachydrine ethyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-2 FSI) were mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A5 of the ionic liquid modified electrolyte.
And (3) testing the charge and discharge capacity of the lithium iron phosphate electrode by using the sample A5 as electrolyte, a lithium sheet as a battery cathode and lithium iron phosphate as a battery anode and assembling a half battery. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) Concentration of 1.0 mol/Kg) was used as a blank control. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test conditions, the ionic liquid provided by the invention is used for modifying the electrolyteThe charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 5mAh/g, the cycling stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 6
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine propyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-3 FSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium stachydrine propyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-3 FSI) were mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain a sample A6 of the ionic liquid modified electrolyte.
Sample A6 is used as electrolyte, a lithium piece is used as a battery cathode, lithium iron phosphate is used as a battery anode, and the assembled half-cell is used for testing the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 7mAh/g, the cycle stability of the battery is improved, and the battery enters a low-rate state again after running under a high multiplying powerAnd at the multiplying power, the lithium ion battery still has higher charge-discharge capacity which is basically consistent with the first charge-discharge capacity.
Example 7
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine butyl ester lithium bis (fluorosulfonyl) imide (P) by mass 1,1-4 FSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium stachydrine butyl ester bis (fluorosulfonyl) imide (P) 1,1-4 FSI) were mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain a sample A7 of the ionic liquid modified electrolyte.
And (3) testing the charge and discharge capacity of the lithium iron phosphate electrode by using the sample A7 as an electrolyte, a lithium sheet as a battery cathode and lithium iron phosphate as a battery anode and assembling a half battery. Specifically, the battery is cycled at the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then cycled at the multiplying power of 0.1C, and the charge and discharge capacity at each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. The results of the different magnification tests are shown in fig. 1. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 16mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 8
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 5 percent of stachydrine amyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-5 FSI) and 95% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 95wt% of organic solvent and 5wt% of lithium stachydrine pentyl ester lithium bis (fluorosulfonyl) imide (P) 1,1-5 FSI) were mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain a sample A8 of the ionic liquid modified electrolyte.
And (3) testing the charge and discharge capacity of the lithium iron phosphate electrode by using the sample A8 as an electrolyte, a lithium sheet as a battery cathode and lithium iron phosphate as a battery anode and assembling a half battery. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) The concentration of (1.0 mol/Kg) was a blank control group. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 15mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 9
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 10 percent of stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-4 TFSI) and 90 percent of organic solvent by massThe organic solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) in a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 90wt% of organic solvent and 10wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine butyl ester 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A9 of the ionic liquid modified electrolyte.
And (3) testing the charge and discharge capacity of the lithium iron phosphate electrode by using the sample A9 as electrolyte, a lithium sheet as a battery cathode and lithium iron phosphate as a battery anode and assembling a half battery. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 10mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 10
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 20 percent of lithium bistrifluoromethylsulfonyl imide (P) by mass 1,1-4 TFSI) and 80% by mass of an organic solvent, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) in a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) Has a concentration of 1.0mol/Kg。
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 90wt% of organic solvent and 10wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine butyl ester 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A10 of the ionic liquid modified electrolyte.
Sample A10 is used as electrolyte, a lithium piece is used as a battery cathode, lithium iron phosphate is used as a battery anode, and a half-cell is assembled to test the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 12mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 11
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 30 percent of stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-4 TFSI) and 70% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
in the roomAt room temperature, 90wt% of organic solvent and 10wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine butyl ester 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A11 of the ionic liquid modified electrolyte.
Sample A11 is used as electrolyte, a lithium piece is used as a battery cathode, lithium iron phosphate is used as a battery anode, and the assembled half-cell is used for testing the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 9mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 12
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 40 percent of stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-4 TFSI) and 60% by mass of an organic solvent, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) in a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
90wt% of organic solvent and 10wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate was added(LiPF 6 ) And dissolving and mixing to obtain a sample A12 of the ionic liquid modified electrolyte.
The sample A12 is used as electrolyte, a lithium plate is used as a battery cathode, lithium iron phosphate is used as a battery anode, and a half battery is assembled to test the charge-discharge capacity of the lithium iron phosphate. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 6mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Example 13
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 50 percent of stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-4 TFSI) and 50% of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 90wt% of organic solvent and 10wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine butyl ester 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A13 of the ionic liquid modified electrolyte.
Sample A13 was used as an electrolyte, and a lithium plate was used as a lithium plateAnd the battery cathode takes the lithium iron phosphate as the battery anode, and the half battery is assembled to test the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is that the battery is respectively circulated under the multiplying power of 0.1C, 0.2C, 0.5C, 1.0C, 2.0C and 5.0C in sequence, and then circulated under the multiplying power of 0.1C, and the charge and discharge capacity under each multiplying power is tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) Concentration of 1.0 mol/Kg) was used as a blank control. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is improved by 2mAh/g, the cycle stability of the battery is improved, and the battery still has higher charge and discharge capacity when running under high multiplying power and then enters low multiplying power again, and is basically consistent with the first charge and discharge capacity.
Comparative example 1
An ionic liquid modified electrolyte is prepared from solvent and lithium hexafluorophosphate (LiPF) 6 ) The solvent is 40 percent of stachydrine butyl ester bis (trifluoromethyl) sulfonyl imide lithium (P) by mass 1,1-4 TFSI) and 60 percent of organic solvent by mass, wherein the organic solvent is formed by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1. Lithium hexafluorophosphate (LiPF) 6 ) The concentration of (b) is 1.0mol/Kg.
A preparation method of an ionic liquid modified electrolyte comprises the following steps:
at room temperature, 90wt% of organic solvent and 10wt% of lithium bistrifluoromethylsulfonimide (P) as stachydrine butyl ester 1,1- 4 TFSI) was mixed well and then lithium hexafluorophosphate (LiPF) was added 6 ) And dissolving and mixing to obtain sample A14 of the ionic liquid modified electrolyte.
The sample A14 is used as an electrolyte, a lithium plate is used as a battery cathode, lithium iron phosphate is used as a battery anode, and a half battery is assembled to test the charge-discharge capacity of the lithium iron phosphate electrode. The specific test is that the battery is respectively and sequentially at 0.1C and 0Cycling at a rate of 2C, 0.5C, 1.0C, 2.0C, 5.0C, and then cycling at a rate of 0.1C, the charge and discharge capacity at each rate was tested. The electrolyte is prepared by mixing a traditional electrolyte (a solvent is prepared by mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) according to a volume ratio of 1 6 ) 1.0 mol/Kg) was used as a blank control. Compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode under the multiplying power of 0.1C is reduced by 10mAh/g, and the battery cannot keep good circulation stability when running under the high multiplying power and then entering the low multiplying power again.
Sample A1 (i.e., P) from the ionic liquid modified electrolyte of FIG. 1 was analyzed 1,1-4 TFSI), the charge and discharge capacities at different charge and discharge rates are listed in the table, and the specific case is shown in table 1.
TABLE 1
Figure BDA0003819914770000131
Figure BDA0003819914770000141
As can be seen from table 1, compared with a blank control group, under the same assembly test condition, after the ionic liquid modified electrolyte provided by the invention is used, the charge and discharge capacity of the lithium iron phosphate electrode at a rate of 0.1-2.0C is improved by 16-21mAh/g, and when the battery enters a low rate (0.1C) again after running at a high rate (5C), the battery still has a higher charge and discharge capacity, which is basically consistent with the first charge and discharge capacity.

Claims (10)

1. The ionic liquid modified electrolyte is characterized by comprising a solvent and lithium salt, wherein the solvent comprises an organic solvent and a stachydrine base ionic liquid, the mass percent of the stachydrine base ionic liquid in the solvent is 1% -50%, and the cation structure of the stachydrine base ionic liquid is as shown in the formula (1):
Figure FDA0003819914760000011
in the formula (1), R 1 、R 2 、R 3 Represents a C1-C6 alkyl group.
2. The ionic liquid modified electrolyte as claimed in claim 1, wherein R in the formula (1) 1 、R 2 、R 3 Are each independently selected from-CH 3 、-CH 2 CH 3 、-CH 2 CH 2 CH 3 、-CH 2 CH 2 CH 2 CH 3 、-CH 2 CH 2 CH 2 CH 2 CH 3 One kind of (1).
3. The ionic liquid modified electrolyte as claimed in claim 1, wherein the anion of the stachydrine-based ionic liquid is selected from one of hexafluorophosphate, tetrafluoroborate, perchlorate, bisoxalato borate, difluorooxalato borate, bisfluorosulfonylimide, and bistrifluoromethylsulfonyl imide.
4. The ionic liquid modified electrolyte as claimed in any one of claims 1 to 3, wherein the stachydrine base ionic liquid is selected from at least one of lithium stachydrine butyl ester bistrifluoromethylsulfonyl imide, lithium stachydrine ethyl ester bistrifluoromethylsulfonyl imide, lithium stachydrine propyl ester bistrifluoromethylsulfonyl imide, lithium stachydrine pentyl ester bistrifluoromethylsulfonyl imide, lithium stachydrine ethyl ester bistluorosulfonylide propyl ester bistrifluorosulfonimide, lithium stachydrine butyl ester bistluorosulfonimide and lithium stachydrine pentyl ester bistrifluorosulfonimide.
5. The ionic liquid modified electrolyte of claim 4, wherein the lithium salt is present in the ionic liquid modified electrolyte in an amount of 0.1 to 4.0mol/Kg.
6. The ionic liquid modified electrolyte as claimed in claim 4, wherein the stachydrine-based ionic liquid accounts for 5-30% of the solvent by mass.
7. The ionic liquid modified electrolyte as claimed in claim 5 or 6, wherein the organic solvent is at least one selected from the group consisting of carboxylic acid esters, carbonic acid esters, aromatic acid esters, lactones, sulfites and sulfoxides; preferably, the organic solvent is a carbonate.
8. The method for preparing an ionic liquid modified electrolyte according to any one of claims 1 to 7, wherein the ionic liquid modified electrolyte is prepared by mixing an organic solvent, a stachydrine-based ionic liquid, and a lithium salt.
9. A lithium battery comprising the ionic liquid modified electrolyte of any one of claims 1 to 7, a negative electrode sheet, and a positive electrode sheet.
10. The lithium battery of claim 9, wherein the negative active material on the negative electrode sheet is selected from at least one of metallic lithium, artificial graphite, natural graphite, mesocarbon microbeads, soft carbon, hard carbon, mesocarbon fibers, lithium titanate, and metallic lithium alloys; the positive active material on the positive plate is lithium iron phosphate.
CN202211044026.7A 2022-08-29 2022-08-29 Ionic liquid modified electrolyte and preparation method and application thereof Pending CN115360428A (en)

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