CN111029654A - Electrolyte and lithium ion battery using same - Google Patents
Electrolyte and lithium ion battery using same Download PDFInfo
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- CN111029654A CN111029654A CN201911325709.8A CN201911325709A CN111029654A CN 111029654 A CN111029654 A CN 111029654A CN 201911325709 A CN201911325709 A CN 201911325709A CN 111029654 A CN111029654 A CN 111029654A
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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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an electrolyte, which comprises lithium salt, an additive and an organic solvent, wherein the additive comprises the following components in percentage by mass in the electrolyte: 0.1 to 5 percent of sulfonic pyridine compound and 0.1 to 10 percent of other additives. The sulfonic acid pyridine compound is added into the lithium ion battery electrolyte, and the formed SEI film has good permeability to lithium ions due to the addition of the sulfonic acid pyridine compound, so that the increase of impedance caused by film formation can be reduced, the conductivity of the electrolyte in the lithium ion battery is effectively improved, and the cycle performance of the lithium ion battery is improved; meanwhile, the pyridine sulfonate compound can form an SEI film of lithium sulfonate salts and has good high-temperature tolerance, so that the contact decomposition of the electrolyte and the surface of an electrode under a high-temperature condition can be effectively inhibited, and the high-temperature effect of the battery is improved.
Description
Technical Field
The invention relates to the field of batteries, in particular to an electrolyte and a lithium ion battery using the same.
Background
In recent years, lithium ion batteries have attracted much attention because they have higher energy densities than other conventional ion batteries. With the rapid development of the application field, people put higher requirements on the energy density, rate capability, applicable temperature, cycle life and safety of the lithium ion battery
At present, the problems of low oxidation potential, poor wettability with anode materials and the like of the conventional carbonate-based high-voltage electrolyte exist, and the practical application of the high-voltage lithium ion battery is severely restricted. The lithium salt is a provider of lithium ions in the electrolyte and is an important component of the electrolyte of the lithium ion battery, but LiPF is the most commonly used lithium salt6The thermal stability in a non-aqueous solvent is poor, and the stability of a battery system is seriously influenced. LiTFSI has high solubility and conductivity, but severely corrodes the Al current collector at voltages above 3.7V. The high energy density of the battery requires that the battery must have a higher voltage, and at the same time, the complex working environment also puts higher demands on the performance of the lithium ion battery at high and low temperatures. The traditional solution is to add high-temperature or low-temperature additives into the electrolyte aiming at different working environments, but the lithium ion battery used in the field of power batteries cannot work only in the high-temperature or low-temperature environment, the future lithium ion battery must have the capability of normally working at-20 ℃ to 60 ℃ and a wider temperature range, and if the high-temperature and low-temperature additives are added into the electrolyte at the same time, other reactions can occur to cause the reduction of the battery performance.
Therefore, the development of new high voltage electrolyte systems to provide a safe, stable environment is one of the keys to the development of lithium ion batteries.
For example, chinese patent publication No. CN106099183A discloses an electrolyte containing pyridinium propanesulfonate, which is mainly prepared from the following components: electrolyte lithium salt, propane sulfonic acid pyridine salt, other additives and a non-aqueous organic solvent, wherein: the concentration of the electrolyte lithium salt in the electrolyte is 0.5-2 mol/L; the mass percentage of the propane sulfonic pyridine salt in the electrolyte is 0.1-10%; the mass percentage of the other additives in the electrolyte is 0.5-10%. The electrolyte containing the propane sulfonic acid pyridinium provided by the invention has stable performance and does not generate substances harmful to human bodies. The electrolyte has larger influence on the cycle performance and the high-temperature performance of the battery, and compared with other common additives, the propane sulfonic acid pyridinium salt serving as the additive can improve the high-temperature storage performance of the battery. However, the molecular formula of the propane sulfonic acid pyridinium is large, and when the propane sulfonic acid pyridinium is used as an electrolyte additive, a formed SEI film has high impedance and is not beneficial to the low-temperature cycle performance of a lithium ion battery.
Disclosure of Invention
In view of the above, the present invention provides an electrolyte capable of stably operating under conditions of high voltage and large temperature variation of operating environment, and a lithium ion battery using the electrolyte. The sulfonic pyridine compound is added into the electrolyte, so that the permeability of an SEI film to lithium ions is improved, the impedance can be effectively reduced, and the low-temperature performance of the battery is improved; meanwhile, the addition of the pyridine sulfonate compound is beneficial to forming a high-temperature-resistant SEI film, the film can effectively prevent the contact between the electrolyte and an electrode at high temperature, inhibit the decomposition of the electrolyte and improve the high-temperature performance of the battery.
In order to achieve the purpose, the invention adopts the technical scheme that: the electrolyte comprises a lithium salt, an additive and an organic solvent, wherein the additive comprises the following components in percentage by mass in the electrolyte:
sulfonic acid pyridine compound 0.1-5%
1 to 20 percent of other additives
As a preferred embodiment of the present invention, the structural formula of the sulfonic acid pyridine compound is preferably as shown in the following formula:
wherein R is1Represents a saturated or unsaturated alkyl group having 1 to 10 carbon atoms, a halogenated alkyl group, an aromatic group, a cyano group, an alkoxy group.
The sulfonic pyridine compound is more preferably at least one of trifluoromethanesulfonic pyridine, nitrile-sulfonic pyridine, tert-butyl-sulfonic pyridine, fluorosulfonic pyridine, phenylsulfonic pyridine and ethylsulfonic pyridine, and the structural formula of the sulfonic pyridine compound is as follows:
wherein the compound shown in the formula (1) is pyridine trifluoromethanesulfonate; the compound shown in the formula (2) is nitrile sulfonic pyridine; the compound shown in the formula (3) is tert-butyl pyridine sulfonate; the compound shown in the formula (4) is fluorosulfonic acid pyridine; the compound shown in the formula (5) is pyridine phenylsulfonate; the compound shown in the formula (6) is pyridine ethylsulfonate.
In a preferred embodiment of the present invention, the lithium salt is preferably LiPF6、LiBF4、LiClO4、LiBOB、LiODFB、LiAsF6、LiN(SO2CF3)2、LiN(SO2F)2One or more of (a).
As a preferred embodiment of the present invention, the concentration of the lithium salt in the lithium ion battery electrolyte is preferably 0.5 to 2 mol/L.
As a preferred embodiment of the present invention, the other additives are preferably fluoroethylene carbonate (FEC), 1, 3-Propane Sultone (PS), ethylene carbonate (VEC), Vinylene Carbonate (VC), Propylene Carbonate (PC), lithium difluorophosphate (LiPO)2F2) One or more of tris (trimethylsilyl) borate (TMSB), Succinonitrile (SN), Adiponitrile (ADN). More preferably, the other additive is a mixture of vinylene carbonate, fluoroethylene carbonate, 1, 3-propane sultone and adiponitrile.
The organic solvent in the invention can adopt chain carbonate, cyclic carbonate and carboxylic ester, wherein the chain carbonate is selected from one or more of dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC) and dipropyl carbonate (DPC); the cyclic carbonate is selected from one or more of Ethylene Carbonate (EC), Vinylene Carbonate (VC) and Propylene Carbonate (PC); the carboxylic acid ester is selected from one or more of Ethyl Acetate (EA), Ethyl Propionate (EP), Methyl Acetate (MA), propyl acetate (PE), Methyl Propionate (MP), Methyl Butyrate (MB) and Ethyl Butyrate (EB). As a preferred embodiment of the present invention, the organic solvent is preferably one or more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, dipropyl carbonate, ethylene carbonate, vinylene carbonate, propylene carbonate, ethyl acetate, ethyl propionate, methyl acetate, propyl acetate, methyl propionate, methyl butyrate, and ethyl butyrate. The organic solvent is more preferably a mixture of ethylene carbonate, propylene carbonate, diethyl carbonate and ethyl propionate.
The invention also provides a lithium ion battery, which contains the electrolyte.
Preferably, the method for preparing the lithium ion battery comprises the step of injecting the electrolyte of the invention into a fully dried 4.45V LiCoO in a glove box containing inert gas2The graphite soft package battery is prepared by the working procedures of laying aside at 45 ℃, forming by a high-temperature clamp, sealing for the second time and the like.
Compared with the prior art, the invention has the advantages that:
the electrolyte contains the sulfonic pyridine compound, so that the impedance of the battery can be effectively reduced, and the working performance of the battery under the low-temperature condition is improved. Compared with the traditional lithium ion secondary battery without the sulfonic pyridine compound, the electrolyte of the invention is added with the sulfonic pyridine compound, and the addition of the sulfonic pyridine compound improves the permeability of an SEI film to lithium ions, so the impedance is low and the cycle performance is good; meanwhile, the pyridine sulfonate compound can form an SEI film of lithium sulfonate salts and has good high-temperature tolerance, so that the contact decomposition of the electrolyte and the surface of an electrode under a high-temperature condition can be effectively inhibited, and the high-temperature effect of the battery is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
Example 1
The electrolyte is prepared by the following method: in a glove box, Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC) and Ethyl Propionate (EP) were mixed in a weight ratio of 25: 10: 30: 35 to obtain a mixed solvent, and then adding lithium hexafluorophosphate to the mixed solvent to dissolve the lithium hexafluorophosphate to prepare an electrolyte solution having a lithium hexafluorophosphate concentration of 1.2M. Then, propylene carbonate (VC), fluoroethylene carbonate (FEC), 1, 3-propane sultone (1,3-PS), and Adiponitrile (ADN) were added to the electrolyte; and adding pyridine trifluoromethanesulfonate into the solution, and uniformly stirring to obtain the electrolyte containing pyridine trifluoromethanesulfonate. The mass percent of the propylene carbonate (VC) in the electrolyte is 0.5%, the mass percent of the fluoroethylene carbonate (FEC) in the electrolyte is 6.0%, the mass percent of the 1, 3-propane sultone (1,3-PS) in the electrolyte is 2.5%, the mass percent of the Adiponitrile (ADN) in the electrolyte is 2%, and the mass percent of the trifluoromethane pyridine sulfonate in the electrolyte is 0.5%. The electrolyte formulation is shown in table 1.
Examples 2 to 24
Examples 2 to 24 are also specific examples of the preparation of the electrolyte containing the pyridine sulfonate compound, and the parameters and the preparation method are the same as those of example 1 except for the parameters shown in table 1. The electrolyte formulation is shown in table 1.
Comparative example 1
The lithium ion battery electrolyte is prepared by the following method: in a glove box, Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC) and Ethyl Propionate (EP) were mixed in a weight ratio of 25: 10: 30: 35 to obtain a mixed solvent, and then adding lithium hexafluorophosphate to the mixed solvent to dissolve the lithium hexafluorophosphate to prepare an electrolyte solution having a lithium hexafluorophosphate concentration of 1.2M. And then adding propylene carbonate (VC), fluoroethylene carbonate (FEC), 1, 3-propane sultone (1,3-PS) and Adiponitrile (ADN) into the electrolyte, and uniformly stirring to obtain the lithium ion battery electrolyte. Wherein the mass percent of the propylene carbonate (VC) in the electrolyte is 0.5%, the mass percent of the fluoroethylene carbonate (FEC) in the electrolyte is 6.0%, the mass percent of the 1, 3-propane sultone (1,3-PS) in the electrolyte is 2.5%, and the mass percent of the Adiponitrile (ADN) in the electrolyte is 2%. The electrolyte formulation is shown in table 1.
Comparative example 2
Comparative example 2 the preparation is as in comparative example 1, the formulation is detailed in table 1, except that: comparative example 2 lithium difluorophosphate (LiPO) was also added to the electrolyte in an amount of 1% by mass2F2)。
Comparative example 3
Comparative example 3 the preparation is as in comparative example 1, the formulation is detailed in table 1, except that: comparative example 3 tris (trimethylsilyl) phosphate (TMSP) was also added to the electrolyte at 1% by mass.
Comparative example 4
Comparative example 4 was prepared as in comparative example 1, with the formulation detailed in table 1, except that: comparative example 4 Methylene Methanedisulfonate (MMDS) was further added to the electrolyte in an amount of 1% by mass.
TABLE 1 electrolyte formulations for the examples and comparative examples
Note: the concentration of lithium salt is the molar concentration in the electrolyte;
the contents of the additive I and the additive II are the mass percentage contents in the electrolyte;
the proportion of each component in the solvent is mass ratio.
Lithium ion battery performance testing
The electrolyte prepared in each example and comparative example was injected into fully dried 4.45V LiCoO2In the graphite soft package battery, after the working procedures of laying aside at 45 ℃, forming by a high-temperature clamp, sealing secondarily and the like, the lithium ion battery is obtained, and the battery performance test is carried out, and the result is shown in table 2. Wherein:
1. normal temperature cycle performance
Under the condition of normal temperature (25 ℃), the lithium ion battery is charged to 4.45V under the constant current and the constant voltage of 1C, and then is discharged to 3.0V under the constant current of 1C. After 500 cycles of charge and discharge, capacity retention rate after 500 cycles was calculated:
2. high temperature cycle performance
Under the condition of high temperature (45 ℃), the lithium ion battery is charged to 4.45V under the constant current and constant voltage of 1C, and then is discharged to 3.0V under the constant current of 1C. After 300 cycles of charge and discharge, the capacity retention rate after the 300 th cycle was calculated as:
3. high temperature storage Properties
The lithium ion battery was subjected to primary 1C/1C charging and discharging (discharge capacity is designated DC) at room temperature (25 ℃ C.)0) Then charging the battery to 4.45V under the condition of 1C constant current and constant voltage; the lithium ion battery is stored in a high-temperature box at 60 ℃ for 1 month, and after being taken out, 1C discharge (the discharge capacity is recorded as DC) is carried out at normal temperature1) (ii) a Then, 1C/1C charging and discharging (discharge capacity is designated as DC) were carried out under ambient conditions2) Calculating the capacity retention rate and the capacity recovery rate of the lithium ion battery by using the following formulas:
4. low temperature cycle performance
Under the condition of low temperature (10 ℃), the lithium ion battery is charged to 4.45V under the constant current and constant voltage of 1C, and then is discharged to 3.0V under the constant current of 1C. After 50 cycles of charge and discharge, the capacity retention rate after the 50 th cycle was calculated as:
the cell performance results for each of the above specific examples are shown in table 2:
table 2 results of performance test of lithium ion batteries of comparative examples and examples
From the data from the above tests, it can be seen that the electrolyte containing pyridine sulfonate additive was used for 4.45V LiCoO2When the graphite soft package battery is used, the high and low temperature performance and the cycle performance of the battery can be obviously improved. This is because the addition of the pyridine sulfonate compound can form a dense SEI film on the surface of the electrode, which is oxidized preferentially to Li, by oxidizing the electrolyte solution+The permeability of the film is good, the impedance can be effectively reduced, the impedance of an SEI film formed by VC, 1,3-PS is large, and the difference of the impedances is more obvious particularly in a low-temperature environment; meanwhile, the pyridine sulfonate additive can form an SEI film of lithium sulfonate salts and has good high-temperature tolerance, so that the contact decomposition of the electrolyte and the surface of an electrode under a high-temperature condition can be effectively inhibited, and the high-temperature effect of the battery is improved. The comparative examples show that when the same additive is added in different amounts, about 1% of the pyridine sulfonate additive is added into the electrolyte to have the most significant effect on improving the battery performance, because when the additive is used in a small amount, the additive is not sufficient to show excellent performance, but when the additive is added in an excessively high amount, the formed SEI film increases the impedance to a different extent, affects the cycle performance, and particularly has a more significant effect on the low-temperature cycle performance. Meanwhile, by comparing the examples with comparative examples 2, 3 and 4, it can be found that lithium difluorophosphate (LiPO)2F2) And tris (trimethylsilyl) phosphate (TMSP) only to electricityThe low-temperature performance of the battery is improved, the Methylene Methanedisulfonate (MMDS) only improves the high-temperature performance of the battery, and the sulfonic pyridine compound improves the performance of the battery more comprehensively and is more favorable for being used as an additive in electrolyte.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The electrolyte comprises a lithium salt, an additive and an organic solvent, and is characterized in that the additive comprises the following components in percentage by mass in the electrolyte:
sulfonic acid pyridine compound 0.1-5%
1 to 20 percent of other additives
2. The electrolyte of claim 1, wherein the pyridine sulfonate compound has the formula:
wherein R is1Represents a saturated or unsaturated alkyl group having 1 to 10 carbon atoms, a halogenated alkyl group, an aromatic group, a cyano group, an alkoxy group.
3. The electrolyte of claim 2, wherein the pyridine sulfonate compound is at least one selected from the group consisting of pyridine trifluoromethanesulfonate, pyridine nitrile sulfonate, pyridine tert-butyl sulfonate, pyridine fluorosulfonate, pyridine phenylsulfonate, and pyridine ethylsulfonate.
4. The electrolyte of claim 1, wherein the lithium salt is selected from LiPF6、LiBF4、LiClO4、LiBOB、LiODFB、LiAsF6、LiN(SO2CF3)2、LiN(SO2F)2One or more of (a).
5. The electrolyte of claim 1, wherein the other additives are one or more of fluoroethylene carbonate, 1, 3-propane sultone, ethylene carbonate, vinylene carbonate, propylene carbonate, lithium difluorophosphate, tris (trimethylsilyl) borate, succinonitrile, adiponitrile.
6. The electrolyte of claim 5, wherein the other additive is a mixture of vinylene carbonate, fluoroethylene carbonate, 1, 3-propane sultone, and adiponitrile.
7. The electrolyte of claim 1, wherein the organic solvent is one or more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, dipropyl carbonate, ethylene carbonate, vinylene carbonate, propylene carbonate, ethyl acetate, ethyl propionate, methyl acetate, propyl acetate, methyl propionate, methyl butyrate, and ethyl butyrate.
8. The electrolyte of claim 7, wherein the organic solvent is a mixture of ethylene carbonate, propylene carbonate, diethyl carbonate, and ethyl propionate.
9. The electrolyte of claim 1, wherein the concentration of the lithium salt in the lithium ion battery electrolyte is 0.5-2 mol/L.
10. A lithium ion battery comprising the electrolyte of any one of claims 1 to 9.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111816921A (en) * | 2020-08-31 | 2020-10-23 | 珠海冠宇电池股份有限公司 | Electrolyte additive, electrolyte and battery |
| CN111834665A (en) * | 2020-06-24 | 2020-10-27 | 东莞市杉杉电池材料有限公司 | High-nickel ternary lithium ion battery electrolyte and lithium ion battery |
| CN111883834A (en) * | 2020-07-24 | 2020-11-03 | 香河昆仑化学制品有限公司 | Non-aqueous lithium ion battery electrolyte additive, electrolyte containing non-aqueous lithium ion battery electrolyte additive and lithium ion battery |
| CN112054241A (en) * | 2020-10-15 | 2020-12-08 | 广州天赐高新材料股份有限公司 | Fluorine-containing sulfonate electrolyte additive, electrolyte containing additive and lithium ion battery |
| CN113851718A (en) * | 2021-10-15 | 2021-12-28 | 大连中比动力电池有限公司 | Additive for electrolyte capable of improving low-temperature performance of lithium battery and electrolyte |
| CN114024027A (en) * | 2021-10-29 | 2022-02-08 | 湖南法恩莱特新能源科技有限公司 | High-concentration electrolyte and preparation method and application thereof |
| WO2022197094A1 (en) * | 2021-03-16 | 2022-09-22 | 주식회사 엘지에너지솔루션 | Non-aqueous electrolyte for lithium secondary battery and lithium secondary battery comprising same |
| CN114024027B (en) * | 2021-10-29 | 2024-04-19 | 湖南法恩莱特新能源科技有限公司 | High-concentration electrolyte and preparation method and application thereof |
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| CN112054241B (en) * | 2020-10-15 | 2022-06-21 | 广州天赐高新材料股份有限公司 | Fluorine-containing sulfonate electrolyte additive, electrolyte containing additive and lithium ion battery |
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| CN113851718A (en) * | 2021-10-15 | 2021-12-28 | 大连中比动力电池有限公司 | Additive for electrolyte capable of improving low-temperature performance of lithium battery and electrolyte |
| CN114024027A (en) * | 2021-10-29 | 2022-02-08 | 湖南法恩莱特新能源科技有限公司 | High-concentration electrolyte and preparation method and application thereof |
| CN114024027B (en) * | 2021-10-29 | 2024-04-19 | 湖南法恩莱特新能源科技有限公司 | High-concentration electrolyte and preparation method and application thereof |
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