CN109524714B - Lithium ion battery electrolyte and lithium ion battery - Google Patents
Lithium ion battery electrolyte and lithium ion battery Download PDFInfo
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- CN109524714B CN109524714B CN201811318376.1A CN201811318376A CN109524714B CN 109524714 B CN109524714 B CN 109524714B CN 201811318376 A CN201811318376 A CN 201811318376A CN 109524714 B CN109524714 B CN 109524714B
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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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- 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
In order to overcome the problems of insufficient cycle performance and thermal stability of the existing lithium ion battery, the invention provides a lithium ion battery electrolyte, which comprises a solvent, lithium salt and the following additives:
2-dicyanovinyl-4-vinyl-1, 3-dioxolane and
Description
Technical Field
The invention belongs to the technical field of secondary batteries, and particularly relates to a lithium ion battery electrolyte and a lithium ion battery.
Background
Lithium ion batteries have the advantages of high specific energy, long cycle life, low self-discharge, and the like, and are widely used in consumer electronics products and energy storage and power batteries. With the wide application of lithium ion batteries, the cycle life of the lithium ion battery becomes an important index of the lithium ion battery, and in addition, the lithium ion battery shows an unstable phenomenon after cycling, for example, the thermal stability of the lithium ion battery after cycling becomes worse, and in order to ensure the safety of use, the cycle performance of the lithium ion battery is improved, and at the same time, the thermal stability of the lithium ion battery after cycling needs to be improved. It follows that the safety performance of lithium ion batteries is also of particular importance.
The thermal stability of the lithium ion battery after circulation is influenced by a plurality of factors, wherein the electrolyte, as an important component of the lithium ion battery, has a great influence on the thermal stability performance after circulation.
Therefore, there is a need for an electrolyte with excellent performance to improve the cycle performance of a lithium ion battery and also improve the thermal stability of the lithium ion battery.
Disclosure of Invention
The invention provides a lithium ion battery electrolyte and a lithium ion battery, aiming at the problems of insufficient cycle performance and thermal stability of the existing lithium ion battery.
The technical scheme adopted by the invention for solving the technical problems is as follows:
in one aspect, an embodiment of the present invention provides an electrolyte for a lithium ion battery, including a solvent, a lithium salt, and the following additives:
2-dicyanovinyl-4-vinyl-1, 3-dioxolane and
n, N-dimethyl-m-phenylenediamine;
the content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte is less than or equal to 10% by mass, and the content of the N, N-dimethyl-m-phenylenediamine in the electrolyte is less than or equal to 5% by mass.
The electrolyte of the lithium ion battery provided by the invention is added with 2-dicyano vinyl-4-vinyl-1, 3-dioxolane and N, N-dimethyl m-phenylenediamine as additives, and the inventor finds that the combination of 2-dicyano vinyl-4-vinyl-1, 3-dioxolane or N, N-dimethyl m-phenylenediamine has obvious synergistic effect on improving the cycle performance and the thermal stability of the lithium ion battery compared with the single addition of 2-dicyano vinyl-4-vinyl-1, 3-dioxolane or N, N-dimethyl m-phenylenediamine in the electrolyte, passive films are generated on both the anode and the cathode, and the stability of the passive films under extreme conditions is improved.
Optionally, the mass percentage content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte is 0.05-10%.
Optionally, the content of the N, N-dimethyl m-phenylenediamine in the electrolyte is 0.01-5% by mass.
Optionally, the concentration of the lithium salt in the electrolyte is 0.5M to 2M.
Optionally, the lithium salt includes one or more of an organic lithium salt and an inorganic lithium salt.
Optionally, the lithium salt is selected from lithium salts containing fluorine.
Optionally, the lithium salt is selected from one or more of hexafluorophosphate, hexafluoroarsenate, perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, and lithium tris (trifluoromethylsulfonyl) methide.
Optionally, the solvent is two or more selected from ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, methyl formate, ethyl propionate, propyl propionate, methyl butyrate and tetrahydrofuran.
Optionally, the electrolyte consists of a solvent, a lithium salt, 2-dicyanovinyl-4-vinyl-1, 3-dioxolane and N, N-dimethyl m-phenylenediamine.
On the other hand, the embodiment of the invention also provides a lithium ion battery, which comprises a positive plate, a negative plate, a diaphragm and the electrolyte.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
One embodiment of the invention discloses a lithium ion battery electrolyte, which comprises a solvent, lithium salt and the following additives:
2-dicyanovinyl-4-vinyl-1, 3-dioxolane and
n, N-dimethyl-m-phenylenediamine;
the content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte is less than or equal to 10% by mass, and the content of the N, N-dimethyl-m-phenylenediamine in the electrolyte is less than or equal to 5% by mass.
The inventor finds that the combination of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane or the N, N-dimethyl m-phenylenediamine has obvious synergistic effect on improving the cycle performance and the thermal stability of the lithium ion battery, and passivation films are generated on both the positive electrode and the negative electrode and the stability of the passivation film is improved under extreme conditions compared with the single addition of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane or the N, N-dimethyl m-phenylenediamine in the electrolyte.
The introduction of the cyano group in the 2-dicyano vinyl-4-vinyl-1, 3-dioxolane can effectively complex metal ions in a system, further stabilize the system and improve high-temperature circulation and thermal shock resistance after circulation.
In some embodiments, the content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte is 0.05 to 10% by mass, and preferably, the content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte is 0.1 to 5% by mass.
Specifically, the mass percentage content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte can be 0.1%, 0.2%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%.
In some embodiments, the content of the N, N-dimethyl-m-phenylenediamine in the electrolyte is 0.01 to 5% by mass, and preferably, the content of the N, N-dimethyl-m-phenylenediamine in the electrolyte is 0.1 to 3% by mass.
Specifically, the content of the N, N-dimethyl-m-phenylenediamine in the electrolyte solution may be 0.1%, 0.2%, 0.5%, 1%, 1.5%, 2%, 2.5%, 3% by mass.
When the content ratio of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane to the 3, 4-ethylenedioxythiophene is within the above range, the electrolyte circulation performance and the thermal stability improvement effect are optimal.
The amount of the lithium salt may vary over a wide range, and in some embodiments, the concentration of the lithium salt in the electrolyte is 0.5M to 2M. When the concentration of the lithium salt is too low, the conductivity of the electrolyte is low, and the multiplying power and the cycle performance of the whole battery system can be influenced; when the concentration of the lithium salt is too high, the viscosity of the electrolyte is too high, which is also not beneficial to the improvement of the rate of the whole battery system. In a more preferred embodiment, the lithium salt concentration is 0.9M to 1.3M.
In some embodiments, the lithium salt includes one or more of an organic lithium salt and an inorganic lithium salt.
For example: LiPF6，LiBF4，LiSbF6，LiAsF6，LiTaF6，LiAlCl4，Li2B10Cl10，Li2B10F10，LiClO4，LiCF3SO3Salts of lithium chelated orthoborates and chelated orthophosphates, e.g. lithium bis (oxalato) borate [ LiB (C)2O4)2]Lithium dimalonate borate [ LiB (O)2CCH2CO2)2]Lithium bis (difluoromalonate) borate [ LiB (O)2CCF2CO2)2](malonic acid oxalic acid) lithium borate [ LiB (C)2O4)(O2CCH2CO2)]Lithium (difluoromalonic acid oxalic acid) borate [ LiB (C)2O4)(O2CCF2CO2)]Lithium tris (oxalato) phosphate [ LiP (C)2O4)3]And lithium tris (difluoromalonate) phosphate [ LiP (O)2CCF2CO2)3]And any combination of two or more of the foregoing lithium salts.
In some embodiments, the lithium salt is selected from lithium fluoride salts.
In a preferred embodiment, the lithium salt is selected from one or more of hexafluorophosphate, hexafluoroarsenate, perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, lithium tris (trifluoromethylsulfonyl) methide.
In some embodiments, the solvent is selected from non-aqueous organic solvents.
In a preferred embodiment, the solvent is selected from two or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, methyl formate, ethyl propionate, propyl propionate, methyl butyrate, tetrahydrofuran.
In some embodiments, the electrolyte solution further includes other additives for promoting the formation of the SEI film, and specifically, the additives include, but are not limited to: vinylene carbonate and its derivatives, ethylene carbonate derivatives having non-conjugated unsaturated bonds in the side chain thereof, cyclic carbonates substituted with halogen, and salts of chelate orthoborates and chelate orthophosphoric esters.
Specifically, the additive comprises one or more of vinylene carbonate, ethylene carbonate, methylene ethylene carbonate, fluoroethylene carbonate, trifluoromethyl ethylene carbonate and difluoroethylene carbonate.
In one embodiment, the electrolyte is composed of a solvent, a lithium salt, 2-dicyanovinyl-4-vinyl-1, 3-dioxolane, and N, N-dimethyl-m-phenylenediamine.
Another embodiment of the present invention provides a lithium ion battery, including a positive electrode sheet, a negative electrode sheet, a separator, and the electrolyte as described above.
The positive plate comprises a positive current collector and a positive active slurry layer positioned on the positive current collector, wherein the positive active slurry layer comprises a positive active material, a positive binder and a positive conductive agent; the negative plate comprises a negative current collector and a negative active slurry layer positioned on the negative current collector, wherein the negative active slurry layer comprises a negative active material, a negative binder and a negative conductive agent. The specific types of the positive electrode active material, the positive electrode binder, the positive electrode conductive agent, the negative electrode active material, the negative electrode binder and the negative electrode conductive agent are not particularly limited and can be selected according to requirements.
Preferably, the positive active material is selected from lithium cobaltate (LiCoO)2) Lithium nickel manganese cobalt ternary material, lithium iron phosphate (LiFePO)4) Lithium manganate (LiMn)2O4) One or more of (a).
Preferably, the negative active material is selected from graphite and/or silicon, such as natural graphite, artificial graphite, mesophase micro carbon spheres (abbreviated as MCMB), hard carbon, soft carbon, silicon-carbon composite, Li-Sn alloy, Li-Sn-O alloy, Sn, SnO2Spinel-structured lithiated TiO2-Li4Ti5O12And Li-Al alloy.
The lithium ion battery provided by the invention has the following beneficial effects:
in the electrolyte provided by the invention, the additive combination has synergistic effect to generate passive films on both the anode and the cathode, and the passive films can be kept stable in an extreme environment, so that high-temperature circulation and thermal shock resistance after circulation are improved.
The present invention will be further illustrated by the following examples.
Example 1
This embodiment is used to illustrate a lithium ion battery and a method for manufacturing the same disclosed in the present invention, and includes the following operation steps:
preparing an electrolyte: EC, DEC, PC were mixed at 1: 1: 1 as an organic solvent. Adding the additive with the mass percentage content shown in the example 1 in the table 1 into the organic solvent, uniformly mixing, and adding LiPF6Obtaining LiPF6The concentration is 1.1molAn electrolyte of/L.
Manufacturing a positive plate: the positive electrode active material lithium cobaltate (LiCoO)2) The conductive agent CNT (Carbon nano tube) and the adhesive polyvinylidene fluoride are fully stirred and mixed in the N-methyl pyrrolidone solvent according to the weight ratio of 97:1.5:1.5, so that uniform anode slurry is formed. And coating the slurry on an Al foil of a positive current collector, drying and cold pressing to obtain the positive plate.
And (3) manufacturing a negative plate: the negative electrode active material graphite, the conductive agent acetylene black, the binder styrene butadiene rubber and the thickener sodium carboxymethyl cellulose are fully stirred and mixed in a proper amount of deionized water solvent according to the mass ratio of 95:2:2:1 to form uniform negative electrode slurry. And coating the slurry on a Cu foil of a negative current collector, drying and cold pressing to obtain the negative plate.
Manufacturing the lithium ion battery: the PE porous polymer film is used as a separation film.
The positive pole piece, the isolating membrane and the negative pole piece are sequentially stacked, so that the isolating membrane is positioned between the positive pole and the negative pole, the isolating effect is achieved, and then the bare cell can be wound. And placing the bare cell into an outer packaging bag, respectively injecting the prepared electrolyte into the dried battery, and performing vacuum packaging, standing, formation, shaping and other processes to complete the preparation of the lithium ion battery.
TABLE 1
Examples 2 to 5
Examples 2 to 5 are provided to illustrate the lithium ion battery electrolyte, the lithium ion battery and the preparation method thereof disclosed in the present invention, including most of the operation steps as in example 1, and the differences are as follows:
in the preparation operation of the electrolyte: the additive with the mass percentage content shown in the embodiment 2-5 in the table 1 is added into the organic solvent.
Comparative examples 1 to 5
Comparative examples 1 to 5 are provided for comparative purposes to illustrate the lithium ion battery electrolyte, the lithium ion battery and the preparation method thereof disclosed in the present invention, including most of the operation steps as in example 1, and the differences are as follows:
in the preparation operation of the electrolyte: the additive with the mass percentage content shown in comparative examples 1-5 in the table 1 is added into the organic solvent.
Performance testing
The lithium ion batteries prepared in the above examples 1 to 5 and comparative examples 1 to 5 were subjected to the following performance tests:
45 degree cycle testing of the cell:
the test method comprises the following steps: charging the lithium ion battery to 4.45V at constant current and constant voltage of 1C in a constant temperature box with the temperature of 45 +/-2 ℃, cutting off at 0.05C, then discharging to 3V at 1C, and carrying out multiple charging and discharging cycles according to the conditions. The capacity retention after 50, 100, 300 and 500 cycles of the battery was calculated, 5 each.
Wherein the retention rate (corresponding cycle number discharge capacity)/(third cycle discharge capacity) × 100%
The capacity of the battery after cycling through the different cycles is reported in table 2.
TABLE 2 Capacity Retention after cycling
| Cell number | 50 times | 100 times (twice) | 300 times (twice) | 500 times (times) |
| Comparative example 1 | 95.6 | 90.10 | 78.6 | 62.5 |
| Comparative example 2 | 95.5 | 91.23 | 82.3 | 68.7 |
| Comparative example 3 | 96.1 | 91.30 | 83.15 | 68.4 |
| Comparative example 4 | 96.1 | 92.23 | 86.4 | 75.1 |
| Comparative example 5 | 96.2 | 89.90 | 78 | 60.7 |
| Example 1 | 97.3 | 95.23 | 92.3 | 88.7 |
| Example 2 | 96.7 | 94.40 | 90.6 | 84.1 |
| Example 3 | 96.7 | 93.93 | 88.55 | 82.3 |
| Example 4 | 97.7 | 94.20 | 90.7 | 84.2 |
| Example 5 | 96.6 | 93.53 | 88.5 | 80.7 |
When the data in tables 1 and 2 are combined, it can be seen that the electrolyte of comparative example 2, in which 11 mass% of 2-dicyanovinyl-4-vinyl-1, 3-dioxolane is added alone, has slightly improved cycle performance as compared to comparative example 1. In examples 1 to 5, when 5 mass% of 2-dicyanovinyl-4-vinyl-1, 3-dioxolane and 1 mass% of N, N-dimethyl-m-phenylenediamine were simultaneously added to the electrolyte, the electrolyte cycle performance was significantly improved. However, when the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte exceeds 10% or the content of N, N-dimethyl-m-phenylenediamine exceeds 5%, the cycle performance of the battery is not improved but even deteriorated, and particularly, the comparative example L5 in which 11% by mass of 2-dicyanovinyl-4-vinyl-1, 3-dioxolane and 6% by mass of N, N-dimethyl-m-phenylenediamine are added to the electrolyte has a cycle retention of the battery much lower than that of the other groups.
Thermal shock test of the cell after 500 weeks of 45 degree cycling:
the test method comprises the following steps: testing the thickness of the battery cell at room temperature, fully charging the battery for 500 weeks in a test box at 45 +/-2 ℃, placing the battery in a constant temperature box at 150 +/-2 ℃ for 1 hour, and monitoring the voltage change and the surface temperature of the battery and observing the state of the battery.
The conditions of the batteries of the respective examples after the thermal shock test are recorded in table 3.
TABLE 3
| Cell number | Thermal shock resistance test |
| Comparative example 1 | 0/5PASS；5/5FIRE |
| Comparative example 2 | 1/5PASS；4/5FIRE |
| Comparative example 3 | 1/5PASS；4/5FIRE |
| Comparative example 4 | 1/5PASS；4/5FIRE |
| Comparative example 5 | 0/5PASS；5/5FIRE |
| Example 1 | 5/5PASS |
| Example 2 | 5/5PASS |
| Example 3 | 5/5PASS |
| Example 4 | 5/5PASS |
| Example 5 | 5/5PASS |
The data in tables 1 and 3 are combined to show that compared with the lithium ion batteries provided in comparative examples 1-5, the thermal shock resistance of the lithium ion battery adopting the technical scheme of the application after circulation is improved. When the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane exceeds 10 percent, the passing rate is reduced, probably because excessive additives increase the film resistance during the circulation process to cause the precipitation of metal lithium and deteriorate the stability of the battery cathode, and the thermal shock performance of the battery after the circulation is deteriorated. However, the addition of N, N-dimethyl m-phenylenediamine can effectively reduce the precipitation of metal lithium in the circulation process and improve the thermal shock performance of the battery core after circulation. Therefore, the two additives are matched and used at the same time, so that the thermal shock performance of the battery after circulation can be obviously improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The lithium ion battery electrolyte is characterized by comprising a solvent, lithium salt and the following additives:
2-dicyanovinyl-4-vinyl-1, 3-dioxolane and
n, N-dimethyl-m-phenylenediamine;
the content of the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane in the electrolyte is less than or equal to 10% by mass, and the content of the N, N-dimethyl-m-phenylenediamine in the electrolyte is less than or equal to 5% by mass.
2. The lithium ion battery electrolyte of claim 1, wherein the 2-dicyanovinyl-4-vinyl-1, 3-dioxolane is present in the electrolyte in an amount of 0.05-10% by weight.
3. The lithium ion battery electrolyte of claim 1, wherein the content of N, N-dimethyl-m-phenylenediamine in the electrolyte is 0.01-5% by mass.
4. The lithium ion battery electrolyte of claim 1, wherein the concentration of the lithium salt in the electrolyte is between 0.5M and 2M.
5. The lithium ion battery electrolyte of claim 1, wherein the lithium salt comprises one or more of an organic lithium salt and an inorganic lithium salt.
6. The lithium ion battery electrolyte of claim 1, wherein the lithium salt is selected from a fluorine-containing lithium salt.
7. The lithium ion battery electrolyte of claim 1, wherein the lithium salt is selected from one or more of hexafluorophosphate, hexafluoroarsenate, perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, and lithium tris (trifluoromethylsulfonyl) methide.
8. The lithium ion battery electrolyte of claim 1, wherein the solvent is selected from two or more of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, methyl formate, ethyl propionate, propyl propionate, methyl butyrate, and tetrahydrofuran.
9. The lithium ion battery electrolyte of claim 1, wherein the electrolyte is comprised of a solvent, a lithium salt, 2-dicyanovinyl-4-vinyl-1, 3-dioxolane, and N, N-dimethyl meta-phenylenediamine.
10. A lithium ion battery comprising a positive electrode sheet, a negative electrode sheet, a separator and the electrolyte according to any one of claims 1 to 9.
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