CN110994025A - Electrolyte additive, electrolyte and lithium ion battery - Google Patents
Electrolyte additive, electrolyte and lithium ion battery Download PDFInfo
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- CN110994025A CN110994025A CN201911254811.3A CN201911254811A CN110994025A CN 110994025 A CN110994025 A CN 110994025A CN 201911254811 A CN201911254811 A CN 201911254811A CN 110994025 A CN110994025 A CN 110994025A
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- electrolyte
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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 additive, an electrolyte and a lithium ion battery. The electrolyte additive can be applied to battery electrolyte, can improve the stability of the electrolyte and the film-forming property of a positive electrode interface and a negative electrode interface of a battery under high voltage, and further improves the cycle performance of the battery.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to an electrolyte additive, an electrolyte and a lithium ion battery.
Background
The lithium ion battery has the advantages of high specific energy, large specific power, long cycle life, small self-discharge, environmental friendliness and the like, is popular with consumers, and is widely applied to the fields of 3C electronic products (such as mobile communication, digital cameras, video cameras and the like), electric automobiles, military aerospace and the like. Along with the popularization of intelligent digital products, the application of new energy automobiles is more and more extensive, the application of lithium ion batteries in daily life of people is more and more extensive, and the demand of consumers on the high-energy density lithium ion batteries is more and more urgent. The important means for improving the energy density of the lithium ion battery is to improve the gram capacity of the anode material by improving the charge cut-off voltage of the battery, so that the energy density of the lithium ion battery is improved. The electrolyte is used as an important component of the lithium ion battery, plays a role in transmitting lithium ions in the charge and discharge process, and has a great influence on the high-temperature performance and the high-voltage working performance of the battery. However, the electrolyte solvent used conventionally is easily oxidized and decomposed on the surface of the positive electrode at high temperature and high voltage, and the decomposition of the electrolyte promotes the deterioration reaction of the positive and negative electrode active materials, thereby causing the reduction of the cycle performance of the lithium ion battery.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides an electrolyte additive, an electrolyte and a lithium ion battery, wherein the electrolyte additive can be applied to the electrolyte of the battery, and can improve the stability of the electrolyte and the film-forming property of a positive electrode interface and a negative electrode interface of the battery under high voltage, so that the cycle performance of the battery is improved.
The technical scheme adopted by the invention is as follows:
the invention provides an electrolyte additive, which comprises the following components in percentage by mass (0.1-5): (0.1-10) pentafluorophenyl methanesulfonate and lithium difluorooxalatoborate. The structural formula of the pentafluorophenyl methanesulfonate is
According to some embodiments of the invention, the mass ratio of the pentafluorophenyl methanesulfonate to the lithium difluorooxalato borate is (0.2-3): (0.5-5).
In a second aspect of the present invention, an electrolyte is provided, which includes an electrolyte lithium salt, an organic solvent, and any one of the electrolyte additives provided in the first aspect of the present invention, and the electrolyte additive is 0.3% to 11% by mass in the electrolyte.
Specifically, the mass percentage content of pentafluorophenyl methanesulfonate in the electrolyte additive in the electrolyte can be 0.1-5%, and the mass percentage content of lithium difluoro-oxalato-borate in the electrolyte can be 0.1-10%. When the mass percentage content of the pentafluorophenyl methanesulfonate in the electrolyte is less than 0.1%, the pentafluorophenyl methanesulfonate cannot function as a high voltage additive; when the content is more than 5%, a dense passivation film is easily formed on the positive and negative electrodes to increase the impedance, and the battery performance is deteriorated. When the mass percentage content of the lithium difluoro (oxalyl) borate in the additive is less than 0.1 percent, the film forming effect is not ideal and is not obvious; when the amount is more than 8%, the resistance of the battery in electrochemical reaction is too high, and the amounts of both are strictly controlled.
In the electrolyte additive, the upper limit of the mass percentage content range of the pentafluorophenyl methanesulfonate in the electrolyte can be selected from 5% and 3%, the lower limit of the mass percentage content range can be selected from 0.1% and 0.2%, and the mass percentage content of the pentafluorophenyl methanesulfonate in the electrolyte is preferably 0.2% -3%; the upper limit of the mass percentage content range of the lithium difluoro (oxalato) borate in the electrolyte can be selected from 10%, 8%, 5% and 4%, the lower limit can be selected from 0.1%, 0.2%, 0.5% and 1%, and the mass percentage content of the lithium difluoro (oxalato) borate in the electrolyte is preferably 0.1% -8%, and more preferably 0.5% -5%.
According to some embodiments of the invention, the electrolytic lithium salt is an organic lithium salt or an inorganic lithium salt.
According to some embodiments of the invention, the electrolytic lithium salt is selected from a lithium salt of a fluorine-containing element or a lithium element.
According to some embodiments of the invention, the electrolyte lithium salt may be selected from at least one of lithium hexafluorophosphate, lithium hexafluoroarsenate, lithium perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, lithium tris (trifluoromethylsulfonyl) methide.
According to some embodiments of the invention, the concentration of the electrolyte lithium salt in the electrolyte solution is 0.5 to 2 mol/L. The electrolyte lithium salt concentration 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; the concentration of the electrolyte lithium salt is too high, the viscosity of the electrolyte is too high, and the multiplying power of the whole battery system is also influenced. Preferably, the concentration of the electrolyte lithium salt in the electrolyte is 0.9-1.3 mol/L.
According to some embodiments of the present invention, the organic solvent is an organic complex solvent, and may be specifically selected from at least two of Ethylene Carbonate (EC), Propylene Carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC), methyl formate, ethyl propionate, Propyl Propionate (PP), methyl butyrate, and tetrahydrofuran.
In a third aspect of the invention, there is provided a lithium ion battery comprising any one of the electrolytes provided in the second aspect of the invention. Specifically, the lithium ion battery includes a positive electrode sheet, a negative electrode sheet, a separator disposed between the positive electrode sheet and the negative electrode sheet, and an electrolyte.
According to some embodiments of the present invention, the positive electrode sheet includes a positive electrode current collector and a positive electrode membrane coated on the positive electrode current collector, and the material of the positive electrode membrane includes a positive electrode active material, a conductive agent and a binder; the negative plate comprises a negative current collector and a negative diaphragm coated on the negative current collector, and the material of the negative diaphragm comprises a negative active material, a conductive agent and a binder.
The positive active material may be selected from lithium cobaltate (LiCoO)2) Lithium nickel manganese cobalt ternary material, lithium iron phosphate (LiFePO)4) Lithium manganate (LiMn)2O4) At least one of; the negative electrode active material is selected from natural graphite, artificial graphite, mesophase micro carbon spheres (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 upper limit charging voltage of the lithium ion battery is 4.5V.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides an electrolyte additive, which comprises the following components in percentage by mass (0.1-5): (0.1-10) pentafluorophenyl methanesulfonate and lithium difluoro-oxalato-borate, and the electrolyte additive can be applied to the electrolyte of a lithium ion battery. The pentafluorophenyl methanesulfonate has a lower oxidation potential than a solvent, can be oxidized and polymerized on the surface of a battery anode to form a compact solid electrolyte phase interface film (CEI), can effectively reduce the decomposition of the solvent on the anode, and is very beneficial to the battery performance because the polymer formed by the pentafluorophenyl methanesulfonate and lithium covers the surface of the anode, and the polymer is not easily dissolved by an electrolyte solvent, so the CEI is more stable; the CEI can effectively prevent the side reaction of the anode material and the electrolyte on the surface of the anode and can effectively reduce the increase of the interface impedance of the anode in the circulation process; meanwhile, the polymeric film can prevent elements such as Mn, Co and the like in the positive electrode material from dissolving out, and inhibit the electrolyte from generating oxidation gas to cause the battery to swell. Lithium difluorooxalato borate (LiODFB) can form a stable SEI film on a negative electrode, so that an ion-conducting solvent is prevented from being further reduced in the charge and discharge processes. When the pentafluorophenyl methanesulfonate and the lithium difluoro oxalato borate (LiODFB) are used in a matched mode, the pentafluorophenyl methanesulfonate and the lithium difluoro oxalato borate (LiODFB) can generate stable passive films on the positive electrode and the negative electrode of the secondary battery under the synergistic effect, and the long cycle performance and the overcharge performance of the battery can be improved due to the existence of effective and stable CEI and SEI. The electrolyte additive is applied to the electrolyte of the lithium ion battery, the additive can improve the film forming performance under high voltage, the film thickness is thin, compact and stable, the positive and negative electrode interfaces can be protected, meanwhile, the additive can improve the stability of the electrolyte, electrons in the battery can be absorbed during overcharge testing, the reaction heat is reduced, and the safety performance of the battery is improved; further, the lithium ion battery adopting the electrolyte has the advantages that the charging upper limit voltage can reach 4.5V, and the long-cycle capacity retention rate is high.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Preparation of electrolyte
Mixing Ethylene Carbonate (EC), diethyl carbonate (DEC) and Propylene Carbonate (PC) according to the mass ratio of 1:1:1, and uniformly mixing to obtain the productAn organic solvent. Then, the additive A pentafluorophenyl methanesulfonate and the additive B difluoro oxalatoborate (refer to Table 1 specifically) were added in different proportions, and after mixing uniformly, lithium hexafluorophosphate (LiPF) was added6) And calculating the required mass of lithium hexafluorophosphate according to the concentration of the lithium salt of 1.1mol/L, uniformly stirring to obtain comparative example electrolyte L1# -L5 # and example electrolyte L6# -L11 #, and hermetically storing at normal temperature for later use. Wherein, the additive A pentafluorophenyl methanesulfonate and the additive B difluoro oxalato borate (LiODFB) in each electrolyte are matched to form a corresponding electrolyte additive, and the concrete structural formula of the pentafluorophenyl methanesulfonate (CAS number: 161912-36-3) is as follows:
TABLE 1 contents of additive A and additive B in comparative and example electrolytes
Note: the mass percentages of additive a and additive B in the electrolyte are given in table 1.
Preparation of (II) lithium ion battery
(1) Preparing a positive plate: the positive electrode active material lithium cobaltate (LiCoO)2) The conductive agent Carbon Nano Tube (CNT) and the adhesive polyvinylidene fluoride (PVDF) are fully stirred and mixed in N-methyl pyrrolidone (NMP) solvent according to the weight ratio of 97:1.5:1.5 to form uniform anode slurry; and coating the slurry on an Al foil of a positive current collector, drying and cold pressing to obtain the positive plate.
(2) Preparing a negative plate: fully stirring and mixing a negative active material graphite, a conductive agent acetylene black, a binder Styrene Butadiene Rubber (SBR), a thickening agent carboxymethyl cellulose sodium salt (CMC) and deionized water solvent according to a weight 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.
(3) Assembling: the method comprises the steps of stacking a positive plate, a diaphragm (a PE porous polymer film) and a negative plate in sequence, arranging the diaphragm between the positive plate and the negative plate to play a role in isolation, then winding to form a bare cell, then placing the bare cell into an outer packaging bag, respectively injecting the prepared electrolyte solution L1-L11 into a dried battery, then performing vacuum-pumping packaging, standing, formation, shaping and other processes, and correspondingly preparing the lithium ion battery C1-C11.
Specifically, the lithium ion batteries C1# to C11# prepared by the method and the corresponding electrolytes have no difference in other aspects except for different electrolyte additives.
(III) testing of the Performance of the batteries
1. Battery overcharge test
The overcharge test is respectively carried out on the lithium ion batteries C1# to C11# prepared in the above, and the specific test method comprises the following steps: discharging the semi-charged battery to 3.0V at 25 ℃ by using 0.5C, then charging to 6V by using 1C constant current, and when the 6V constant voltage charging time is more than 4h, not setting cut-off current, simultaneously testing the temperature change of the battery in the charging process and observing the state of the tested battery, wherein the battery does not ignite or explode, and the surface temperature rise is lower than 150 ℃, namely the battery passes. The overcharge test of the battery was performed by the above method, and the results are shown in table 2 below.
TABLE 2 Battery overcharge test results
| Lithium ion battery numbering | The electrolyte used is | Overcharge test pass rate |
| Battery C1# | Comparative example electrolyte L1# | 0/10 |
| Battery with a battery cellC2# | Comparative example electrolyte L2# | 0/10 |
| Battery C3# | Comparative example electrolyte L3# | 5/10 |
| Battery C4# | Comparative example electrolyte L4# | 7/10 |
| Battery C5# | Comparative example electrolyte L5# | 8/10 |
| Battery C6# | Examples electrolyte L6# | 10/10 |
| Battery C7# | Examples electrolyte L7# | 10/10 |
| Battery C8# | Examples electrolyte L8# | 10/10 |
| Battery C9# | Examples electrolyte L9# | 10/10 |
| Battery C10# | Examples electrolyte L10# | 10/10 |
| Battery C11# | Examples electrolyte L11# | 10/10 |
As can be seen from table 1 and table 2, compared with the batteries C1# to C5#, the battery C6# to C11# uses an electrolyte solution containing pentafluorophenyl methanesulfonate and lithium difluoro oxalato borate at a proper ratio, so that the overcharge pass rate of the battery is significantly improved.
2. Battery cycle performance test
The lithium ion battery C1-C11 # prepared by the method is subjected to cycle performance test respectively, and the specific test method comprises the following steps: the battery is placed in a constant temperature box at 25 ℃, is charged to 4.45V at a constant current and a constant voltage of 1C, is discharged at 1C, is circulated for 500 weeks, and the capacity retention rate of the battery is calculated according to the following formula:
capacity retention (%) — discharge capacity (mAh) at different cycle cycles/discharge capacity (mAh) at 3 rd cycle × 100%.
The above method was used to perform the battery cycle performance test, and the results are shown in table 3 below.
TABLE 3 Battery cycling Performance test results
As can be seen from table 1 and table 3, compared with the batteries C1# to C5#, the electrolyte of the batteries C6# to C11# is added with a proper amount of pentafluorophenyl methanesulfonate and lithium difluorooxalato borate, so that the high-temperature cycle capacity retention rate of the lithium ion battery can be significantly improved, and the capacitance retention rate of the battery is relatively low without using the combination of the pentafluorophenyl methanesulfonate and the lithium difluorooxalato borate or the improper addition ratio of the pentafluorophenyl methanesulfonate and the lithium difluorooxalato borate.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. An electrolyte additive is characterized by comprising the following components in percentage by mass (0.1-5): (0.1-10) pentafluorophenyl methanesulfonate and lithium difluorooxalatoborate.
2. The electrolyte additive according to claim 1, wherein the mass ratio of the pentafluorophenyl methanesulfonate to the lithium difluorooxalato borate is (0.2-3): (0.5-5).
3. An electrolytic solution, comprising an electrolytic lithium salt, an organic solvent and the electrolyte additive according to claim 1 or 2; the electrolyte additive accounts for 0.3-11% of the electrolyte by mass.
4. The electrolyte of claim 3, wherein the electrolytic lithium salt is an organic lithium salt or an inorganic lithium salt.
5. The electrolyte of claim 4, wherein the electrolytic lithium salt is selected from a lithium salt of a fluorine-containing element or a lithium element.
6. The electrolyte of claim 5, wherein the electrolyte lithium salt is selected from at least one of lithium hexafluorophosphate, lithium hexafluoroarsenate, lithium perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, and lithium tris (trifluoromethylsulfonyl) methide.
7. The electrolyte according to claim 4, wherein the concentration of the electrolyte lithium salt in the electrolyte is 0.5 to 2 mol/L.
8. The electrolyte of claim 3, wherein the organic solvent is selected from at least two of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, methyl formate, ethyl propionate, propyl propionate, methyl butyrate, and tetrahydrofuran.
9. A lithium ion battery comprising a positive electrode sheet, a negative electrode sheet, a separator provided between the positive electrode sheet and the negative electrode sheet, and the electrolyte solution according to any one of claims 3 to 8.
10. The lithium ion battery of claim 9, wherein the positive electrode sheet comprises a positive electrode current collector and a positive electrode membrane coated on the positive electrode current collector, and the material of the positive electrode membrane comprises a positive electrode active material, a binder and a conductive agent; the negative plate comprises a negative current collector and a negative diaphragm coated on the negative current collector, and the material of the negative diaphragm comprises a negative active material, a binder and a conductive agent.
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Application publication date: 20200410 |