CN109346763B - Electrolyte and lithium ion battery - Google Patents
Electrolyte and lithium ion battery Download PDFInfo
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- CN109346763B CN109346763B CN201811223562.7A CN201811223562A CN109346763B CN 109346763 B CN109346763 B CN 109346763B CN 201811223562 A CN201811223562 A CN 201811223562A CN 109346763 B CN109346763 B CN 109346763B
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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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- 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
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Abstract
The invention discloses an electrolyte and a lithium ion battery prepared from the electrolyte. The aniline compound and the thiophene compound in the electrolyte are combined with each other, so that the performance of the passive films on the positive electrode and the negative electrode in the electrolyte can be improved in a synergistic manner, the passive films are more stable, and the prepared lithium ion battery has more excellent high and low temperature impact resistance.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to an electrolyte and a lithium ion battery.
Background
Since the last 90 th century, the japan SONY corporation successfully commercialized the lithium ion battery, and the lithium ion battery has been widely used in the field of electronic products. Compared with other traditional storage batteries, the lithium ion battery has the characteristics of high specific energy, strong heavy current discharge capacity, long cycle life, high energy storage efficiency and the like. Therefore, the lithium ion battery becomes the most competitive battery of the new generation, is known as green and environment-friendly energy, and is the first choice technology for solving the current environmental pollution problem and energy problem.
Generally, a lithium ion battery includes a casing, a cell enclosed in the casing, and an electrolyte, where the cell generally includes a positive electrode, a negative electrode, and a separator separating the two electrodes. As the application range of lithium ion batteries becomes wider, the performance requirements of lithium ion batteries are higher, and how to improve some of the above components of lithium ion batteries to obtain better high and low temperature impact resistance is also a hot issue.
Disclosure of Invention
The invention aims to solve the technical problem of how to provide an electrolyte and a lithium ion battery using the electrolyte, and the formula of the electrolyte can enable the lithium ion battery to have better high and low temperature impact resistance.
The technical scheme adopted by the invention is as follows:
an electrolyte comprises a lithium salt, an organic solvent and an additive, wherein the additive comprises an aniline compound and a thiophene compound, and the aniline compound is at least one of compounds shown in a general formula (1):
wherein R is1、R2Each independently selected from C1-C10 hydrocarbyl groups;
the hydrocarbon group herein includes at least alkyl, alkenyl, alkynyl, aryl, alkaryl, and aralkyl groups, including, for example, but not limited to, methyl, ethyl, propyl, hexyl, octyl, decyl, ethenyl, propenyl, allyl, ethynyl, propynyl, propargyl, phenyl, benzyl, tolyl, and the like.
Preferably, R1、R2Each independently selected from C1-C10 alkyl.
Further preferably, R1And R2Are all methyl.
More preferably, the aniline compound is N, N-dimethyl m-phenylenediamine.
Preferably, the thiophene compound is at least one represented by the general formula (2):
wherein R is3、R4、R5、R6Each independently selected from hydrogen or a C1-C10 hydrocarbyl group;
the hydrocarbon group herein includes at least alkyl, alkenyl, alkynyl, aryl, alkaryl, and aralkyl groups, including, for example, but not limited to, methyl, ethyl, propyl, hexyl, octyl, decyl, ethenyl, propenyl, allyl, ethynyl, propynyl, propargyl, phenyl, benzyl, tolyl, and the like.
More preferably, the thiophene compound is 3, 4-ethylenedioxythiophene.
Preferably, the aniline compound is contained in an amount of 0.05 to 10 wt% and the thiophene compound is contained in an amount of 0.01 to 10 wt%, based on the total weight of the electrolyte.
More preferably, the aniline compound is contained in an amount of 0.1 to 5 wt%.
More preferably, the content of the thiophene compound is 0.1 to 5 wt%.
Preferably, the lithium salt contains fluorine.
Preferably, the lithium salt is selected from at least one of hexafluorophosphate, hexafluoroarsenate, perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, and lithium tris (trifluoromethylsulfonyl) methide.
Still more preferably, the concentration of the lithium salt is 0.5 to 2mol/L based on the total volume of the electrolyte. 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 are affected. The lithium salt concentration is too high, the viscosity of the electrolyte is too high, and the multiplying power of the whole battery system is also influenced.
Still more preferably, the concentration of the lithium salt is 0.9 to 1.3 mol/L.
Preferably, the organic solvent is 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.
A lithium ion battery comprises the electrolyte. Meanwhile, the lithium ion battery also comprises a positive plate, a negative plate and a diaphragm.
Further, the lithium ion battery specifically comprises a positive current collector forming a positive plate, a positive diaphragm coated on the positive current collector, a negative current collector forming a negative plate, a negative diaphragm coated on the negative current collector, an isolating film, electrolyte and packaging foil;
the anode diaphragm comprises an anode active material, a binder and a conductive agent, and the cathode diaphragm comprises a cathode active material, a binder and a conductive agent.
Preferably, the positive active material is at least one of lithium cobaltate, a nickel-cobalt-manganese-lithium ternary material, lithium iron phosphate and lithium manganate.
Preferably, the negative active material is graphite.
The invention has the beneficial effects that:
the inventor unexpectedly finds that the aniline compound and the thiophene compound are synergistic when the aniline compound and the thiophene compound are used as additives of lithium ion battery electrolyte at the same time, so that the high and low temperature impact resistance of the lithium ion battery is improved. The lithium ion battery prepared according to the electrolyte can effectively stabilize a reaction system under the conditions of high temperature and high pressure or frequent temperature switching, reduces the exposure of active sites in the reaction system, and better ensures and improves the high and low temperature impact resistance of the battery.
In addition, the inventor also finds that the lithium ion battery prepared by the method also has quite excellent continuous charging performance under the high-temperature condition, and the lithium ion battery is outstanding in a floating charge test at 45 ℃.
The inventors have analyzed that good synergy of this additive combination may be associated with passive films. In the first charge-discharge process of the lithium ion battery, the electrode material and the electrolyte react on a solid-liquid phase interface to form a passivation layer covering the surface of the electrode material. This passivation layer is also referred to as a "Solid Electrolyte Interface film", i.e., SEI film/passivation film. This passivation layer is an interfacial layer that has the characteristics of a solid electrolyte. The combination of the aniline and thiophene compounds can make the passive films on the positive and negative pole pieces more stable after being formed, so that the high-temperature impact resistance and the continuous charging performance are obtained.
Detailed Description
The conception, the specific structure, and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below, so that the objects, the features, and the effects of the present invention can be fully understood. 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. In addition, all the connection/connection relations referred to in the patent do not mean that the components are directly connected, but mean that a better connection structure can be formed by adding or reducing connection auxiliary components according to specific implementation conditions. All technical characteristics in the invention can be interactively combined on the premise of not conflicting with each other.
Example 1
1. Preparation of the electrolyte
Mixing Ethylene Carbonate (EC), diethyl carbonate (DEC), Polycarbonate (PC) in a ratio of 1: 1 as an organic solvent. Adding a certain amount of N, N-dimethyl m-phenylenediamine and 3, 4-ethylene dioxythiophene into an organic solvent, uniformly mixing, and then adding a certain amount of LiPF6Obtaining LiPF6The mixed solution with the concentration of 1.1mol/L is the prepared electrolyte.
2. Preparation of the Battery
2.1 preparation of Positive electrode plate
The positive electrode active material lithium cobaltate (LiCoO)2) The conductive agent Carbon Nano Tube (CNT) and the adhesive polyvinylidene fluoride are 97: 1.5: 1.5 fully stirring and mixing in N-methyl pyrrolidone solvent 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.
2.2 preparation of negative plate
The method comprises the following steps of mixing a negative electrode active material graphite, a conductive agent acetylene black, a binder styrene butadiene rubber and a thickener sodium carboxymethyl cellulose according to a mass ratio of 95: 2: 2: 1 in a proper amount of deionized water solvent, fully stirring and mixing to form uniform cathode slurry. And coating the slurry on a Cu foil of a negative current collector, drying and cold pressing to obtain a negative pole piece.
2.3 preparation of lithium ion batteries
The positive pole piece, the isolating membrane and the negative pole piece are sequentially stacked, the isolating membrane is positioned between the positive pole and the negative pole, the isolating effect is achieved, and then the bare cell is formed by winding. And (2) placing the bare cell into an outer packaging bag, injecting the electrolyte prepared in the step (1) into the dried battery, and performing vacuum packaging, standing, formation, shaping and other processes to complete the preparation of the lithium ion battery.
Example 2
Comparative experiment
The electrolyte is prepared according to the contents of N, N-dimethyl m-phenylenediamine and 3, 4-ethylene dioxythiophene in the following table, wherein the numerical value represents the weight percentage of each component in the electrolyte.
TABLE 1 content of additives in different formulations
Corresponding lithium ion batteries were prepared according to the different electrolyte formulations described above, following the procedure in example 1.
And carrying out corresponding high and low temperature impact test on the prepared lithium ion battery. The specific test method comprises the following steps:
a. measuring the initial discharge capacity of the battery at normal temperature, and then fully charging;
b. placing the battery in an experimental oven, then reducing the temperature in the experimental oven to-40 +/-2 ℃, and keeping for 1 h; the temperature conversion time is not more than 30 min;
c. the temperature of the test chamber is raised to 70 +/-2 ℃ again, and the temperature conversion time is not more than 30 min.
And (3) repeating the steps a-C for 10 times, checking the appearance of the battery, placing the battery at normal temperature for 24 hours, discharging the battery to 3.0V at 0.2C, recording the residual discharge capacity, discharging the battery to 3V at 0.2C after the battery is fully charged at 0.7C, recording the recovery capacity, and calculating the residual rate and the recovery rate.
Wherein the remaining rate is (remaining discharge capacity)/(initial discharge capacity) × 100%,
the recovery rate is (recovery capacity)/(initial discharge capacity) × 100%.
The situation of the residual recovery capacity of the battery after temperature shock is shown in table 2, wherein the cell numbers C1# to C11# are in one-to-one correspondence with the electrolyte numbers L1# to L11 #.
In addition, the cell was also subjected to a float charge test at 45 ℃. The specific test method is as follows:
testing the thickness of the battery cell at room temperature, charging the battery to full charge at constant current and constant voltage of 0.5C in a test box at 45 +/-2 ℃, testing the thickness of the battery cell after 30 days, 45 days and 60 days without setting a cutoff current, and calculating the expansion rate of the battery cell.
Wherein, the cell expansion rate is (thickness during the floating charging process-thickness before entering the box)/(thickness before entering the box) x 100%.
The swelling condition of the floating thickness of the battery after the floating charge test at 45 ℃ is shown in table 2.
TABLE 2 comparative test results
C6# is a scheme without adding N, N-dimethyl m-phenylenediamine and 3, 4-ethylenedioxythiophene. C7# and C8# are respectively schemes of independently adding 11 wt% of N, N-dimethyl metaphenylene diamine and 11 wt% of 3, 4-ethylenedioxythiophene, and the residual rate and the recovery rate of the schemes are improved to a certain extent compared with those of C6#, which shows that the capacity of the schemes after temperature shock is slightly improved. Meanwhile, the thickness expansion at different times is slightly less than C6 #. The results of the temperature impact test and the float test of the C9# and the C10#, which are respectively added with 3 wt% of 3, 4-ethylenedioxythiophene and 5% of N, N-dimethyl m-phenylenediamine on the basis of the C7# and the C8#, are not obviously improved compared with the results of the C7# and the C8 #. In addition, in combination with C11#, it can be seen that when the additive of the electrolyte employs N, N-dimethyl-m-phenylenediamine in excess of 10 wt% or 3, 4-ethylenedioxythiophene in excess of 10 wt%, the performance of the above two tests of the battery is not improved, but even deteriorated, especially C11# with 11 wt% N, N-dimethyl-m-phenylenediamine and 11 wt% 3, 4-ethylenedioxythiophene added to the electrolyte, which shows battery performance much worse than the other groups.
The contents of the two additives in C1-C5 # are both less than 10 wt%, and as can be seen from the results in Table 2, the temperature impact test result and the floating charge test result are both obviously superior to those of C6#, which shows that when N, N-dimethyl m-phenylenediamine is selected from aniline compounds and 3, 4-ethylenedioxythiophene is selected from thiophene compounds as the additive component of the electrolyte, the contents of the additives are within 10 wt%, the stability of the battery in the high and low temperature impact test and the continuous charging performance of the battery at high temperature can be better improved, the improvement can be related to the passive films on the positive and negative pole pieces, and the use of the additive combination can optimize the passive films on the positive and negative pole pieces. Particularly, C1# and C2# are superior to C3# and C4# are superior to C5#, which shows that when the content of N, N-dimethyl m-phenylenediamine is 0.1-5 wt% and the content of 3, 4-ethylenedioxythiophene is 0.1-5 wt%, the system of the battery can be stabilized under the conditions of high temperature and high pressure or frequent temperature switching, the exposure of active sites is reduced, and the performance of the battery is better ensured.
Example 3
An electrolytic solution was different from L4# in example 2 in that N, N-dimethyl-m-phenylenediamine was replaced with N, N-dimethyl-p-phenylenediamine.
Example 4
An electrolytic solution was different from L4# in example 2 in that N, N-dimethyl-m-phenylenediamine was replaced with N-isopropyl-N- (ethylphenyl) benzene-1, 3-diamine, and 3, 4-ethylenedioxythiophene was replaced with a thiophene compound represented by the formula (3):
while the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. An electrolyte comprises a lithium salt, an organic solvent and an additive, and is characterized in that the additive comprises an aniline compound and a thiophene compound, wherein the aniline compound is at least one of compounds shown in a general formula (1):
wherein R is1、R2Each independently selected from C1-C10 hydrocarbyl groups; the content of the aniline compound is 0.05-10 wt%, and the content of the thiophene compound is 0.01-10 wt%.
2. The electrolyte of claim 1, wherein R is1And said R2Are all methyl.
3. The electrolyte according to claim 2, wherein the aniline compound is N, N-dimethyl-m-phenylenediamine.
4. The electrolyte according to claim 1, wherein the thiophene compound is at least one represented by the general formula (2):
wherein R is3、R4、R5、R6Each independently selected from hydrogen or a C1-C10 hydrocarbyl group.
5. The electrolyte of claim 4, wherein the thiophenic compound is 3, 4-ethylenedioxythiophene.
6. The electrolyte of claim 1, wherein the aniline compound is present in an amount of 0.1 to 5 wt%.
7. The electrolyte of claim 1, wherein the thiophenic compounds are present in an amount of 0.1-5 wt%.
8. The electrolyte of any one of claims 1-7, wherein the lithium salt is selected from at least one of hexafluorophosphate, hexafluoroarsenate, perchlorate, lithium trifluorosulfonyl, lithium difluoro (trifluoromethylsulfonyl) imide, lithium bis (fluorosulfonyl) imide, and lithium tris (trifluoromethylsulfonyl) methide.
9. A lithium ion battery comprising the electrolyte of any one of claims 1 to 8.
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| CN110190329B (en) * | 2019-05-20 | 2022-02-22 | 惠州市豪鹏科技有限公司 | Application of 4, 4-bis-1, 3, 2-dioxazole thiophene-2, 2-dioxide, electrolyte and lithium ion battery |
| CN114361591B (en) * | 2021-12-23 | 2024-05-17 | 惠州市豪鹏科技有限公司 | Electrolyte and battery |
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| CN104577200A (en) * | 2015-02-06 | 2015-04-29 | 宁德新能源科技有限公司 | Electrolyte additive and application thereof |
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| TWI487161B (en) * | 2011-11-16 | 2015-06-01 | Univ Nat Taiwan Science Tech | Lithium-ion battery and method for fabricating the same |
| CN104124470B (en) * | 2013-04-25 | 2017-05-03 | 中国科学院宁波材料技术与工程研究所 | High safety battery electrolyte solution |
| CN108346824A (en) * | 2017-01-25 | 2018-07-31 | 索尼公司 | Nonaqueous electrolytic solution and nonaqueous electrolytic solution secondary battery |
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Patent Citations (5)
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|---|---|---|---|---|
| CN101145622A (en) * | 2007-09-04 | 2008-03-19 | 武汉大学 | Reversible over-charge protective electrolyte additive of lithium ion battery and its making method |
| CN102569896A (en) * | 2010-12-10 | 2012-07-11 | 比亚迪股份有限公司 | Lithium ion secondary battery and preparation method thereof |
| DE102014203707A1 (en) * | 2014-02-28 | 2015-09-03 | Robert Bosch Gmbh | Additive combination for lithium cell |
| CN104577200A (en) * | 2015-02-06 | 2015-04-29 | 宁德新能源科技有限公司 | Electrolyte additive and application thereof |
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