CN113823841B - Electrolyte and preparation method and application thereof - Google Patents
Electrolyte and preparation method and application thereof Download PDFInfo
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- CN113823841B CN113823841B CN202111272902.7A CN202111272902A CN113823841B CN 113823841 B CN113823841 B CN 113823841B CN 202111272902 A CN202111272902 A CN 202111272902A CN 113823841 B CN113823841 B CN 113823841B
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000000654 additive Substances 0.000 claims abstract description 12
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 11
- 159000000002 lithium salts Chemical class 0.000 claims abstract description 11
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims abstract description 10
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 9
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 8
- OBAJXDYVZBHCGT-UHFFFAOYSA-N tris(pentafluorophenyl)borane Chemical compound FC1=C(F)C(F)=C(F)C(F)=C1B(C=1C(=C(F)C(F)=C(F)C=1F)F)C1=C(F)C(F)=C(F)C(F)=C1F OBAJXDYVZBHCGT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 5
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910003473 lithium bis(trifluoromethanesulfonyl)imide Inorganic materials 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000004146 energy storage Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- 230000000694 effects Effects 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000003181 co-melting Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Classifications
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—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
- H01M10/0568—Liquid materials characterised by the solutes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
- H01M2300/0037—Mixture of solvents
- H01M2300/004—Three solvents
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
Abstract
The application discloses an electrolyte, a preparation method and application thereof. An electrolyte, the preparation raw materials include: a solvent comprising ethylene carbonate, propylene carbonate, and methyl ethyl carbonate; a lithium salt comprising lithium bis (trifluoromethanesulfonyl) imide; in the electrolyte, the molar concentration of the lithium salt is 1.6-2.5M; additives including lithium carbonate, lithium silicate, cyclohexane and tris (pentafluorophenyl) borane. The electrolyte provided by the application can improve the safety performance, the cycle performance, the multiplying power performance and the high-low temperature performance of a secondary battery containing the obtained electrolyte by adjusting the types of the solvent, the lithium salt and the additive in the electrolyte.
Description
Technical Field
The application belongs to the technical field of secondary batteries, and particularly relates to an electrolyte and a preparation method and application thereof.
Background
With the rapid development of new energy automobiles, portable power supplies, energy storage and other fields, people put forward higher requirements on the performance of lithium batteries, and the importance of high-performance lithium ion batteries is increasingly outstanding. The electrolyte is an important component of the lithium ion battery, and has important influence on the output voltage, the multiplying power performance, the applicable temperature range, the cycle performance, the safety performance and the like of the battery.
At present, side reactions are easy to occur at the electrode interface of some commercial electrolytes, so that transition metal elements are dissolved, and the circulation capacity of the battery is reduced. Because most solvents are inflammable organic matters with low boiling point, low flash point and high volatility, the electrolyte is highly inflammable and extremely volatile, and has the safety problem, the further application and development of the lithium ion battery are limited to a great extent, and meanwhile, different additives have different action mechanisms and different film forming thicknesses on electrodes, and the application is difficult. And the electrolyte is easy to generate side reaction at the electrode interface, so that the transition metal element is dissolved, and the circulation capacity of the battery is reduced. Because most solvents are inflammable organic matters with low boiling point, low flash point and high volatility, the electrolyte is highly inflammable and extremely volatile, and has the safety problem, so that the further application and development of the lithium ion battery are limited to a great extent.
Therefore, it is important to provide an electrolyte with comprehensive and balanced performance, and to enable the electrolyte to simultaneously meet the high-low temperature performance and the safety performance of the battery.
Disclosure of Invention
The present application aims to solve at least one of the technical problems in the prior art described above. Therefore, the application provides the electrolyte, and the safety performance, the cycle performance, the multiplying power performance and the high-low temperature performance of the secondary battery prepared by using the electrolyte can be obviously improved by adjusting the types and the content proportion relation of the solvent, the lithium salt and the additive in the electrolyte.
The application also provides a preparation method of the electrolyte.
The application also provides a secondary battery with the electrolyte.
The application also provides an application of the secondary battery.
According to one aspect of the present application, there is provided an electrolyte, the preparation raw materials comprising:
a solvent comprising ethylene carbonate, propylene carbonate, and methyl ethyl carbonate;
a lithium salt comprising lithium bis (trifluoromethanesulfonyl) imide; in the electrolyte, the molar concentration of the lithium salt is 1.6-2.5M;
additives including lithium carbonate, lithium silicate, cyclohexane and tris (pentafluorophenyl) borane.
According to a preferred embodiment of the application, there is at least the following advantageous effect:
1. at low temperature, the impedance of the electrolyte body is increased due to the reduction of the conductivity, and meanwhile, the impedance of the SEI film and the charge transfer impedance are also obviously increased, so that the electrode polarization is increased and the low-temperature performance of the battery is reduced;
the ethylene carbonate adopted by the application has better film forming property, the propylene carbonate has low melting point, is a good low-temperature cosolvent, and the methyl ethyl carbonate has low viscosity, so that the mixed solvent has good film forming property, low-temperature co-melting property and lower viscosity; thus ensuring a low resistance of the electrolyte at low temperatures.
2. The lithium bistrifluoromethylsulfonylimide can effectively disperse negative charges in ions due to the strong electron-withdrawing property of perfluoroalkyl groups, reduce coulomb effect between anions and cations, and enlarge the liquid range of the system. Meanwhile, the electrolyte has lower lattice energy, and can obviously reduce the melting point of a system, so that the electrochemical performance of the electrolyte at low temperature can be improved.
3. When Li 2 SiO 3 When deposited on the surface of an electrode, it has excellent electrochemical stability and electronic insulation and is possible to protect the electrolyte from oxidative decomposition, lithium carbonate Li 2 CO 3 Is one of the effective components of SEI film, is an insulator of electrons and a good medium for transferring lithium ions, li 2 CO 3 The particles cover the electrode surface to form a protective layer, which can inhibit the decomposition of the electrolyte.
4. The wettability of the electrolyte to the diaphragm and the electrode can be improved by adding cyclohexane, the interface impedance is reduced, and the rate capability is improved.
5. The tris (pentafluorophenyl) borane as an anion receiver can promote stability of an SEI film and reduce impedance of the SEI film, and can promote cycle performance of a lithium bistrifluoromethane sulfonyl imide battery. Meanwhile, the migration of anions in the electrolyte can be inhibited, and the migration number of lithium ions in the electrolyte is improved. The capacity of the diaphragm for storing electrolyte can be obviously improved through the interaction between the tri (pentafluorophenyl) borane TPFPB and the mixed solvent.
In some embodiments of the application, the ratio of the ethylene carbonate, the propylene carbonate, and the methyl ethyl carbonate, in parts by volume, is 100:25 to 600: 100-700 parts.
In some embodiments of the application, the ratio of the ethylene carbonate, the propylene carbonate, and the methyl ethyl carbonate, in parts by volume, is 100: 250-500: 100-700 parts.
In some embodiments of the application, the additive comprises 1 to 5% by mass of the electrolyte.
In some embodiments of the application the mass ratio of the tris (pentafluorophenyl) borane to the cyclohexane is 1:1 to 6.
The second aspect of the application provides a preparation method of the electrolyte, which comprises the steps of mixing the solvent under a protective atmosphere, dissolving the lithium salt and the additive into the solvent, and mixing.
In some embodiments of the application, the protective atmosphere conditions are selected from argon or nitrogen.
In some embodiments of the application, the temperature of the mixing is 50 to 70 ℃.
In a third aspect, the present application provides a secondary battery, the preparation raw material comprising the electrolyte.
A fourth aspect of the present application provides the use of a secondary battery in the field of power batteries, energy storage batteries and consumer electronics batteries.
Detailed Description
The conception and the technical effects produced by the present application will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present application. It is apparent that the described embodiments are only some embodiments of the present application, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present application based on the embodiments of the present application.
Example 1
The embodiment prepares an electrolyte, which comprises the following specific processes:
s1: mixing Ethylene Carbonate (EC), propylene Carbonate (PC) and methyl ethyl carbonate (EMC);
s2: and adding lithium bistrifluoro methanesulfonimide, lithium carbonate accounting for 0.3 percent of the mass of the electrolyte, lithium silicate accounting for 0.3 percent of the mass of the electrolyte, cyclohexane and tris (pentafluorophenyl) borane into the mixture obtained in the step S1, and uniformly mixing to obtain the electrolyte.
Examples 2 to 4
An electrolyte was prepared separately, the preparation method, the content of lithium carbonate and the content of lithium silicate were the same as in example 1, and they were different from example 1 only in the proportion of some of the raw materials for preparation, and the specific proportions are shown in table 1.
Table 1 composition of the electrolyte provided in examples and comparative examples
The additive proportion wt% refers to the mass of the additive in the electrolyte.
Comparative example 1
This comparative example produced an electrolyte, which differs from example 1 in particular in that:
the electrolyte comprises the following components: the complex solvent in step S1 of example 1 was replaced with methyl ethyl carbonate.
Comparative example 2
An electrolyte was prepared in this comparative example, and the specific difference from example 1 was that:
the electrolyte comprises the following components: the cyclohexane of example 1 was not added in step S2.
Comparative example 3
This comparative example prepared an electrolyte, the preparation method being different from example 1 in that:
the electrolyte comprises the following components: the lithium carbonate of example 1 was not added in step S2.
Test examples
The test example tests the performance of the button cell prepared in the application example. Wherein:
the application example provides a lithium ion secondary battery, in particular:
positive electrode active material (NCM 851005), binder (polyvinylidene fluoride, PVDF) and conductive agent (acetylene black) in a mass ratio of 96:2:2;
negative electrode active material: a graphite-based carbon material;
battery size: 2025 type button cell.
In the test of cycle performance: the voltage range is 2.8-4.25V; the first week adopts 0.1C multiplying power charge and discharge, and the rest cycles adopt 1C multiplying power charge and discharge; the test temperature is controlled to be 22-26 ℃; the first week discharge capacity was recorded, as well as the capacity retention after 200 weeks of cycling.
In the test of rate performance: the voltage range is 2.8-4.25V; the current multiplying power is sequentially 0.1C, 0.5C, 1C, 2C and 5C, and each multiplying power circulates for 5 weeks; recording the ratio of the discharge capacity at each multiplying power to the first-week discharge capacity;
in the high-low temperature performance test: the test voltage is 2.8-4.25V; firstly, activating at 25 ℃ for 3 weeks at 0.1C, then, firstly, circulating at-10 ℃ for 50 weeks at 1C multiplying power (low temperature), then, heating to 65 ℃, and performing charge-discharge circulation at 1C for 50 weeks (high temperature); recording capacity retention after 50 weeks of cycling;
safety performance test: after charging to 4.25V, the positive electrode and the negative electrode of the button cell are forced to be short-circuited, then charging is carried out again, after the cycle is carried out for 5 times in sequence, whether a cell failure signal such as obvious short circuit appears on a charging curve or not is observed.
5 parallel tests were performed for each test; the test results are shown in Table 2.
Table 2 electrochemical performance results of lithium ion batteries obtained in application examples
The lithium ion secondary batteries containing the electrolytes of examples 1 to 4 of the present application have superior rate performance, safety performance and low temperature performance. In comparative example 1, the mixed solvent of the present application is not included, so that the conductivity is reduced, the impedance of the electrolyte body is increased, and the impedance of the SEI film and the charge transfer impedance are also obviously increased, so that the electrode polarization is increased and the low-temperature performance of the battery is reduced; the cyclohexane of the present application was not included in comparative example 2, so that the wettability of the electrolyte to the separator and the electrode was lowered, the interface resistance was increased, the rate performance was lowered, and the lithium carbonate of the present application was not included in comparative example 3, so that the stability performance of the corresponding battery was lowered.
The present application is not limited to the above-described embodiments, and various changes may be made within the knowledge of one of ordinary skill in the art without departing from the spirit of the present application. Furthermore, embodiments of the application and features of the embodiments may be combined with each other without conflict.
Claims (6)
1. An electrolyte is characterized by comprising the following raw materials:
a solvent, wherein the solvent is ethylene carbonate, propylene carbonate and methyl ethyl carbonate;
a lithium salt, wherein the lithium salt is lithium bis (trifluoromethanesulfonyl) imide; in the electrolyte, the molar concentration of the lithium salt is 1.6M;
additives, which are lithium carbonate, lithium silicate, cyclohexane and tris (pentafluorophenyl) borane;
the proportion of the ethylene carbonate, the propylene carbonate and the methyl ethyl carbonate is 1:3:1, a step of;
the additive accounts for 1 percent of the electrolyte by mass;
the mass ratio of the tris (pentafluorophenyl) borane to the cyclohexane is 1:2.
2. the method for preparing an electrolyte according to claim 1, comprising mixing the solvent under a protective atmosphere, and then mixing the lithium salt and the additive with the solvent.
3. The method of claim 2, wherein the protective atmosphere conditions are selected from argon or nitrogen.
4. The method according to claim 2, wherein the temperature of the mixing is 50-70 ℃.
5. A secondary battery, wherein the preparation raw material comprises the electrolyte prepared by the preparation method according to any one of claims 2 to 4.
6. Use of the secondary battery according to claim 5 in the field of power batteries, in the field of energy storage batteries and in the field of consumer electronics batteries.
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| "锂离子电池高压电解液成膜添加剂及溶剂的研究";韩占立;《中国优秀硕士学位论文全文数据库（电子期刊） 工程Ⅱ辑》(第2019年第01期);第三章 3.3节结果与讨论 * |
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