CN108206299B - Lithium ion battery and electrolyte thereof - Google Patents
Lithium ion battery and electrolyte thereof Download PDFInfo
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- CN108206299B CN108206299B CN201611178918.0A CN201611178918A CN108206299B CN 108206299 B CN108206299 B CN 108206299B CN 201611178918 A CN201611178918 A CN 201611178918A CN 108206299 B CN108206299 B CN 108206299B
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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
- H01M10/05—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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- 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 a lithium ion battery electrolyte, comprising lithiumA salt, an organic solvent and an additive, wherein the additive comprises a compound shown in a formula I and a compound shown in a formula II, and the structural formula of the additive is shown as follows:
wherein n is 1-9, R1、R2、R3Independently selected from a halogen atom, a phenyl group, an alkane group with 0-9 carbon atoms completely or partially substituted by a halogen atom, and a cyclic alkyl group with 0-9 carbon atoms completely or partially substituted by a halogen atom; r4、R5、R6、R7At least one of which is selected from F, Br or Cl. Compared with the prior art, the compound of the formula I and the compound of the formula II are added into the electrolyte as additives, so that the problem of high-temperature gas generation of the lithium ion battery can be obviously solved, the cycle storage performance of the lithium ion battery is improved, and the lithium ion battery has good application value. The invention also discloses a lithium ion battery.
Description
Technical Field
The invention belongs to the field of new energy materials, and particularly relates to a lithium ion battery and an electrolyte thereof, wherein the lithium ion battery improves the problem of high-temperature gas production and has good storage performance.
Background
Lithium ion batteries have the advantages of high specific energy, high working voltage, wide application temperature range, low self-discharge rate, long cycle life, no pollution, good safety performance and the like, are widely researched and applied to mobile electronic devices such as mobile phones, portable computers, video cameras, cameras and the like in recent years, and gradually replace traditional batteries in the fields of aviation, aerospace, navigation, artificial satellites, small medical instruments and military communication equipment.
In the modern times, the pursuit of high energy density of lithium ion batteries has become a great trend, and at present, the improvement of the working voltage of a positive electrode material, the use of a high-gram-capacity high-nickel material and the use of a negative electrode material with higher discharge capacity are commonly used respectively. The oxidation of the anode high-nickel material in a lithium-removed state is obviously enhanced along with the increase of the nickel content, and the electrolyte is easily oxidized and decomposed on the surface of the lithium-removed high-nickel material, so that the cycle life of the battery cell is shortened, and great challenge is provided for the current electrolyte. The silicon material has a theoretical specific capacity far higher than that of the graphite negative electrode material, and has huge volume expansion in the circulation process, and in addition, a Solid Electrolyte Interface (SEI) film of the negative electrode is broken in the circulation process, so that the electrolyte is reduced and decomposed, a large amount of byproducts are generated, and the circulation performance is deteriorated. Particularly, when the fully charged battery is used or stored at a high temperature, the activity of the reaction between the positive electrode and the negative electrode and the electrolyte is further enhanced, the reaction heat release is greatly increased, a large amount of gas is generated, the volume expansion of the battery is caused, and the short circuit in the battery can be caused in a serious case.
In view of the above, it is necessary to provide a lithium ion battery and an electrolyte thereof with improved high temperature gas generation and good cycle storage performance.
Disclosure of Invention
The invention aims to: the lithium ion battery and the electrolyte thereof have the advantages of overcoming the problem of serious high-temperature gas production of the conventional lithium ion battery and improving the high-temperature gas production problem and have good storage performance.
In order to achieve the above object, the present invention provides an electrolyte for a lithium ion battery, comprising a lithium salt, an organic solvent and an additive, wherein the additive comprises a compound of formula I and a compound of formula II, and the structural formula of the additive is as follows:
wherein n is 1-9, R1、R2、R3Independently selected from a halogen atom, a phenyl group, an alkane group with 0-9 carbon atoms completely or partially substituted by a halogen atom, and a cyclic alkyl group with 0-9 carbon atoms completely or partially substituted by a halogen atom; r4、R5、R6、R7At least one of which is selected from F, Br or Cl.
As an improvement of the electrolyte of the lithium ion battery, the compound shown in the formula II is fluoroethylene carbonate, 1, 2-difluoroethylene carbonate or chloroethylene carbonate; the structural formulas of fluoroethylene carbonate, 1, 2-difluoroethylene carbonate and chloroethylene carbonate are as follows:
as an improvement of the lithium ion battery electrolyte, the compound shown in the formula I accounts for 0.01-5% of the total mass of the lithium ion battery electrolyte. When the content of the compound in the formula I in the electrolyte is too low, the additive cannot form a compact SEI film on the positive electrode, and the high-temperature storage gas production of a system is not obviously improved; when the content of the compound of formula I is too high, the interfacial resistance of the surface of the positive electrode is significantly increased due to the formation of an excessively thick SEI film, and the 25 c 45 c cycle performance of the battery is also deteriorated.
As an improvement of the lithium ion battery electrolyte, the compound shown in the formula I accounts for 0.1-3% of the total mass of the lithium ion battery electrolyte.
As an improvement of the lithium ion battery electrolyte, the compound shown in the formula II accounts for 0.5-30% of the total mass of the lithium ion battery electrolyte. The content of the compound of formula II is related to the negative electrode material composition and content: when the content of the compound in the formula II in the electrolyte is too low, an active interface of a negative electrode can be caused, particularly, active particles of the negative electrode can not be effectively protected in a silicon-based negative electrode system, and then a large amount of side reactions can occur, for example, a large amount of reducing gas is generated to destroy the stability of the interface, so that the cycle performance of a battery cell is aggravated; on the contrary, when the content of the formula II compound in the electrolyte is too high, particularly at high temperature, during the charging and discharging processes of the lithium battery, the high nickel material in a strong oxidation state contacts with the electrolyte to generate an oxidative decomposition reaction, and the generated by-products, such as HF, can cause the damage of the structure of the positive electrode material and also deteriorate the cycle performance of the lithium battery.
As an improvement of the lithium ion battery electrolyte of the present invention, the additive further includes a cyclic ester compound containing a sulfur-oxygen double bond, such as: vinyl sulfate, and the like. The method has the effects of further improving the storage performance of the lithium battery and improving the cycle performance of the lithium battery to a certain extent.
As an improvement of the electrolyte of the lithium ion battery of the present invention, the lithium saltIs a routine choice, optionally, including but not limited to LiPF6、LiBF4、LiN(SO2F)2、LiN(CF3SO2)2、LiClO4、LiAsF6、LiB(C2O4)2、LiBF2(C2O4)、LiN(SO2RF)2、LiN(SO2F)(SO2RF) Wherein R isFIs Cn′F2n′+1And n' is 1 to 10.
As an improvement of the lithium ion battery electrolyte, the lithium salt accounts for 6.25-25% of the total mass of the lithium ion battery electrolyte.
As an improvement of the lithium ion battery electrolyte, the organic solvent can be selected according to actual requirements, and is preferably a non-aqueous organic solvent, such as a compound having 1-8 carbon atoms and containing at least one ester group.
As an improvement of the electrolyte of the lithium ion battery, the organic solvent is one or more of ethylene carbonate, propylene carbonate, butylene carbonate, pentylene carbonate, fluoroethylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate and methyl ethyl carbonate, and can also be one or more of halogenated derivatives of the above compounds.
In order to achieve the above object, the present invention further provides a lithium ion battery, including a positive electrode, a negative electrode, a separator, and an electrolyte, where the electrolyte includes a lithium salt, an organic solvent, and an additive, and the additive includes a compound of formula I and a compound of formula II, and its structural formula is as follows:
wherein n is 1-9, R1、R2、R3Independently selected from a halogen atom, a phenyl group, an alkane group with 0-9 carbon atoms completely or partially substituted by a halogen atom, and a cyclic alkyl group with 0-9 carbon atoms completely or partially substituted by a halogen atom; r4、R5、R6、R7At least one of which is selected from F, Br or Cl.
Compared with the prior art, the lithium ion battery and the electrolyte thereof have the following characteristics:
according to the electrolyte containing the compound of the formula I and the compound of the formula II, the compound of the formula II can form a compact and high-toughness Solid Electrolyte Interface (SEI) film on a negative electrode, so that the cycle performance of a lithium ion battery is improved, and meanwhile, the problem of gas generation in the battery is serious; by introducing the compound of the formula I, the polymerization reaction can be effectively carried out on the positive electrode interface and a compact and uniform SEI film is formed, the contact between the high-oxidation-state positive electrode material and the electrolyte in the charging and discharging processes of the lithium battery is effectively isolated, the problem of serious gas generation caused by the compound of the formula II is solved, the corrosion damage of hydrofluoric acid (HF) to the negative electrode is prevented, and the positive electrode interface and the negative electrode interface of the lithium battery are stable. Particularly, the electrolyte system containing the compounds of the formula I and the formula II is applied to a high-energy-density high-nickel/silicon negative electrode lithium ion battery system, and the gas production inhibition effect is obvious. In addition, the vinyl sulfate compound is matched with the compounds in the formula I and the formula II for use, so that the defect of serious gas generation in high-temperature storage of the lithium battery is overcome, the electrode interface of the lithium battery is ensured to be stable, the cycle performance of the lithium battery is not affected, the cycle residual capacity of the lithium battery is effectively improved, and the lithium battery has good electrochemical performance.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present invention clearer, the present invention is further described in detail with reference to the following embodiments. It should be understood that the examples described in this specification are for the purpose of illustration only and are not intended to limit the invention, and the formulation, proportions, etc. of the examples may be selected appropriately without materially affecting the results.
Example 1
The lithium ion batteries (batteries for short) S1 are prepared according to the following method:
(1) preparation of positive plate
Lithium nickel cobalt manganese oxide (LiNi)0.8Co0.1Mn0.1O2) Mixing a binder (polyvinylidene fluoride) and a conductive agent (conductive carbon black) according to a weight ratio of 98:1:1, adding N-methylpyrrolidone (NMP), and stirring under the action of a vacuum stirrer until the system becomes uniform and transparent to obtain anode slurry; uniformly coating the positive electrode slurry on an aluminum foil with the thickness of 12 mu m; and (3) airing the aluminum foil at room temperature, transferring the aluminum foil to a 120 ℃ oven for drying for 1h, and then performing cold pressing and slitting to obtain the positive plate.
(2) Preparation of negative plate
Mixing a silicon-carbon compound, a conductive agent (conductive carbon black) and a binding agent polyacrylate according to a weight ratio of 98:1:1, adding deionized water, and stirring in a vacuum stirrer to obtain negative electrode slurry; uniformly coating the negative electrode slurry on a copper foil; and (3) airing the copper foil at room temperature, transferring the copper foil to a 120 ℃ oven for drying for 1h, and then performing cold pressing and slitting to obtain the negative plate.
(3) Preparation of the electrolyte
In a drying room, EC and DEC which are subjected to rectification dehydration purification treatment are uniformly mixed to form an organic solvent, a fully dried lithium salt is dissolved in the organic solvent, and then lithium salt LiPF is added into the organic solvent6And the additive is 8 wt% of fluoroethylene carbonate and 0.5 wt% of propylene trifluoroacetate, and the electrolyte is obtained by uniformly mixing. Wherein the concentration of the lithium salt is 1mol/L, the content of the lithium salt is 12.5 percent of the total mass of the electrolyte, and the weight ratio of EC, EMC and DEC is EC: EMC: DEC: 1: 1.
(4) Preparation of lithium ion battery
Stacking the conventionally cut positive plate, the conventionally cut negative plate and the lithium battery isolation film in sequence to enable the lithium battery isolation film to be positioned between the positive plate and the negative plate to play an isolation role, and then winding to obtain a bare cell; and (3) placing the bare cell in an outer packaging foil, injecting the prepared electrolyte into the dried battery, and performing vacuum packaging, standing, formation, shaping and other processes to obtain the lithium ion battery (S1 for short).
Examples 2 to 19(S2 to S19) and comparative examples 1 to 8(D1 to D8) were prepared in the same manner as example 1, except that the additives in the electrolyte, the types and contents of the additives in detail, are shown in Table 1.
TABLE 1 kinds and amounts of electrolyte additives in comparative examples 1 to 8 and examples 1 to 19
Note: in Table 1, "-" indicates that no substance was added.
Performance testing
Cycle testing of lithium ion batteries at 25 ℃ and 45 ℃
The batteries obtained in comparative examples 1 to 8 and examples 1 to 19 were subjected to the following tests, respectively: the method comprises the steps of charging a battery to 4.2V at a constant current of 1C at 25 ℃ and 45 ℃ respectively, then charging at a constant voltage until the current is 0.05C, and then discharging at a constant current of 1C to 2.8V, wherein the first cycle is realized, the battery is circulated for multiple times according to the conditions, and the capacity retention rates of the battery after 200 times, 400 times and 600 times of circulation are respectively calculated, wherein the capacity retention rates after circulation are calculated according to the following formula, and relevant test data refer to tables 2 and 3.
Capacity retention after cycling ═ 100% (discharge capacity corresponding to cycling/discharge capacity of the first cycle).
TABLE 2 Cyclic Capacity Retention ratios at 25 ℃ of the batteries obtained in comparative examples 1 to 8 and examples 1 to 19
TABLE 3 Cyclic Capacity Retention ratios at 45 ℃ of the batteries obtained in comparative examples 1 to 8 and examples 1 to 19
Storage test of lithium ion battery at 80 DEG C
The following tests were performed on the batteries S1 to S19 and the batteries D1 to D8, respectively:
charging the lithium ion battery to 4.2V at room temperature at a constant current of 1C, then charging at a constant voltage of 4.2V to a current of 0.05C, and testing the volume V of the battery0(ii) a Then the lithium ion battery is placed into a constant temperature box with the temperature of 80 ℃, the lithium ion battery is stored for 10 days, and the volume of the test battery is taken out on the nth day and is recorded as VnThe volume expansion rate of the lithium ion battery at the 10 th day is calculated by the following formula, and the results are shown in table 4.
Volume expansion rate (%) after high-temperature storage of lithium ion battery for n days is (V)n-V0)/V0× 100%, where n is the number of days of high temperature storage of the lithium ion battery.
TABLE 4 storage volume expansion at 80 ℃ of the batteries obtained in comparative examples 1 to 8 and examples 1 to 19
As can be seen from tables 2 and 3, the batteries S1 to S5 and S8 to S19, to which the additives of formula I and formula II were added simultaneously, had substantially the same capacity retention rates at cycles of 25 and 45 ℃, as compared with the batteries D2 to D3, to which the compound of formula II was added alone; however, compared with the batteries only added with the compounds of the formula I from D5 to D8, the capacity retention rate of the batteries at 25 and 45 ℃ is obviously higher. This shows that the introduction of a reasonable amount of the compound of formula I in a sufficient amount of the compound of formula II as a film forming additive for silicon negative electrodes does not greatly affect the cycle performance of lithium batteries at 25 ℃ and 45 ℃.
As can be seen from Table 4, the batteries S1-S19, in which the compounds of formula I and formula II were simultaneously added as additives to the electrolyte, both had a low volume expansion rate after storage at high temperatures. It can be seen from S1-S5, S8 and S19 that the combination of the compound of formula I (including the mixture) and the compound of formula II can well solve the problem of serious gas generation caused by the film-forming additive (the compound of formula II). Along with the increase of the content of the compound of the formula I, the gas generation at high temperature of the battery is effectively inhibited; when the content of the compound in the formula I reaches 5 percent, the inhibition effect of gas production tends to be flat. However, when the amount of formula I added is too high (S6,6 wt%), an SEI film is formed too thick on the negative electrode, DCR of the battery is increased, normal and high temperature cycles are deteriorated, and electrochemical performance of the battery is greatly reduced.
The amount of the negative electrode film forming agent (the compound of the formula II) is related to the negative electrode material component of a battery design system, and for a battery with high energy density design, for example, the negative electrode active material is selected from silicon and silicon materials, the higher the content of the active material is, the more the amount of the film forming additive (the compound of the formula II) is needed. When the content of the compound of formula II in the electrolyte is too high, particularly at high temperature, during the charging and discharging processes of the lithium battery, the high nickel material in a strong oxidation state contacts with the electrolyte to generate an oxidative decomposition reaction, and the generated by-products, such as HF, can damage the structure of the positive electrode material and also deteriorate the cycle performance of the lithium battery. In the electrolyte system, the S3, the S8, the S9 and the S14-S19 show that the addition of the compounds of the formula I and the formula II can form a stable SEI film when more and less additives of the formula II are added into the electrolyte system, the gas generation problem can be effectively inhibited by the addition of the compounds of the formula I, the cycle performance of the lithium battery at 25 ℃ and 45 ℃ is the same, and the gas generation problem of high-temperature storage is also effectively inhibited.
In addition, the additive C (vinyl sulfate) is combined with the compounds of the formula I, the formula II and the like, so that the electrochemical properties of the cell, such as the cycle performance, the capacity storage and the like, can be further improved. In conclusion, the compound shown in the formula I is used as a gas production inhibitor, the compound shown in the formula II is used as a film forming agent, and the compound is jointly applied to the electrolyte, so that the storage and gas production problems of the lithium ion battery at the high temperature of 80 ℃ can be remarkably improved on the basis that the cycle performance of the prepared lithium ion battery at the temperature of 25 ℃ and 45 ℃ is consistent with the original level.
Appropriate changes and modifications to the embodiments described above will become apparent to those skilled in the art from the disclosure and teachings of the foregoing description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (8)
1. A lithium ion battery electrolyte comprises a lithium salt, an organic solvent and an additive, wherein the additive comprises a compound of formula I and a compound of formula II, wherein the compound of formula I has a structural formula shown as follows:
wherein n is 1-9, R1、R2、R3Independently selected from a halogen atom, a phenyl group, an alkane group with 0-9 carbon atoms completely or partially substituted by a halogen atom, and a cyclic alkyl group with 0-9 carbon atoms completely or partially substituted by a halogen atom;
the compound of formula II is:
2. the lithium ion battery electrolyte of claim 1, wherein the compound of formula I accounts for 0.01-5% of the total mass of the lithium ion battery electrolyte.
3. The lithium ion battery electrolyte of claim 2, wherein the compound of formula I accounts for 0.1-3% of the total mass of the lithium ion battery electrolyte.
4. The lithium ion battery electrolyte of claim 1, wherein the compound of formula II accounts for 0.5-30% of the total mass of the lithium ion battery electrolyte.
5. The lithium ion battery electrolyte of claim 1 wherein the additive further comprises a cyclic ester compound containing a sulfur-oxygen double bond.
6. The lithium ion battery electrolyte of claim 1, wherein the lithium salt is LiPF6、LiBF4、LiN(SO2F)2、LiN(CF3SO2)2、LiClO4、LiAsF6、LiB(C2O4)2、LiBF2(C2O4)、LiN(SO2RF)2、LiN(SO2F)(SO2RF) Wherein R isFIs Cn′F2n′+1And n' is 1 to 10.
7. The lithium ion battery electrolyte of claim 1, wherein the organic solvent is a non-aqueous organic solvent.
8. A lithium ion battery comprises a positive electrode, a negative electrode, a separation film and an electrolyte, and is characterized in that the electrolyte is the lithium ion battery electrolyte of any one of claims 1 to 7.
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| CN201611178918.0A CN108206299B (en) | 2016-12-19 | 2016-12-19 | Lithium ion battery and electrolyte thereof |
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| CN111540870A (en) * | 2020-05-08 | 2020-08-14 | 中航锂电技术研究院有限公司 | Diaphragm, preparation method and lithium ion battery |
| CN115732756B (en) * | 2021-08-30 | 2023-11-28 | 张家港市国泰华荣化工新材料有限公司 | Electrolyte and secondary battery using same |
| CN116190794A (en) * | 2023-04-27 | 2023-05-30 | 广州天赐高新材料股份有限公司 | Nonaqueous electrolyte and lithium ion battery containing same |
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| CN101682084A (en) * | 2007-06-07 | 2010-03-24 | 株式会社Lg化学 | Non-aqueous electrolyte solution for lithium ion secondary battery and lithium ion secondary battery having the same |
| CN103477492A (en) * | 2011-04-11 | 2013-12-25 | 宇部兴产株式会社 | Non-aqueous electrolyte solution and electricity-storage device using same |
| CN103597648A (en) * | 2011-06-08 | 2014-02-19 | 株式会社Lg化学 | Non-aqueous electrolyte and lithium secondary battery using same |
| CN105914401A (en) * | 2016-06-27 | 2016-08-31 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery containing same |
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| CN103730688B (en) * | 2014-01-09 | 2016-06-08 | 宁德新能源科技有限公司 | Lithium ion battery and electrolyte thereof |
| CN104269576B (en) * | 2014-10-09 | 2017-09-22 | 东莞新能源科技有限公司 | A kind of electrolyte and the lithium ion battery using the electrolyte |
| CN105355975B (en) * | 2015-10-20 | 2018-08-21 | 宁德新能源科技有限公司 | electrolyte and lithium ion battery including the electrolyte |
| CN105742707B (en) * | 2016-04-08 | 2018-08-14 | 深圳新宙邦科技股份有限公司 | A kind of electrolyte for lithium ion battery and lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101682084A (en) * | 2007-06-07 | 2010-03-24 | 株式会社Lg化学 | Non-aqueous electrolyte solution for lithium ion secondary battery and lithium ion secondary battery having the same |
| CN103477492A (en) * | 2011-04-11 | 2013-12-25 | 宇部兴产株式会社 | Non-aqueous electrolyte solution and electricity-storage device using same |
| CN103597648A (en) * | 2011-06-08 | 2014-02-19 | 株式会社Lg化学 | Non-aqueous electrolyte and lithium secondary battery using same |
| CN105914401A (en) * | 2016-06-27 | 2016-08-31 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery containing same |
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