CN111326796B - High-temperature lithium ion battery electrolyte and lithium ion battery - Google Patents
High-temperature lithium ion battery electrolyte and lithium ion battery Download PDFInfo
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- CN111326796B CN111326796B CN202010156808.4A CN202010156808A CN111326796B CN 111326796 B CN111326796 B CN 111326796B CN 202010156808 A CN202010156808 A CN 202010156808A CN 111326796 B CN111326796 B CN 111326796B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0567—Liquid materials characterised by the additives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a high-temperature lithium ion battery electrolyte which comprises lithium salt, an organic solvent and an additive, wherein the additive comprises an oxalato lithium borate compound shown as a formula I, wherein R is1And R2One of them is-PO2F2And the other is-F; or R1And R2Are all-PO2F2. In addition, the invention also relates to a lithium ion battery. Compared with the prior art, the electrolyte disclosed by the invention improves the high-temperature storage performance and the cycle performance of the lithium ion battery.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a high-temperature lithium ion battery electrolyte and a lithium ion battery.
Background
With the rise of the electronic consumer market in recent years, more and more electronic manufacturers and consumers have higher requirements on the high-temperature cycle and high-temperature storage performance of lithium ion batteries, especially in the recent hot bluetooth headset market and the mobile phone market. However, the lithium ion battery is easy to generate flatulence under a high-temperature working environment (45-90 ℃), can generate spontaneous combustion seriously, and causes immeasurable damage to the personal safety of a user.
The main reasons for the poor high-temperature performance of the lithium ion battery are as follows: 1) the electrolyte is oxidized and decomposed on the surface of the positive electrode material. The oxidation activity of the anode active material is high, and the reaction between the anode active material and the electrolyte is further intensified under the high-temperature condition, so that the oxidation product of the electrolyte is continuously deposited on the surface of the anode, and the internal resistance and the thickness of the battery are continuously increased. 2) And dissolving out and reducing metal ions in the crystal lattice of the positive electrode material. In one aspect, LiPF in electrolyte at high temperature6Is easy to useHF generated by decomposition corrodes the active material of the positive electrode, so that metal ions are dissolved out, and metal simple substances are generated on the surface of the negative electrode after transition metal ions penetrate through an SEI film, so that the impedance of the electrode is continuously increased, and the performance of the battery is deteriorated.
In view of the above, it is necessary to provide an electrolyte solution that can effectively improve the problem of poor high-temperature performance of the battery.
Disclosure of Invention
One of the objects of the present invention is: aiming at the defects of the prior art, the high-temperature lithium ion battery electrolyte is provided, and the storage performance and the cycle performance of the lithium ion battery in a high-temperature environment (45-90 ℃) are improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-temperature lithium ion battery electrolyte comprises lithium salt, an organic solvent and an additive, wherein the additive comprises a lithium oxalato borate compound shown as a formula I,
wherein R is1And R2One of them is-PO2F2And the other is-F; or R1And R2Are all-PO2F2。
Specifically, the additive comprises
And/or
As an improvement of the high-temperature lithium ion battery electrolyte, the mass of the lithium oxalato borate compound accounts for 0.1-15% of the total mass of the electrolyte. Preferably, the mass of the lithium oxalato borate compound accounts for 0.1-3% of the total mass of the electrolyte. When the content of the lithium oxalato borate compound is too low, a dense, thin and uniform protective film is difficult to be sufficiently formed on the surface of the positive electrode, so that the oxidative decomposition reaction of the metal ion catalytic electrolyte cannot be effectively inhibited; when the content of the lithium oxalato-borate compound is too high, lithium difluorophosphate generated by the reaction cannot be well dissolved in the electrolyte.
As an improvement of the high-temperature lithium ion battery electrolyte, the additive also comprises at least one of vinylene carbonate, ethylene carbonate and fluoroethylene carbonate. The performance of the SEI film formed by the fluoroethylene carbonate is good, a compact structure layer can be formed, the impedance is not increased, the electrolyte can be effectively prevented from being further decomposed, and the low-temperature performance of the electrolyte is improved. Because vinylene carbonate has good high-low temperature performance and an anti-ballooning function, the vinylene carbonate is commonly used as a novel organic film forming additive and an overcharge protection additive of a lithium ion battery, and can improve the capacity and prolong the cycle life of the battery.
As an improvement of the high-temperature lithium ion battery electrolyte, the additive also comprises at least one of 1, 3-propane sultone, 1, 4-butane sultone, 1, 3-propylene sultone, succinonitrile, adiponitrile, ethylene glycol dipropionitrile ether and 1,3, 6-hexane tricarbonitrile. After the 1, 3-propylene sultone is added into the electrolyte, a solid electrolyte liquid phase interface film can be formed on the surface of a battery electrode, so that co-intercalation and reductive decomposition of solvent molecules at a negative electrode are inhibited, and the cycle performance and the high-temperature performance of the lithium ion battery are improved. The addition of nitrile additives can greatly inhibit LiPF6Reacts with trace acid and water, thereby improving the performance of the battery. However, the resistance of the film formed by the nitrile additive is relatively large, which is detrimental to the high temperature performance of the battery. However, the lithium oxalato borate compound shown in formula I can effectively consume HF generated by SEI formation and LiF causing increase of film resistance, and reduce SEI film resistance, so that the mutual cooperation of the HF and the LiF can effectively improve the high-temperature performance of the battery.
As an improvement of the electrolyte of the high-temperature lithium ion battery, the lithium salt is LiPF6、LiBF4、LiClO4、LiFSI、LiTFSI、LiBOB、LiDFOB、LiFAP、LiSbF6、LiCF3SO3、LiN(SO2CF3)2、LiN(SO2C2F5)2、LiN(SO2CF3)2、LiN(SO2C4F9)2、LiC(SO2CF3)3、LiPF3(C3F7)3、LiB(CF3)4And LiBF3(C2F5) At least one of (1).
As an improvement of the high-temperature lithium ion battery electrolyte, the organic solvent comprises at least one of ethylene carbonate, ethyl methyl carbonate, diethyl carbonate, propylene carbonate, ethyl propionate and propyl propionate.
As an improvement of the high-temperature lithium ion battery electrolyte, the mass of the lithium salt accounts for 12-18% of the total mass of the electrolyte.
The second purpose of the invention is: the lithium ion battery comprises a positive electrode, a negative electrode, a diaphragm arranged between the positive electrode and the negative electrode at intervals, and an electrolyte, wherein the electrolyte is the high-temperature lithium ion battery electrolyte as claimed in any one of claims 1 to 8.
As an improvement of the lithium ion battery of the present invention, the active material of the positive electrode is a ternary material.
Compared with the prior art, the invention at least has the following beneficial effects:
1) the lithium ion battery has the advantages that the main component of the SEI film formed on the surfaces of the positive electrode and the negative electrode comprises LiF, when the LiF is excessive, the impedance of the SEI film is increased, and the adverse effect is caused on the charge and discharge efficiency and long cycle of the lithium ion battery2F2And LiBF4First, the reaction consumes LiF reducing cell impedance; II, reaction of LiPO2F2The complex effect can be generated with transition metal elements in the anode material, and the stability of the anode active material is improved, so that the high-temperature cycle performance of the battery is effectively improved, and the volume expansion of the battery at high temperature is inhibited; thirdly, ODFB (LiBF) generated by the reaction2C2O4) The film forming capability of the electrolyte to the electrode can be enhanced, and the high-temperature performance of the battery is improved. The reaction mechanism of the lithium oxalato borate compound is specifically as follows:
2) the lithium oxalato borate compound added into the electrolyte has a fluorine-containing group, and the fluorine-containing group enables the protective film to show higher thermal stability due to high oxidation stability of the fluorine-containing group.
3) The lithium oxalato borate compound added into the electrolyte can react with H in the electrolyte2O, HF, and removing water and acid.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the embodiments of the present invention are not limited thereto.
In the following comparative examples and examples, the lithium oxalato borate compound used had the following structural formula:
comparative example 1
1) Preparation of positive plate
The positive electrode ternary active material NMC523, the conductive carbon black Super-P, the graphene CNT and the binder polyvinylidene fluoride (PVDF) were mixed in a mass ratio of 97.1:1:0.7:2, and then dispersed in N-methyl-2-pyrrolidone (NMP) to obtain a positive electrode slurry. And uniformly coating the slurry on two sides of the aluminum foil, drying, rolling and vacuum drying, and welding an aluminum outgoing line by using an ultrasonic welding machine to obtain the positive plate, wherein the thickness of the pole piece is 120-150 mu m.
2) Preparation of negative plate
The negative electrode active material artificial graphite, conductive carbon black Super-P, binder Styrene Butadiene Rubber (SBR) and carboxymethyl cellulose (CMC) were mixed in a mass ratio of 97:0.5:1.3:1.2, and then dispersed in ionic water to obtain a negative electrode slurry. Coating the slurry on two sides of the copper foil, drying, rolling and vacuum drying, and welding a nickel outgoing line by using an ultrasonic welding machine to obtain the negative plate, wherein the thickness of the pole piece is 120-150 mu m.
3) Preparation of the electrolyte
Ethylene Carbonate (EC), diethyl carbonate (DEC), Propylene Carbonate (PC) and Propyl Propionate (PP) were mixed in a mass ratio of EC: DEC: PC: PP ═ 2:2:1:5, and then 4.0 wt% PS, 3.5 wt% FEC, 1% SN, 0.5% ODFB and 0.5% FSI by mass were added, respectively, followed by 14.0 wt% lithium hexafluorophosphate (LiPF)6) Fully mixing and dissolving for later use.
4) Preparation of the Battery
Placing an isolating membrane with the thickness of 16 mu m between the positive plate and the negative plate, then winding a sandwich structure consisting of the positive plate, the negative plate and the diaphragm, flattening the wound body, then placing the flattened wound body into an aluminum-plastic film packaging bag, and baking the flattened wound body in vacuum at 80 ℃ for 48 hours to obtain a battery cell to be injected with liquid; respectively injecting the prepared electrolyte into a battery cell in a glove box with the dew point controlled below-40 ℃, carrying out vacuum packaging, standing for 24h, and then carrying out conventional formation and capacity grading according to the following steps: charging at 0.05C for 180min, charging at 0.2C to 3.95V, and vacuum sealing twice; then further charging to 4.2V at a constant current of 0.2C, standing for 24h at normal temperature, and discharging to 3.0V at a constant current of 0.2C; finally, the mixture is charged to 4.2V at a constant current of 0.2C and is put aside for standby.
Example 1
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 0.1 wt% of compound a.
The rest is the same as comparative example 1 and will not be described again.
Example 2
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 0.5 wt% of compound a.
The rest is the same as comparative example 1 and will not be described again.
Example 3
In contrast to comparative example 1: in this example, the electrolyte was further added with the compound a in a mass fraction of 1.0 wt%.
The rest is the same as comparative example 1 and will not be described again.
Example 4
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 1.5 wt% of compound a.
The rest is the same as comparative example 1 and will not be described again.
Example 5
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 2.0 wt% of compound a.
The rest is the same as comparative example 1 and will not be described again.
Example 6
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 2.5 wt% of compound a.
The rest is the same as comparative example 1 and will not be described again.
Example 7
In contrast to comparative example 1: in this example, 3.0 wt% of compound a was also added to the electrolyte.
The rest is the same as comparative example 1 and will not be described again.
Example 8
In contrast to comparative example 1: in this example, the electrolyte was further added with 0.1 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 9
In contrast to comparative example 1: in this example, the electrolyte was further added with 0.5 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 10
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 1.0 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 11
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 1.5 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 12
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 2.0 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 13
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 2.5 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 14
In contrast to comparative example 1: in this example, 3.0 wt% of compound b was added to the electrolyte.
The rest is the same as comparative example 1 and will not be described again.
Example 15
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 2.0 wt% of compound a and a mass fraction of 1.0 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Example 16
In contrast to comparative example 1: in this example, the electrolyte was further added with a mass fraction of 1.0 wt% of compound a and a mass fraction of 2.0 wt% of compound b.
The rest is the same as comparative example 1 and will not be described again.
Performance testing
The following performance tests were performed on the batteries prepared in comparative example 1 and examples 1 to 16:
1) EIS performance test: EIS test is carried out on comparative example 1 and examples 1-16, and the test conditions are as follows: the frequency range is 100 kHz-0.01 Hz, and the amplitude is 10 mV; the tested data were subjected to circuit fitting to obtain SEI impedance, the results of which are shown in table 1.
2) And (3) testing high-temperature cycle performance: the batteries prepared in comparative example 1 and examples 1 to 16 were placed in an oven at a constant temperature of 45 ℃, and were charged to 4.2V at a constant current of 0.2C and then the constant voltage charging current was decreased to 0.02C, and then discharged to 3.0V at a constant current of 0.2C, and the cycle was repeated for 300 weeks, and the discharge capacity per week was recorded, and the capacity retention rate in the high-temperature cycle was calculated according to the following formula: the n-week capacity retention rate is 100% of the n-week discharge capacity/1-week discharge capacity.
The specific results of the above performance tests are shown in table 1.
TABLE 1EIS and high temperature cycling test results
As can be seen from the data in table 1:
1) as is clear from comparison of examples 1 to 16 with comparative example 1, the film formation resistances of the batteries were all reduced by adding the lithium oxalato borate compound additive.
2) By comparing the two lithium oxalato borate compounds, it was found that the more difluorophosphate groups, the less film formation resistance, because the more difluorophosphate groups, the more LiF are consumed by the reaction, and thus the cell resistance can be reduced to a greater extent.
3) When different contents of the lithium oxalato borate compound a were added to the electrolyte, respectively, the battery performance obtained was the most excellent at a content of 2.5% (example 6), and the high and low temperature discharge performance of the other example sample batteries was the second order. Similarly, when different contents of lithium oxalato borate compound b are added to the electrolyte, the battery performance is better when the contents are 2%, 2.5% and 3% (example 12, example 13 and example 14), and the high and low temperature discharge performance of the batteries with other contents is inferior, and the overall performance of example 12, example 13 and example 14 is similar, and example 12 is the best in view of the cost problem.
4) The effect of the combined addition and the single addition of the two lithium oxalato borate compounds of the compound a and the compound b in the same proportion on the performance of the battery is similar.
Variations and modifications to the above-described embodiments may also occur to those skilled in the art, which fall within the scope of the invention as disclosed and taught herein. Therefore, the present invention is not limited to the above-mentioned embodiments, and any obvious improvement, replacement or modification made by those skilled in the art based on the present invention is within the protection scope 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 (10)
1. The high-temperature lithium ion battery electrolyte is characterized in that: comprises lithium salt, organic solvent and additive, wherein the additive comprises lithium oxalato borate compound shown in formula I,
formula I
Wherein R is1And R2One of them is-PO2F2And the other is-F; or R1And R2Are all-PO2F2。
2. The high temperature lithium ion battery electrolyte of claim 1, wherein: the mass of the lithium oxalato borate compound accounts for 0.1-15% of the total mass of the electrolyte.
3. The high temperature lithium ion battery electrolyte of claim 2, wherein: the mass of the lithium oxalato borate compound accounts for 0.1-3% of the total mass of the electrolyte.
4. The high temperature lithium ion battery electrolyte of claim 1, wherein: the additive also includes at least one of vinylene carbonate, ethylene carbonate and fluoroethylene carbonate.
5. The high temperature lithium ion battery electrolyte of claim 1, wherein: the additive also comprises at least one of 1, 3-propane sultone, 1, 4-butane sultone, 1, 3-propene sultone, succinonitrile, adiponitrile, ethylene glycol dipropionitrile ether and 1,3, 6-hexane trinitrile.
6. The high temperature lithium ion battery electrolyte of claim 1, wherein: the lithium salt is LiPF6、LiBF4、LiClO4、LiFSI、LiTFSI、LiBOB、LiDFOB、LiFAP、LiSbF6、LiCF3SO3、LiN(SO2C2F5)2、LiN(SO2CF3)2、LiN(SO2C4F9)2、LiC(SO2CF3)3、LiPF3(C3F7)3、LiB(CF3)4And LiBF3(C2F5) At least one of (1).
7. The high temperature lithium ion battery electrolyte of claim 1, wherein: the organic solvent comprises at least one of ethylene carbonate, ethyl methyl carbonate, diethyl carbonate, propylene carbonate, ethyl propionate and propyl propionate.
8. The high temperature lithium ion battery electrolyte of claim 1, wherein: the mass of the lithium salt accounts for 12-18% of the total mass of the electrolyte.
9. The utility model provides a lithium ion battery, includes anodal, negative pole, interval set up in anodal with diaphragm between the negative pole to and electrolyte, its characterized in that: the electrolyte is the high-temperature lithium ion battery electrolyte as defined in any one of claims 1 to 8.
10. The lithium ion battery of claim 9, wherein: the active substance of the positive electrode is a ternary material.
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| CN107195966A (en) * | 2017-04-26 | 2017-09-22 | 湛江市金灿灿科技有限公司 | The high voltage tertiary cathode material system lithium-ion battery electrolytes that a kind of high/low temperature performance is taken into account |
| CN110506358A (en) * | 2017-03-30 | 2019-11-26 | 三井化学株式会社 | Nonaqueous electrolyte for battery and lithium secondary battery |
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| KR20160029457A (en) * | 2014-09-05 | 2016-03-15 | 에스케이이노베이션 주식회사 | Electrolyte for Lithium Secondary Battery and Lithium Secondary Battery Containing the Same |
| EP3211706A4 (en) * | 2014-10-22 | 2018-07-04 | Mitsui Chemicals, Inc. | Lithium secondary battery |
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| CN110506358A (en) * | 2017-03-30 | 2019-11-26 | 三井化学株式会社 | Nonaqueous electrolyte for battery and lithium secondary battery |
| CN107195966A (en) * | 2017-04-26 | 2017-09-22 | 湛江市金灿灿科技有限公司 | The high voltage tertiary cathode material system lithium-ion battery electrolytes that a kind of high/low temperature performance is taken into account |
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