CN113013486A - Electrolyte and lithium ion battery comprising same - Google Patents

Electrolyte and lithium ion battery comprising same Download PDF

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Publication number
CN113013486A
CN113013486A CN202110212758.1A CN202110212758A CN113013486A CN 113013486 A CN113013486 A CN 113013486A CN 202110212758 A CN202110212758 A CN 202110212758A CN 113013486 A CN113013486 A CN 113013486A
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electrolyte
lithium
performance
lithium ion
ion battery
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母英迪
王龙
王海
李素丽
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Zhuhai Cosmx Battery Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
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  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
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  • Secondary Cells (AREA)

Abstract

The invention provides an electrolyte for a lithium ion battery and the lithium ion battery comprising the electrolyte, wherein 4, 5-dicyano-2-trifluoromethyl imidazole lithium and a nitrile compound are combined to form a stable low-impedance interface film on the surface of a positive plate, so that the decomposition of side reaction of the electrolyte catalyzed by the dissolution of metal ions is inhibited, and the high-temperature storage performance, the high-temperature cycle performance and the safety performance of a battery cell are improved. Meanwhile, the organic germanium compound shown in the formula 1 can participate in film formation on the surfaces of a positive electrode and a negative electrode to form a firm SEI film with high ionic conductivity and low impedance, so that the reductive decomposition of electrolyte on the surface of the negative electrode is effectively inhibited, the chemical and dynamic performance of a negative electrode interface is obviously improved, lithium ions can be efficiently transferred, the low-temperature performance of the battery cell is obviously improved, and the combined use of the three additives is favorable for the battery cell to consider the high-temperature storage performance, the cycle performance, the low-temperature discharge performance and the safety performance.

Description

Electrolyte and lithium ion battery comprising same
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an electrolyte and a lithium ion battery comprising the same.
Background
In recent years, lithium ion batteries have been widely used in the fields of smart phones, tablet computers, smart wearing, electric tools, electric automobiles, and the like. With the wide application of lithium ion batteries, the use environment and demand of consumers for lithium ion batteries are continuously increasing, which requires that the lithium ion batteries have the characteristics of high and low temperature performance. However, the lithium ion battery has potential safety hazard in the use process, and serious safety accidents, fire and even explosion easily occur under some abuse conditions such as high-temperature thermal shock and the like of the battery.
The electrolyte is used as an important component of the lithium ion battery and has great influence on the performance of the battery. In order to solve these problems, safety performance can be improved by adding a flame retardant (such as trimethyl phosphate, etc.) to the electrolyte, but the use of these additives causes severe deterioration of battery performance. Therefore, the development of lithium ion battery electrolyte capable of ensuring safety without affecting the electrochemical performance of the battery is urgently needed at present.
Disclosure of Invention
The invention aims to provide an electrolyte and a lithium ion battery comprising the same, wherein the lithium ion battery has high safety and good high-temperature storage performance, high-temperature cycle performance and low-temperature discharge performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electrolyte comprising a non-aqueous organic solvent, an additive, and a lithium salt; the additive comprises an organic germanium compound shown in a formula 1, 4, 5-dicyano-2-trifluoromethyl imidazole lithium and a nitrile compound;
Figure BDA0002952961070000021
according to the invention, the mass ratio of the sum of the addition amount of the organogermanium compound shown in the formula 1 and the 4, 5-dicyano-2-trifluoromethyl imidazole lithium to the addition amount of the nitrile compound in the electrolyte is 1 (1-10), such as 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9 or 1: 10.
According to the invention, the organogermanium compound of formula 1 is added in an amount of 0.1 wt% to 0.8 wt%, such as 0.2 wt% to 0.5 wt%, for example 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt% or 0.8 wt% of the total mass of the electrolyte.
According to the invention, the lithium 4, 5-dicyano-2-trifluoromethylimidazole is added in an amount of 0.1 to 1 wt.%, such as 0.2 to 0.5 wt.%, for example 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 or 1.0 wt.%, based on the total mass of the electrolyte.
According to the invention, the nitrile compound is added in an amount of 0.5 to 5 wt.%, preferably 1 to 3 wt.%, for example 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.2, 1.5, 1.8, 2, 2.2, 2.5, 2.8, 3, 3.2, 3.5, 3.8, 4, 4.2, 4.5, 4.8 or 5 wt.% of the total mass of the electrolyte.
According to the invention, the nitrile compound is selected from at least one of 1,3,6 hexanetricarbonitrile, 1,3, 5-cyclohexanetricarbonitrile, glycerol trinitrile, 2,3,5, 6-pyrazine tetracarbonitrile and tetracyanoethylene.
According to the invention, the additive further comprises at least one of tris (trimethylsilane) phosphite, tris (trimethylsilyl) borate, trimethylsilylimidazole, lithium bistrifluoromethanesulfonimide, lithium bistrifluorosulfonimide, 1, 3-propanesultone, 1, 3-propene sultone, ethylene sulfite, vinyl sulfate, vinylene carbonate, fluoroethylene carbonate, lithium dioxalate borate, lithium difluorooxalato phosphate and vinyl carbonate, and the addition amount of the additive accounts for 0-10 wt% of the total mass of the electrolyte, such as 0 wt%, 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt% or 10 wt%.
According to the present invention, the non-aqueous organic solvent is selected from a mixture of at least one of cyclic carbonates and at least one of linear carbonates and linear carboxylates, mixed in an arbitrary ratio.
According to the invention, the cyclic carbonate is selected from at least one of ethylene carbonate and propylene carbonate, the linear carbonate is selected from at least one of dimethyl carbonate, diethyl carbonate and ethyl methyl carbonate, and the linear carboxylate is selected from at least one of ethyl propionate, propyl propionate and propyl acetate.
According to the present invention, the lithium salt is selected from at least one of lithium bistrifluoromethylsulfonyl imide, lithium bisfluorosulfonimide and lithium hexafluorophosphate.
According to the invention, the lithium salt is added in an amount of 13 to 20 wt%, for example 13, 14, 15, 16, 17, 18, 19 or 20 wt%, based on the total mass of the electrolyte.
The invention also provides a preparation method of the electrolyte, which comprises the following steps:
mixing a non-aqueous organic solvent, a lithium salt and an additive comprising an organogermanium compound represented by formula 1, 4, 5-dicyano-2-trifluoromethylimidazole lithium and a nitrile compound to prepare the electrolyte.
Illustratively, the method comprises the steps of:
preparing a nonaqueous organic solvent in a glove box filled with argon and qualified in water oxygen content, and then quickly adding a fully dried lithium salt and an additive comprising an organogermanium compound shown in formula 1, 4, 5-dicyano-2-trifluoromethyl imidazole lithium and a nitrile compound into the nonaqueous organic solvent to prepare the electrolyte.
The invention also provides a lithium ion battery which comprises the electrolyte.
According to the invention, the lithium ion battery also comprises a positive plate, a negative plate and a diaphragm arranged between the positive plate and the negative plate; the positive plate comprises a positive current collector and a mixed layer of a positive active material, a conductive agent and a binder coated on the positive current collector; the negative electrode sheet includes a negative electrode current collector and a mixed layer of a negative electrode active material, a conductive agent and a binder coated thereon.
According to the invention, the positive active material is lithium cobaltate or lithium cobaltate subjected to doping coating treatment by one or more elements of Al, Mg, Ti and Zr, or a lithium metal compound with a spinel structure or an olivine structure; the median diameter D of the positive electrode active material5010 to 26 μm, and a specific surface area of 0.1 to 0.4m2/g。
According to the invention, when the positive electrode material is coated, the compacted density of the positive electrode material is 3.9-4.4 mg/cm3。
According to the invention, the negative active material is graphite or a graphite composite material containing 1-15 wt.% SiOx/C or Si/C; the median diameter D of the negative electrode active material508 to 25 μm, and a specific surface area of 0.7 to 5.0m2/g。
According to the invention, when the negative electrode material is coated, the compacted density of the negative electrode material is 1.60-1.85 mg/cm3。
According to the invention, the diaphragm comprises a substrate and a composite layer of inorganic particles and polymers coated on the substrate, and the thickness of the composite layer is 1-5 μm.
According to the present invention, the composite layer of inorganic particles and polymer comprises a mixture of titanium oxide and polyvinylidene fluoride-hexafluoropropylene copolymer.
According to the present invention, the charge cut-off voltage of the lithium ion battery is 4.45V or more.
The invention has the beneficial effects that:
the invention provides an electrolyte for a lithium ion battery and the lithium ion battery comprising the electrolyte, wherein 4, 5-dicyano-2-trifluoromethyl imidazole lithium and a nitrile compound are combined to form a stable low-impedance interface film on the surface of a positive plate, so that the decomposition of side reaction of the electrolyte catalyzed by the dissolution of metal ions is inhibited, and the high-temperature storage performance, the high-temperature cycle performance and the safety performance of a battery cell are improved. Meanwhile, the organic germanium compound shown in the formula 1 can participate in film formation on the surfaces of a positive electrode and a negative electrode to form a firm SEI film with high ionic conductivity and low impedance, so that the reductive decomposition of electrolyte on the surface of the negative electrode is effectively inhibited, the chemical and dynamic performance of a negative electrode interface is obviously improved, lithium ions can be efficiently transferred, the low-temperature performance of the battery cell is obviously improved, and the combined use of the three additives is favorable for the battery cell to consider the high-temperature storage performance, the cycle performance, the low-temperature discharge performance and the safety performance.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Comparative examples 1 to 6 and examples 1 to 11
The lithium ion batteries of comparative examples 1 to 6 and examples 1 to 11 were each prepared according to the following preparation method, except for the selection and addition of additives, and the specific differences are shown in table 1.
(1) Preparation of positive plate
LiCo serving as a positive electrode active material0.998Al0.001Mg0.0005Ni0.0005O2Mixing polyvinylidene fluoride (PVDF) serving as a binder and acetylene black serving as a conductive agent according to a weight ratio of 97:1.5:1.5, adding N-methylpyrrolidone (NMP), and stirring under the action of a vacuum stirrer until a mixed system becomes uniform and flowable anode slurry; uniformly coating the positive electrode slurry on an aluminum foil with the thickness of 9-12 mu m; baking the coated aluminum foil in 5 sections of baking ovens with different temperature gradients, drying the aluminum foil in a baking oven at 120 ℃ for 8 hours, and rolling and cutting to obtain the required positive plate.
(2) Preparation of negative plate
Preparing a graphite negative electrode material with the mass ratio of 96.4%, a conductive carbon black (SP) conductive agent with the mass ratio of 1%, a sodium carboxymethyl cellulose (CMC) dispersing agent with the mass ratio of 1.3% and a Styrene Butadiene Rubber (SBR) binder with the mass ratio of 1.3% into negative electrode slurry by a wet process, coating the negative electrode slurry on the surface of a negative electrode current collector copper foil, drying (the temperature is 85 ℃, the time is 5 hours), rolling and die cutting to obtain a negative electrode sheet.
(3) Preparation of electrolyte
In a glove box filled with argon (moisture)<10ppm, oxygen content<1ppm), Ethylene Carbonate (EC), Propylene Carbonate (PC), dimethyl carbonate (DEC) and Propyl Propionate (PP) were mixed uniformly in a mass ratio of 20:20:10:50, and LiPF in an amount of 14 wt% based on the total mass of the nonaqueous electrolytic solution was slowly added to the mixed solution6And additives (the specific dosage and selection are shown in table 1), and uniformly stirring to obtain the electrolyte.
(4) Preparation of the separator
A polyethylene separator having a thickness of 7 μm was coated with a 2 μm thick composite layer of a mixture of titanium oxide and polyvinylidene fluoride-hexafluoropropylene copolymer.
(5) Preparation of lithium ion battery
Winding the prepared positive plate, the diaphragm and the prepared negative plate to obtain a naked battery cell without liquid injection; placing the bare cell in an outer packaging foil, injecting the prepared electrolyte into the dried bare cell, and performing vacuum packaging, standing, formation, shaping, sorting and other processes to obtain the required lithium ion battery.
TABLE 1 compositions of electrolytes for lithium ion batteries prepared in comparative examples 1 to 6 and examples 1 to 11
Figure BDA0002952961070000061
The lithium ion batteries obtained in the above comparative examples and examples were subjected to electrochemical performance tests, and the following descriptions were made:
(1)45 ℃ cycling experiment:
placing the batteries obtained in the above examples and comparative examples in an environment of (45 +/-2) DEG C, standing for 2-3 hours, when the battery body reaches (45 +/-2) DEG C, keeping the cut-off current of the battery at 0.05C according to 1C constant current charging, standing for 5min after the battery is fully charged, then discharging to the cut-off voltage of 3.0V at 0.7C constant current, recording the highest discharge capacity of the previous 3 cycles as the initial capacity Q, and when the cycles reach the required times, recording the last time of the batteryDischarge capacity Q1The results are reported in Table 2.
The calculation formula used therein is as follows: capacity retention (%) ═ Q1/Q×100％。
(2) High temperature storage at 85 ℃ for 6 hours experiment:
the cells obtained in the above examples and comparative examples were subjected to a charge-discharge cycle test at a charge-discharge rate of 0.5C for 3 times at room temperature, and then charged to a full charge state at a rate of 0.5C, and the maximum discharge capacity Q of the previous 0.5C cycles was recorded2And battery thickness T1. The fully charged cells were stored at 85 ℃ for 6 hours and the cell thickness T after 6 hours was recorded2And 0.5C discharge capacity Q3And calculating to obtain experimental data such as the thickness change rate, the capacity retention rate and the like of the battery stored at high temperature, and recording the results as shown in table 2.
The calculation formula used therein is as follows:
capacity retention (%) ═ Q3/Q2×100％；
Thickness change rate (%) - (T)2-T1)/T1×100％
(3) Low-temperature discharge experiment:
discharging the batteries obtained in the above examples and comparative examples to 3.0V at ambient temperature of 25 + -3 deg.C at 0.2C, and standing for 5 min; charging at 0.7C, changing to constant voltage charging when the voltage at the cell terminal reaches the charging limit voltage, stopping charging until the charging current is less than or equal to the cut-off current, standing for 5 minutes, discharging to 3.0V at 0.2C, and recording the discharge capacity as the normal temperature capacity Q4. Then the battery cell is charged at 0.7C, when the voltage of the battery cell terminal reaches the charging limiting voltage, constant voltage charging is changed, and charging is stopped until the charging current is less than or equal to the cut-off current; after the fully charged battery was left to stand at-10. + -. 2 ℃ for 4 hours, it was discharged to a cut-off voltage of 3.0V at a current of 0.4C, and the discharge capacity Q was recorded5The low-temperature discharge capacity retention rate was calculated and reported in table 2.
The calculation formula used therein is as follows: low-temperature discharge capacity retention (%) ═ Q5/Q4×100％。
(4) Thermal shock test at 130 ℃:
the cells obtained in the above examples and comparative examples were heated at an initial temperature of 25. + -. 3 ℃ by convection or a circulating hot air oven at a temperature change rate of 5. + -. 2 ℃/min to 130. + -. 2 ℃ for 60min, and the test was terminated, and the results of the cell conditions were recorded as shown in Table 2.
TABLE 2 results of experimental tests on batteries obtained in comparative examples 1 to 6 and examples 1 to 9
Figure BDA0002952961070000081
As can be seen from the results of table 2: it can be seen from example 9 and other examples that the battery performance is the best when the ratio of the sum of the addition amounts of the organogermanium compound represented by formula 1 and 4, 5-dicyano-2-trifluoromethylimidazolium lithium to the addition amount of the nitrile compound is in the range of 1 (1 to 10) to the electrolyte.
It can be seen from comparative examples 1 to 6 that the electrolyte solution simultaneously added with the organogermanium compound represented by formula 1, 4, 5-dicyano-2-trifluoromethylimidazolium lithium and the nitrile compound provides a battery having higher safety, high-temperature cycle performance, high-temperature storage performance and low-temperature discharge performance, as compared with example 1.
In conclusion, the lithium ion battery electrolyte provided by the invention contains an organic germanium compound shown in formula 1, 4, 5-dicyano-2-trifluoromethyl imidazole lithium, nitrile compound and other additives which are optimally combined, and the lithium ion battery has high safety and excellent high-temperature cycle performance, high-temperature storage and low-temperature discharge performance through the synergistic effect of the additives.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. An electrolyte, wherein the electrolyte comprises a non-aqueous organic solvent, an additive, and a lithium salt; the additive comprises an organic germanium compound shown in a formula 1, 4, 5-dicyano-2-trifluoromethyl imidazole lithium and a nitrile compound;
Figure FDA0002952961060000011
2. the electrolyte solution according to claim 1, wherein the mass ratio of the sum of the addition amounts of the organogermanium compound represented by formula 1 and 4, 5-dicyano-2-trifluoromethylimidazolium to the addition amount of the nitrile compound is 1 (1-10).
3. The electrolyte of claim 1, wherein the organogermanium compound represented by formula 1 is added in an amount of 0.1 to 0.8 wt% based on the total mass of the electrolyte.
4. The electrolyte of claim 1, wherein the lithium 4, 5-dicyano-2-trifluoromethylimidazole is added in an amount of 0.1 to 1 wt% based on the total mass of the electrolyte.
5. The electrolyte according to claim 1, wherein the nitrile compound is added in an amount of 0.5 to 5 wt% based on the total mass of the electrolyte.
6. The electrolyte of claim 1, wherein the nitrile compound is selected from at least one of 1,3,6 hexanetricarbonitrile, 1,3, 5-cyclohexanetricarbonitrile, glycerol trinitrile, 2,3,5, 6-pyrazine tetracarbonitrile, and tetracyanoethylene.
7. The electrolyte of any one of claims 1-6, wherein the additive further comprises at least one of tris (trimethylsilane) phosphite, tris (trimethylsilyl) borate, trimethylsilylimidazole, lithium bistrifluoromethanesulfonylimide, lithium bistrifluorosulfonylimide, 1, 3-propanesultone, ethylene sulfite, vinyl sulfate, vinylene carbonate, fluoroethylene carbonate, lithium dioxalate borate, lithium difluorooxalato phosphate, and vinyl carbonate, added in an amount of 0 to 10 wt% based on the total mass of the electrolyte.
8. The electrolyte as claimed in claim 1, wherein the non-aqueous organic solvent is selected from a mixture of at least one of cyclic carbonates and at least one of linear carbonates and linear carboxylates, in any proportion; and/or the presence of a gas in the gas,
the lithium salt is at least one selected from lithium bis (trifluoromethyl) sulfonyl imide, lithium bis (fluoro) sulfonyl imide and lithium hexafluorophosphate.
9. A lithium ion battery comprising the electrolyte of any of claims 1-8.
10. The lithium ion battery of claim 9, wherein the lithium ion battery has a charge cut-off voltage of 4.45V and above.
CN202110212758.1A 2021-02-25 2021-02-25 Electrolyte and lithium ion battery comprising same Pending CN113013486A (en)

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CN113571773A (en) * 2021-06-23 2021-10-29 惠州锂威新能源科技有限公司 Lithium ion battery electrolyte and lithium ion battery containing same
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Application publication date: 20210622