CN111900481A - Electrolyte for high-nickel anode material lithium ion battery - Google Patents
Electrolyte for high-nickel anode material lithium ion battery Download PDFInfo
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- CN111900481A CN111900481A CN202010885290.8A CN202010885290A CN111900481A CN 111900481 A CN111900481 A CN 111900481A CN 202010885290 A CN202010885290 A CN 202010885290A CN 111900481 A CN111900481 A CN 111900481A
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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 discloses an electrolyte of a lithium ion battery suitable for a high-nickel anode material, which contains an anhydride additive. Meanwhile, the additive is used as an auxiliary additive to jointly improve the performance of the battery. The additive can be oxidized on the surface of a battery anode material to form a layer of passive film, and the layer of passive film is in close contact with the surface of a high-nickel anode material, so that direct contact between electrolyte and the surface of the anode material is avoided, and oxidative decomposition and side reaction of the electrolyte are inhibited. The passive film on the surface of the anode can effectively inhibit the dissolution of transition metal ions and improve the structural stability of the anode material. Meanwhile, the additive can react with trace water and hydrofluoric acid in the electrolyte, eliminate the hydrofluoric acid in the electrolyte and stabilize lithium hexafluorophosphate, so that the high-nickel lithium ion battery containing the electrolyte disclosed by the invention has better capacity retention rate.
Description
Technical Field
The invention relates to a lithium ion battery electrolyte and application thereof in a lithium ion battery containing a high-nickel anode material, belonging to the field of lithium ion batteries.
Background
The lithium ion battery is widely applied in the fields of portable electronic products, electric automobiles and the like. In order to meet the increasing demand for energy density, efforts are being made to develop a high energy density positive electrode material and to increase the operating voltage of a lithium ion battery.For example, the operating voltage of the high-voltage positive electrode material lithium nickel manganese oxide is as high as 4.9V, but the energy density is lower and the oxidative decomposition phenomenon in a high-voltage environment is serious; layered ternary materials of high energy density, e.g. high nickel positive electrode material lithium nickel cobalt manganese oxide (LiNi)xCoyMnzO2X is not less than 0.5) the specific discharge capacity can reach 200 mAh g-1And the operating voltage is higher, and the method has good application prospect.
In the practical application process of the high-nickel cathode material, some problems still exist, and the use of the high-nickel cathode material is limited. During the preparation process of the cathode material, residual lithium on the surface of the cathode material is easy to react with water; ni in the course of circulation4+The electrolyte is oxidized, side reaction occurs on the surface of the electrode, and irreversible phase change and capacity fading of the electrode material are accelerated. Meanwhile, the commercialized lithium hexafluorophosphate-based electrolyte is easy to react with water to generate harmful substances such as hydrofluoric acid and the like, so that transition metal ions are dissolved out, the capacity decline of the battery is accelerated, and the service life of the battery is shortened. Patent publication No. CN103378360A discloses an organic electrolyte for improving the low-temperature performance of a lithium-manganese battery in 2013, 10.30.2013, the low-temperature performance of the lithium-manganese battery is improved by improving the electrolyte, and firstly, the organic solvent is improved to be a mixed solvent combination of cyclic esters, linear esters, ethers and sulfones; secondly, the additive is selected from additive A and additive B. But is not suitable for high nickel cathode materials and cannot solve the problems of the electrolyte in the practical application process of the high nickel cathode materials.
Disclosure of Invention
In view of the problems of the prior art, the invention aims to provide an electrolyte capable of improving the cycle life of a high-nickel lithium ion battery, which contains an acid anhydride additive, and is characterized in that: the structure is as follows:
according to the technical scheme, the acid anhydride additive is added into the electrolyte of the high-nickel lithium ion battery, so that the high-nickel lithium ion battery can spontaneously react with water and hydrofluoric acid in the electrolyte, hydrolysis of lithium salt is inhibited, the hydrofluoric acid is effectively eliminated, the stability of the electrolyte is improved, the hydrofluoric acid is prevented from corroding the surface of the positive electrode material, and collapse and capacity attenuation of the high-nickel positive electrode material are inhibited.
The additive can be oxidized on the surface of a positive electrode in preference to a solvent to form a compact passivation film, the benzoic anhydride has a symmetrical structure, a product generated during oxidation contains carbon groups and has strong electronegativity, and the surface of a high-nickel positive electrode material contains a large number of high-valence nickel ions, so that the passivation film can be covered on the surface of the high-nickel positive electrode material very tightly.
The benzoic anhydride participates in the formed passivation film to avoid the contact between the electrolyte and the surface of the anode material, and inhibit the oxidative decomposition of the organic solvent. The passivation film can effectively improve the structural stability of the nickel-rich cathode material and inhibit the irreversible phase change of the nickel-rich cathode material in the circulation process, thereby reducing the dissolution of transition metal ions.
Preferably, the anhydride additive accounts for 0.5-5.0% of the total weight of the electrolyte. Within this range, the effect of eliminating hydrofluoric acid is optimal, and excessive acid anhydride additives prevent the formed passivation film from covering the surface of the high-nickel cathode material, thereby reducing the stability of the material structure.
More preferably, the anhydride additive accounts for 1.5-3.5% of the total weight of the electrolyte.
Preferably, the electrolyte is composed mainly of an organic solvent, a lithium salt and an additive, wherein:
the anhydride additive accounts for 0.5-5.0% of the total weight of the electrolyte,
the auxiliary additive accounts for 0.5-2% of the total weight of the electrolyte,
the organic solvent accounts for 80-85% of the total weight of the electrolyte,
the lithium salt accounts for 13-18% of the total weight of the electrolyte.
Preferably, the auxiliary additive is one or more of vinylene carbonate, fluoroethylene carbonate, lithium difluorooxalate phosphate and lithium difluorooxalate borate.
Preferably, the organic solvent is selected from cyclic carbonate and chain carbonate, and the total mass of the cyclic carbonate and the chain carbonate accounts for 80-85% of the total weight of the electrolyte, wherein:
the cyclic carbonates include ethylene carbonate and propylene carbonate.
The chain carbonate includes ethyl methyl carbonate, dimethyl carbonate, and diethyl carbonate.
Preferably, the lithium salt mainly comprises one or more of lithium hexafluorophosphate, lithium dioxalate borate, lithium tetrafluoroborate and lithium bistrifluoromethylsulfonyl imide.
Preferably, the electrolyte comprises the following components in percentage by weight: 1.5-3.5% of benzoic anhydride, 0.5-2% of vinylene carbonate, 80-85% of organic solvent and 13-18% of lithium hexafluorophosphate, wherein the organic solvent is a mixture of propylene carbonate and diethyl carbonate.
The invention also provides the application of the electrolyte, which is used for a lithium ion battery of a high-nickel cathode material. In particular, a high nickel positive electrode material having a nickel content of 60% or more is more preferable, and a high nickel positive electrode material having a nickel content of 70% or more is even more preferable.
Preferably, the high-nickel positive electrode material is nickel cobalt lithium manganate satisfying the structural formula LiNixCoyMnzO2Wherein x is more than or equal to 0.6.
Compared with the prior art, the invention has the following beneficial effects:
the lithium ion battery aiming at the high-nickel positive electrode material provided by the invention contains the anhydride additive, the additive can be oxidized on the surface of the positive electrode in preference to a solvent to form a compact passivation film, the benzoic anhydride has a symmetrical structure, a product generated during oxidation contains carbon base and has stronger electronegativity, and the passivation film can be tightly covered on the surface of the high-nickel positive electrode material because the surface of the high-nickel positive electrode material contains a large amount of high-valence nickel ions. The benzoic anhydride participates in the formed passivation film to avoid the contact between the electrolyte and the surface of the anode material, and inhibit the oxidative decomposition of the organic solvent. The passivation film can effectively improve the structural stability of the nickel-rich cathode material and inhibit the irreversible phase change of the nickel-rich cathode material in the circulation process, thereby reducing the dissolution of transition metal ions.
The additive benzoic anhydride contained in the electrolyte provided by the invention can spontaneously react with trace water and hydrofluoric acid in the electrolyte, so that the hydrolysis of lithium salt lithium hexafluorophosphate is inhibited, the hydrofluoric acid is effectively eliminated, the stability of the electrolyte is improved, the corrosion of the hydrofluoric acid on the surface of a positive electrode material is avoided, and the collapse and capacity attenuation of the positive electrode material are inhibited.
However, the introduction of benzoic anhydride leads to lower coulombic efficiency of the first circle of the battery, and the initial cycle period has larger impedance, so that the introduction of the auxiliary additive improves the coulombic efficiency of the first circle of the battery and reduces the initial impedance of the battery, and meanwhile, the use amounts and types of benzoic anhydride and other auxiliary additives can seriously affect the performance of the battery, and different additive types and additive use amounts need to be controlled according to different nickel contents of the positive electrode material.
In a word, the electrolyte provided by the invention has good compatibility with a high-nickel anode material, particularly has more obvious effect on an anode material with the nickel content of more than 60%, and can be oxidized to form a passivation film high-nickel protective anode material and stabilize the electrolyte, so that a high-nickel lithium ion battery containing the electrolyte provided by the invention has better cycle stability and rate capability.
Drawings
Fig. 1 is an SEM image of the cathode material after cycling in example 1 of the present invention.
Fig. 2 is an SEM image of the cathode material after recycling in comparative example 1 of the present invention.
Detailed description of the preferred embodiments
For better understanding of the above technical solutions, the above technical solutions will be described in detail with reference to the drawings and specific examples, but the embodiments of the present invention are not limited thereto.
The layered lithium nickel manganese oxide and lithium cobaltate with different nickel contents are used as positive electrode materials, metal lithium is selected as a negative electrode material, the electrolyte disclosed by the embodiment of the invention is self-prepared, and the battery is assembled after standing for 12 hours. And carrying out constant-current charge and discharge test on the assembled battery within the voltage range of 3.0-4.3V under the condition of 1C. Prepared by the aboveAll in the glove box (H)2O≤0.01, O2Less than or equal to 0.01).
Example 1
An electrolyte for a high-nickel cathode material lithium ion battery is prepared as follows:
the carbonate-based organic solvent was prepared at a mass ratio of EC: EMC =3:7 (mass ratio). Dissolving lithium salt lithium hexafluorophosphate in the organic solvent, wherein the mass of the organic solvent is 85 wt.% of the total mass, the mass of the lithium salt accounts for 13wt.% of the total weight of the electrolyte, and adding 2.0 wt.% of benzoic anhydride into the electrolyte to obtain the lithium ion battery electrolyte through dissolution.
The lithium ion battery is assembled by using the electrolyte prepared above and a positive electrode material NCM 811.
Example 2
The difference from example 1 is that 2.0 wt.% benzoic anhydride and 0.5 wt.% lithium difluorooxalato phosphate are added to the electrolyte as two-component additives.
Example 3
The difference from example 1 is that 1.0 wt.% benzoic anhydride and 0.5 wt.% lithium difluorooxalato phosphate are added to the electrolyte as two-component additives.
Example 4
The difference from example 1 is that 1.0 wt.% benzoic anhydride and 1.0 wt.% lithium difluorooxalato phosphate are added to the electrolyte as two-component additives.
Example 5
The difference from example 1 is that the positive electrode material NCM622 is selected to assemble the lithium ion battery.
Example 6
The difference from example 3 is that benzoic anhydride was selected to have a mass of 2.0 wt.% of the electrolyte and lithium difluorooxalate phosphate was selected to have a mass of 0.5 wt.%.
Example 7
The difference from example 3 is that benzoic anhydride was selected to have a mass of 1.0 wt.% of the electrolyte and lithium difluorooxalate phosphate was selected to have a mass of 1.0 wt.%.
Example 8
The difference from the embodiment 1 is that the lithium ion battery is assembled by selecting the positive electrode material of which the positive electrode material is NCM 523.
Example 9
The difference from example 1 is that the assembled lithium ion battery with the positive electrode material of NCM11 is selected.
Example 10
The difference from the embodiment 1 is that the lithium ion battery is assembled by selecting the cathode material as lithium cobaltate.
Example 11
Preparing an electrolyte: 15wt% of lithium dioxalate borate, 2wt% of vinylene carbonate, 40 wt% of propylene carbonate, 40 wt% of diethyl carbonate and 3wt% of benzoic anhydride.
The lithium ion battery is assembled by using the electrolyte prepared above and a positive electrode material NCM 811.
Example 12
Preparing an electrolyte: 13wt% of lithium tetrafluoroborate, 1.5wt% of lithium difluorooxalato borate, 40 wt% of ethylene carbonate, 45 wt% of dimethyl carbonate and 0.5 wt% of benzoic anhydride.
The lithium ion battery is assembled by using the electrolyte prepared above and a positive electrode material NCM 811.
Comparative example 1
The difference from example 1 is that no additive benzoic anhydride was added to the electrolyte, and no additive was added.
Comparative example 2
The difference from example 1 is that no additive benzoic anhydride was added to the electrolyte and the mass fraction of lithium difluorooxalate phosphate was 0.5 wt.%.
Comparative example 3
The difference from example 1 is that no additive benzoic anhydride was added to the electrolyte and the mass fraction of lithium difluorooxalate phosphate was 1.0 wt.%.
Comparative example 4
The difference from example 5 is that no additive benzoic anhydride was added to the electrolyte.
Comparative example 5
The difference from example 6 is that no additive benzoic anhydride was added to the electrolyte. The mass fraction containing lithium difluorooxalate phosphate was 0.5 wt.%.
Comparative example 6
The difference from example 7 is that no additive benzoic anhydride was added to the electrolyte. The mass fraction containing lithium difluorooxalate phosphate was 1.0 wt.%.
Comparative example 7
The difference from example 8 is that no additive benzoic anhydride was added to the electrolyte.
Comparative example 8
The difference from example 9 is that no additive benzoic anhydride was added to the electrolyte.
Comparative example 9
The difference from example 10 is that no additive benzoic anhydride was added to the electrolyte.
Comparative example 10
The difference from example 11 is that benzoic acid was used in place of benzoic anhydride in the electrolyte.
Comparative example 11
The difference from example 1 is that the content of benzoic anhydride added to the electrolyte was 10%.
Comparative example 12
The difference from example 1 is that the content of benzoic anhydride added to the electrolyte was 0.1%.
The assembled lithium ion batteries of the above examples and comparative examples were tested for electrochemical performance at 30 ℃ and the results after 100 cycles are shown in table 1 below:
as can be seen from the comparison between the above-mentioned examples 1 and 2 and the comparative example, for the NCM811 cathode material, the cycle retention rate of the lithium ion battery can be greatly improved by the electrolyte containing the additive benzoic anhydride disclosed by the invention within the cut-off voltage range of 3.0-4.3V. The best cycling performance of the battery was obtained when additives 2.0 wt.% and 0.5 wt.% were selected for the NCM811 positive electrode material, but the best cycling performance was obtained when additives 1.0 wt.% and 1.0 wt.% were selected for the NCM622 positive electrode material. This is mainly related to the content of Ni in the positive electrode material, and when the content of Ni is larger, more benzoic anhydride can be oxidized and adhered to the surface of the positive electrode, and as the content of Ni is reduced, too much benzoic anhydride affects the impedance of the battery, and it is necessary to reduce the content of benzoic anhydride and increase the amount of other auxiliary additives.
In order to further improve the performance of the battery, the benzoic anhydride is added as an additive, and other auxiliary additives are also added, as can be seen from comparison between examples 1 and 3, the dosage of the benzoic anhydride additive is closely related to the positive electrode material, and as the content of nickel is reduced, the too much benzoic anhydride can reduce the performance of the battery, so that the dosage of the auxiliary additive needs to be adjusted to further improve the performance of the battery, and as can be seen from comparison between examples 2 and 4 and 5, the dosage of the lithium difluorobis (oxalato) phosphate as the auxiliary additive needs to be matched with the dosage of the benzoic anhydride and the positive electrode material so as not to further improve the performance of the battery. The method is mainly related to the matching property of benzoic anhydride which can be oxidized into a film and a positive electrode material, and meanwhile, the lithium difluorooxalate phosphate can improve the conductivity of the battery, so that the coulombic efficiency of the first circle of the battery is improved, and the performance of the battery is improved by modifying a passivation film.
When the nickel content in the positive electrode material is less than 60%, the improvement of the cycle performance of the lithium ion battery by the electrolyte containing benzoic anhydride is smaller than that of a blank electrolyte, and the performance improvement of the lithium ion battery of lithium cobaltate is smaller when the positive electrode material is used. The passivation film is formed by oxidizing the additive benzoic anhydride, and the passivation film has the existence of acyl-rich groups which are generated by oxidizing the benzoic anhydride and have strong electronegativity, so that the passivation film can be well attached to the surface of the high-nickel anode material, and the structural stability of the anode material is protected. Meanwhile, the benzoic anhydride can eliminate hydrofluoric acid in the electrolyte and stabilize lithium hexafluorophosphate. The more sensitive the material is to water and hydrofluoric acid, the more poor the stability of the material due to the increase of the nickel content in the anode material and the existence of residual lithium on the surface of the material. Benzoic anhydride can react with water and hydrofluoric acid to eliminate the influence of the water and the hydrofluoric acid, so that the electrolyte containing the additive benzoic anhydride has more obvious improvement on the performance of the lithium ion battery.
In summary, the cycle performance of the lithium ion battery can be effectively improved by introducing the benzoic anhydride into the electrolyte, then introducing the auxiliary additive, and adjusting the proportion of the benzoic anhydride and the auxiliary additive according to the characteristics of the positive electrode material.
Claims (10)
1. An electrolyte for a high-nickel cathode material lithium ion battery, the electrolyte comprising an anhydride additive, wherein: the acid anhydride additive has the following structure:
。
2. the electrolyte of claim 1, wherein: the anhydride additive accounts for 0.5-5.0% of the total weight of the electrolyte.
3. The electrolyte of claim 2, wherein: the electrolyte also comprises an organic solvent, lithium salt and an auxiliary additive, wherein the auxiliary additive accounts for 0.5-2% of the total weight of the electrolyte; the organic solvent accounts for 80-85% of the total weight of the electrolyte; the lithium salt accounts for 13-18% of the total weight of the electrolyte.
4. The electrolyte of claim 3, wherein: the auxiliary additive is selected from one or more of vinylene carbonate, fluoroethylene carbonate, lithium difluorooxalate phosphate and lithium difluorooxalate borate.
5. The electrolyte of claim 1, wherein: the mass of the benzoic anhydride accounts for 2% of the total mass of the electrolyte, and the mass of one or more of lithium difluorooxalate phosphate and lithium difluorooxalate borate accounts for 0.5% of the electrolyte.
6. The electrolyte of claim 1, wherein: the mass of the benzoic anhydride accounts for 1% of the total mass of the electrolyte, and the mass of one or more of lithium difluorooxalate phosphate and lithium difluorooxalate borate accounts for 1.0-2.0% of the electrolyte.
7. The electrolyte of claim 3, wherein: the organic solvent contains cyclic carbonate and chain carbonate at the same time, wherein the cyclic carbonate is selected from one or two of ethylene carbonate and propylene carbonate, and the chain carbonate is selected from one or more of ethyl methyl carbonate, dimethyl carbonate and diethyl carbonate.
8. The electrolyte of claim 3, wherein: the lithium salt comprises one or more of lithium hexafluorophosphate, lithium perchlorate, lithium dioxalate borate, lithium tetrafluoroborate and lithium bistrifluoromethylsulfonyl imide.
9. Use of the electrolyte according to any of claims 1 to 8, wherein: the lithium ion battery is used for the high-nickel cathode material.
10. Use of an electrolyte according to claim 9, characterized in that: the high-nickel positive electrode material is nickel cobalt lithium manganate, and satisfies the structural formula LiNixCoyMnzO2Wherein x is more than or equal to 0.6.
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Cited By (3)
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| CN114156536A (en) * | 2021-10-27 | 2022-03-08 | 大连中比动力电池有限公司 | Additive, electrolyte and application of electrolyte in improving low-temperature performance of lithium battery |
| CN114714727A (en) * | 2022-03-31 | 2022-07-08 | 肖冰 | Outer packaging aluminum-plastic film for battery, preparation method and battery |
| EP4145580A4 (en) * | 2021-07-22 | 2023-11-01 | Contemporary Amperex Technology Co., Limited | Electrolyte, lithium-ion battery, and power device |
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Application publication date: 20201106 |