CN114447436A - High-voltage electrolyte of lithium ion battery and application - Google Patents
High-voltage electrolyte of lithium ion battery and application Download PDFInfo
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- CN114447436A CN114447436A CN202210213055.5A CN202210213055A CN114447436A CN 114447436 A CN114447436 A CN 114447436A CN 202210213055 A CN202210213055 A CN 202210213055A CN 114447436 A CN114447436 A CN 114447436A
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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
- 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
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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
- H01M10/42—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
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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
- H01M2300/002—Inorganic electrolyte
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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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Abstract
The invention provides a high-voltage electrolyte of a lithium ion battery and application thereof. The high-voltage electrolyte of the lithium ion battery comprises a non-aqueous organic solvent, lithium salt and a functional additive; the functional additive is one or the combination of more than two of 3-cyano-5-fluorobenzene boric acid, fumaric nitrile, tributyl borate and triisopropyl borate. The lithium ion battery containing the high-voltage electrolyte has excellent stability and safety.
Description
Technical Field
The invention relates to the technical field of electrolyte, in particular to high-voltage electrolyte and application thereof in a lithium ion battery.
Background
The electrolyte serves as an important component of the battery, plays a role in transporting lithium ions between the positive electrode and the negative electrode of the lithium ion battery, and is called as 'blood' of the lithium ion battery. The electrolyte plays a vital role in the specific capacity, the working temperature range, the cycle efficiency, the safety performance and the like of the battery. The selection of a proper electrolyte is the key to obtain a lithium ion secondary battery with high energy density, long cycle life and good safety performance, so that the research of the electrolyte meeting the requirements of the lithium ion battery is very important.
At present, the lithium ion battery electrolyte has the defects of rapid capacity loss and poor cycle performance at high temperature and high pressure, and can not meet the working requirement that the lithium ion battery electrolyte is often at high temperature and high pressure.
In order to meet the above requirements, an electrolyte capable of operating a lithium ion battery under a high voltage condition needs to be developed.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide an electrolyte for a lithium ion battery, which has high pressure resistance, oxidation resistance, and high temperature resistance, so that the lithium ion battery containing the electrolyte has high cycle performance under high pressure.
In order to achieve the technical purpose, the invention firstly provides a high-voltage electrolyte of a lithium ion battery, which comprises a non-aqueous organic solvent, a lithium salt and a functional additive; wherein the mass fraction of the functional additive in the electrolyte is less than 5%, the mass fraction of the nonaqueous organic solvent in the electrolyte is 60-90%, and the mass fraction of the lithium salt in the electrolyte is 10-20%; the functional additive is one or the combination of more than two of 3-cyano-5-fluorobenzene boric acid, fumaric nitrile, tributyl borate and triisopropyl borate.
In a specific embodiment of the invention, the addition amount of the functional additive is 0.1-5% based on 100% of the total mass of the high-voltage electrolyte of the lithium ion battery.
In one embodiment of the present invention, the functional additive is 3-cyano-5-fluorobenzeneboronic acid having the following structural formula:
in the high-voltage electrolyte of the lithium ion battery, a functional additive, such as 3-cyano-5-fluorobenzeneboronic acid, is added into the electrolyte, so that a stable CEI film can be formed on the surface of the positive electrode, and the electrolyte is prevented from continuously generating an oxidation-reduction reaction on the surface of the positive electrode; meanwhile, the oxide film effectively avoids continuous contact between electrolyte and a positive electrode material, thereby protecting the crystal structure of the electrode material, effectively reducing the loss of reversible capacity in the circulation process and improving the stability and the safety of the battery.
In one embodiment of the present invention, the non-aqueous organic solvent is a combination of at least two of ethylene carbonate, propylene carbonate, fluoroethylene carbonate, ethyl methyl carbonate, dimethyl carbonate, dimethoxyethane, and diethyl carbonate.
In one embodiment of the present invention, the lithium salt is one or a combination of two or more of lithium hexafluorophosphate, lithium bis (oxalato) borate, lithium difluorophosphate and lithium trifluoromethanesulfonate. The concentration of the lithium salt used is 0.8mol/L to 1.5 mol/L.
The invention also provides a lithium ion battery, which comprises a positive electrode, a diaphragm, electrolyte and a negative electrode, wherein the electrolyte is the high-voltage electrolyte of the lithium ion battery.
In one embodiment of the present invention, the positive electrode includes a positive current collector foil and a positive active powder material attached to the positive current collector foil.
In one embodiment of the present invention, the separator is one of a polypropylene film, a polyethylene film, a polypropylene/polyethylene/polypropylene composite film, a nylon cloth, a glass fiber, and a asbestos paper.
According to the high-voltage electrolyte of the lithium ion battery, a specific functional additive, especially 3-cyano-5-fluorobenzeneboronic acid is added, and the functional additive, especially 3-cyano-5-fluorobenzeneboronic acid, has a low oxidation-reduction potential, so that a stable CEI film can be formed on the surface of a positive electrode, and the electrolyte is prevented from continuously undergoing an oxidation-reduction reaction on the surface of the positive electrode; meanwhile, the oxide film can effectively avoid the continuous contact of electrolyte and a positive electrode material, thereby protecting the crystal structure of the electrode material, effectively reducing the loss of reversible capacity in the circulation process and improving the stability and the safety of the battery.
Drawings
FIG. 1 is a graph showing the cycle performance of LiNi1/3Co1/3Mn1/3O2/Li batteries prepared in example 1 and comparative example 1.
FIG. 2 is a graph of rate performance of LiNi1/3Co1/3Mn1/3O2/Li batteries prepared in example 1 and comparative example 1.
FIG. 3 is an EIS diagram of LiNi1/3Co1/3Mn1/3O2/Li batteries prepared in example 1 and comparative example 1.
FIG. 4 is an SEM image of LiNi1/3Co1/3Mn1/3O2/Li pole piece in LiNi1/3Co1/3Mn1/3O2/Li batteries prepared in example 1 and comparative example 1.
FIG. 5 is a TEM image of LiNi1/3Co1/3Mn1/3O2/Li cell LiNi1/3Co1/3Mn1/3O2/Li pole piece prepared in example 1 and comparative example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
This example provides a lithium ion half cell, which was prepared by the following procedure.
1.0mol of LiPF6Dissolving the mixture in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) in a volume ratio of 1:1 (the volume is 0.5L) to form a blank electrolyte, and adding 1 wt% of 3-cyano-5-fluorobenzeneboronic acid (CFBA) as an additive into the blank electrolyte, wherein the 3-cyano-5-fluorobenzeneboronic acid accounts for 1% of the total weight of the electrolyte. The LiNi1/3Co1/3Mn1/3O2/Li half-cell is assembled.
Comparative example 1
For comparison, the blank electrolyte was also assembled into a LiNi1/3Co1/3Mn1/3O2/Li half cell, forming comparative example 1.
FIG. 1 shows that when the battery is charged and discharged under the constant current condition within the voltage range of 3-4.5V, the battery capacity is quickly attenuated in the basic electrolyte, and the addition of a small amount of CFBA can obviously improve the electricityThe cycling performance of the cell. After 100 cycles, the specific discharge capacity of the 1 wt% CFBA electrolyte is 142.1mAh g-1The capacity retention rate is respectively as high as 89.4 percent. While the battery circulating in the basic electrolyte is rapidly attenuated to 104.5mAh g from the initial capacity of 157.3mAh g-1-1The capacity retention was only 66.24%. CFBA improves battery cycle life while also improving battery rate performance.
FIG. 2 is a graph of the rate of LiNi1/3Co1/3Mn1/3O2/Li cells in the base electrolyte (comparative example 1) and in the electrolyte containing CFBA (example 1), and it can be seen from FIG. 2 that the capacity of the base electrolyte has been reduced to around 40mAh g-1 when cycled at 5C, while the cells containing CFBA electrolyte remained higher than 110mAh g-1-1The discharge specific capacity and the cycling stability are still good.
FIG. 3 is an impedance plot of LiNi1/3Co1/3Mn1/3O2/Li cells after cycling in the base electrolyte (comparative example 1) and CFBA-containing electrolyte (example 1), EIS analysis further demonstrating that CFBA electrolyte can effectively improve electrode interface stability. As shown in fig. 3, each curve is composed of two semi-circles and one oblique line. The two semicircles from high to medium-high frequency represent the charge transfer resistance (Rct) on the surface passivation film (Rcei) and the electrode, respectively, while the diagonal line in the low frequency region is the Warburg resistance generated by Li + diffusion in the working electrode. As shown in fig. 3, the initial interface resistance of the CFBA electrolyte-containing cell after three activations was slightly greater than the interface resistance in the base electrolyte, since CFBA produced additional resistance in forming a more excellent interface film. After the circulation is carried out for 100 times, the basic electrolyte is continuously oxidized and decomposed under high voltage, and the generated inorganic salt and organic matters are continuously accumulated on the surface of the positive electrode, so that the polarization of the battery in the basic electrolyte is continuously increased, and the resistance is also obviously increased along with the circulation. In comparison, the impedance of the cell with the CFBA electrolyte increased slightly. This indicates that CFBA forms a stable interfacial film on NCM111, suppressing decomposition of the electrolyte.
FIG. 4 is an SEM image of LiNi1/3Co1/3Mn1/3O2/Li battery after circulation in a base electrolyte (comparative example 1) and an electrolyte containing DEPP (example 1), and the NCM111 pole piece before circulation and after circulation in different electrolytes is analyzed by a scanning electron microscope, and the result is that the NCM111 pole piece before circulation and after circulation in different electrolytes is not circulated, and the surface of the pole piece is smooth, and the edge angle of particles can be clearly observed without any covering object as shown in a picture a and a picture d of FIG. 4. After 100 cycles, the surface of the NCM111 electrode sheet circulated in the carbonate electrolyte was covered with a large amount of decomposition products, the particle structure became obscure, and the surface coverage was not uniform, there were many decomposition products in some places and few covering materials in some places, indicating that the conventional electrolyte could not form a uniform interfacial film on the surface of the material (fig. 4, panels b and e). And the coverage on the surface of the electrode material circulating in the CFBA electrolyte is obviously reduced, the coverage is more uniform, and the edges and corners of the particles are also clearly visible. The electrolyte containing CFBA is decomposed on the surface of the material to form a thin film-shaped substance, and the oxidative decomposition of the basic electrolyte on the surface of the anode material is effectively inhibited.
FIG. 5 is a TEM image of LiNi1/3Co1/3Mn1/3O2 before being cycled and after being cycled in a base electrolyte and a CFBA-containing electrolyte, and the TEM can further analyze the oxidation film formation of the electrolyte on the surface of the electrode. As can be seen from fig. 5, the blank sheet had a smooth surface and lattice lines could be observed. A layer of thicker interfacial film is formed on the surface of the pole piece after circulation in the basic electrolyte, and the thickness of the interfacial film is different at different places. The lithium ion is prevented from being extracted in the charging and discharging process, and the cycle performance of the battery is further influenced. And a thin interface film is coated on the surface of the NCM111 pole piece circulating in the CFBA electrolyte, and the positive electrode is separated from the electrolyte by the interface film, so that the positive electrode structure is protected from collapsing in the circulating process, and the continuous oxidative decomposition of the electrolyte is prevented. Consistent with the above SEM conclusions.
Example 2
1.0mol of LiPF6Dissolving in a solvent with the volume ratio of 1:1, forming a blank electrolyte in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (the volume is 0.5L), and adding 0.3 wt% of 3-cyano-5-fluorobenzeneboronic acid as an additive in the blank electrolyte, namely, the 3-cyano-5-fluorobenzeneboronic acid accounts for 0.3% of the total weight of the electrolyte. The LiNi1/3Co1/3Mn1/3O2/Li half-cell is assembled.
Example 3
1.0mol of LiPF6Dissolving in a solvent with the volume ratio of 1:1, forming a blank electrolyte in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (the volume is 0.5L), and adding 0.7 wt% of 3-cyano-5-fluorobenzeneboronic acid as an additive in the blank electrolyte, namely, the 3-cyano-5-fluorobenzeneboronic acid accounts for 0.7% of the total weight of the electrolyte. The LiNi1/3Co1/3Mn1/3O2/Li half-cell is assembled.
Example 4
1.0mol of LiPF6Dissolving in a solvent with the volume ratio of 1:1, forming a blank electrolyte in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) (the volume is 0.5L), and adding 2 wt% of 3-cyano-5-fluorobenzeneboronic acid as an additive in the blank electrolyte, namely, the 3-cyano-5-fluorobenzeneboronic acid accounts for 2% of the total weight of the electrolyte. Assembled into a LiNi1/3Co1/3Mn1/3O2/Li half-cell
Comparative example 2
1.0mol of LiPF6Dissolving in a solvent with the volume ratio of 1:1, 0.5L of mixed solution of Ethylene Carbonate (EC)/dimethyl carbonate (DMC) forms blank electrolyte, and 3-fluoro-phenylboronic acid with the mass ratio of 1 wt% is added into the blank electrolyte as an additive, namely 3-fluoro-phenylboronic acid accounts for 1% of the total weight of the electrolyte. The LiNi1/3Co1/3Mn1/3O2/Li half-cell is assembled.
Comparative example 3
1.0mol of LiPF6Dissolving in a solvent with the volume ratio of 1:1, 0.5L of mixed solution of Ethylene Carbonate (EC)/dimethyl carbonate (DMC) is formed into blank electrolyte, and then 3-cyano-phenylboronic acid with the mass ratio of 1 wt% is added into the blank electrolyte to serve as an additive, namely, the 3-cyano-phenylboronic acid accounts for 1% of the total weight of the electrolyte. The LiNi1/3Co1/3Mn1/3O2/Li half-cell is assembled.
Comparative example 4
1.0mol of LiPF6Dissolving in a solvent with the volume ratio of 1:1 of Ethylene Carbonate (EC)/dimethyl carbonate (DMC) (the volume is 0.5L) to form a blank electrolyte, and then adding phenylboronic acid with the mass ratio of 1 wt% as an additive into the blank electrolyte, namely phenylboronic acidThe acid accounts for 1% of the total weight of the electrolyte. The LiNi1/3Co1/3Mn1/3O2/Li half-cell is assembled.
Test results of lithium ion batteries prepared from the electrolytes of examples 1 to 4 and comparative examples 1 to 4 are shown in table 1.
TABLE 1
| Sample (I) | Specific capacity of first discharge/mAh.g-1 | Capacity retention ratio of 100 cycles/%) |
| Example 1 | 157.4 | 90.2 |
| Example 2 | 149.2 | 81.9 |
| Example 3 | 148.5 | 82.1 |
| Example 4 | 150.7 | 66.4 |
| Comparative example 1 | 157.3 | 65.2 |
| Comparative example 2 | 139.3 | 70.4 |
| Comparative example 3 | 136.5 | 71.2 |
| Comparative example 4 | 138.7 | 69.5 |
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. The high-voltage electrolyte of the lithium ion battery is characterized by comprising a non-aqueous organic solvent, a lithium salt and a functional additive, wherein the mass fraction of the functional additive in the electrolyte is less than 5%, the mass fraction of the non-aqueous organic solvent in the electrolyte is 60-90%, and the mass fraction of the lithium salt in the electrolyte is 10-20%;
wherein the functional additive is one or the combination of more than two of 3-cyano-5-fluorobenzeneboronic acid, fumaronitrile, tributyl borate and triisopropyl borate.
2. The lithium ion high voltage electrolyte of claim 1, wherein the functional additive is added in an amount of 0.1-5% based on 100% of the total mass of the high voltage electrolyte of the lithium ion battery.
3. The high voltage electrolyte of claim 1, wherein the non-aqueous organic solvent is a combination of at least two of ethylene carbonate, propylene carbonate, fluoroethylene carbonate, ethyl methyl carbonate, dimethyl carbonate, dimethoxyethane, diethyl carbonate.
4. The high-voltage electrolyte as claimed in claim 1, wherein the lithium salt is one or a combination of two or more of lithium hexafluorophosphate, lithium bis (oxalato) borate, lithium difluorophosphate and lithium trifluoromethanesulfonate.
5. The high voltage electrolyte of claim 1 or 4, wherein the concentration of the lithium salt is 0.8mol/L to 1.5 mol/L.
6. A lithium ion battery, characterized in that the lithium ion battery comprises a positive electrode, a separator, an electrolyte and a negative electrode, wherein the electrolyte is the high-voltage electrolyte of the lithium ion battery of any one of claims 1 to 5.
7. The lithium ion battery of claim 6, wherein the positive electrode comprises a positive current collector foil and a positive active powder material attached to the positive current collector foil.
8. The lithium ion battery of claim 6, wherein the separator is one of a polypropylene film, a polyethylene film, a polypropylene/polyethylene/polypropylene composite film, nylon cloth, glass fiber, and asbestos paper.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115051030A (en) * | 2022-05-18 | 2022-09-13 | 湖南大学 | Battery electrolyte and lithium ion battery |
| CN115911554A (en) * | 2022-11-18 | 2023-04-04 | 重庆太蓝新能源有限公司 | Electrolyte, battery and electric equipment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115051030A (en) * | 2022-05-18 | 2022-09-13 | 湖南大学 | Battery electrolyte and lithium ion battery |
| CN115911554A (en) * | 2022-11-18 | 2023-04-04 | 重庆太蓝新能源有限公司 | Electrolyte, battery and electric equipment |
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Application publication date: 20220506 |