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CN112290095A - Lithium ion battery electrolyte suitable for high-nickel material system and preparation method thereof - Google Patents

Lithium ion battery electrolyte suitable for high-nickel material system and preparation method thereof Download PDF

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CN112290095A
CN112290095A CN202011153892.0A CN202011153892A CN112290095A CN 112290095 A CN112290095 A CN 112290095A CN 202011153892 A CN202011153892 A CN 202011153892A CN 112290095 A CN112290095 A CN 112290095A
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lithium
ion battery
lithium ion
electrolyte
battery electrolyte
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王鹏
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Gotion High Tech 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
    • H01M10/056—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
    • H01M10/05—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
    • H01M10/0569—Liquid materials characterised by the solvents
    • 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
    • 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
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • H01M2300/0037—Mixture of solvents
    • 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
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • H01M2300/0037—Mixture of solvents
    • H01M2300/004—Three solvents
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a lithium ion battery electrolyte suitable for a high-nickel material system and a preparation method thereof. The film-forming additive can improve the overall ionic conductivity of the electrolyte, and can provide electrons to combine with free phosphorus pentafluoride in the electrolyte to form a stable compound, so that the damage of lithium salt decomposition to a positive and negative electrode SEI film is reduced, and the cycle performance of a lithium ion battery at normal temperature and high temperature is effectively improved.

Description

Lithium ion battery electrolyte suitable for high-nickel material system and preparation method thereof
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a lithium ion battery electrolyte suitable for a high nickel material system and a preparation method thereof.
Background
With the continuous increase of world energy demand, fossil energy on the earth is increasingly consumed, thereby bringing about an increasingly prominent series of environmental problems. High-efficiency, safe, clean and renewable new energy and related technologies become hot spots of research in various countries around the world. Lithium ion batteries have a series of advantages of high voltage, high energy and power density, long cycle life, small self-discharge, environmental friendliness and the like, have become the most efficient energy storage devices at present, are widely applied to mobile electronic devices, and are expected to be developed more widely on electric vehicles and hybrid vehicles. With the technological progress and the continuous development of the market, it is increasingly important and urgent to improve the energy density of the lithium battery.
In order to improve the energy density of the lithium ion battery, researchers optimize and improve a material system and a battery preparation process, and research on a high nickel material direction becomes an important focus of attention of people. The high-nickel anode material is a nickel-containing anode material with the mole fraction of nickel in the material being more than 60%, and has the characteristics of high specific capacity, low cost and the like, but the capacity retention rate and the thermal stability of the material are relatively poor. Under high voltage and higher nickel content, the decomposition process of the conventional electrolyte is greatly accelerated, so that severe ballooning and poor cycle performance are caused; the negative electrode material can continuously form an SEI film in the long-term charge-discharge cycle process, and active lithium is continuously consumed to cause another factor of capacity retention rate reduction. Therefore, under the condition that the material system is kept unchanged, the optimization of the formula of the lithium ion battery electrolyte is an important way for improving the high nickel system battery. The currently used solutions mainly include the development of solvent systems with higher electrochemical stability windows and the addition of film-forming additives that stabilize the SEI film, thereby inhibiting the interaction of the electrolyte and the electrode materials. However, many additive developments can not meet the overall performance indexes such as conductivity, film forming strength and stability, so that further optimization development of electrolyte formula and additives is an urgent need for improving the cycle performance of lithium ion batteries.
Disclosure of Invention
The invention aims to provide a lithium ion battery electrolyte suitable for a high-nickel material system and a preparation method thereof, which can improve the cycle performance of a lithium ion battery at normal temperature and high temperature.
The technical scheme of the invention is as follows:
the lithium ion battery electrolyte suitable for the high nickel material system comprises an organic solvent, a lithium salt electrolyte, an additive and a film forming additive, wherein the film forming additive is a benzotriazole alkyl sulfonic acid lithium hexafluorophosphate compound, and the chemical structural formula of the lithium ion battery electrolyte is as follows:
Figure BDA0002742090000000021
wherein in the chemical structural formula, R1 and R2 are respectively and independently selected from F or C1-5Alkyl group of (1).
The mass of the lithium salt electrolyte accounts for 9-15% of the total mass of the lithium ion battery electrolyte.
The mass ratio of the additive to the film forming additive is 1: (0.5-1), wherein the total mass of the forming additive and the film forming additive accounts for 0.1-5% of the total mass of the lithium ion battery electrolyte.
The lithium compound of benzotriazole alkyl sulfonate hexafluorophosphate is lithium benzotriazole propyl sulfonate hexafluorophosphate or lithium benzotriazole fluoropropyl sulfonate hexafluorophosphate.
The organic solvent is at least one of ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, 1, 4-butyrolactone, methyl ethyl carbonate, dimethyl ether, diphenyl sulfide, acetonitrile, glutaronitrile, sulfolane and methyl propionate.
The organic solvent is prepared from ethylene carbonate, diethyl carbonate and methyl ethyl carbonate according to the mass ratio of (20-30) to (30-50): (30-50) a mixed solvent.
The lithium salt electrolyte is at least one of lithium hexafluorophosphate, lithium difluorooxalato borate, lithium tetrafluoroborate and lithium bis-fluorosulfonylimide.
The additive is at least one of tris (trimethylsilane) phosphate, vinylene carbonate and fluoroethylene carbonate.
A preparation method of lithium ion battery electrolyte comprises the steps of firstly weighing an organic solvent according to a weight ratio, mixing and stirring uniformly, then weighing a lithium salt electrolyte according to a weight ratio, fully dissolving the lithium salt electrolyte in the organic solvent, finally weighing an additive and a film forming additive according to a weight ratio, and sequentially adding the additives and the film forming additive into the organic solvent to be mixed to obtain the lithium ion battery electrolyte.
The invention has the advantages that:
(1) the organic solvent is a mixed solvent formed by mixing ethylene carbonate, diethyl carbonate and ethyl methyl carbonate, has a higher electrochemical window, and maintains the chemical stability of the high-nickel material system battery cell under high voltage.
(2) On one hand, the inherent sulfonic acid functional group of the film forming additive has larger dipole moment, and can combine and dissociate lithium ions in the electrolyte, so that the overall ionic conductivity of the electrolyte is improved; on the other hand, the benzotriazole alkyl lithium hexafluorophosphate can provide electrons to be combined with free phosphorus pentafluoride in the electrolyte to form a stable compound, so that the damage of lithium salt decomposition to the SEI film of the positive and negative electrodes is reduced, the electrolyte stabilizer effect is achieved, and the stability effect of the SEI film in the long-term circulation process of the battery cell is improved.
(3) The additive disclosed by the invention is combined with a film forming additive for use, so that the stability and low impedance characteristics of an SEI film are ensured, and the performance of a lithium ion battery under a high-temperature condition is better exerted.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Preparation of lithium benzotriazolylpropylsulfonate hexafluorophosphate: firstly, adding 0.5mol of benzotriazole into a glass reaction kettle, then adding 200ml of anhydrous acetone, uniformly mixing, then adding 0.5mol of propane sultone into the glass reaction kettle, heating and reacting for 36 hours at 60 ℃ under the protection of nitrogen, filtering to remove filtrate, washing the obtained white solid with anhydrous acetone for three times, and drying in vacuum to obtain benzotriazole propanesulfonic acid inner salt; dissolving the dried benzotriazole propanesulfonic acid inner salt and lithium hexafluorophosphate with an equal molar ratio in dried dimethyl carbonate, heating and stirring at 60 ℃ for 24 hours under the protection of nitrogen, and then removing the dimethyl carbonate by decompression and concentration to obtain the benzotriazole propyl sulfonic acid lithium hexafluorophosphate.
Example 1
A preparation method of a lithium ion battery electrolyte suitable for a high-nickel material system comprises the steps of firstly weighing ethylene carbonate, diethyl carbonate and methyl ethyl carbonate according to the mass ratio of 30:30:40, uniformly mixing to obtain an organic solvent, fully dissolving lithium hexafluorophosphate in the organic solvent, adding vinylene carbonate accounting for 2% of the mass fraction of the whole electrolyte, adding benzotriazole propyl lithium sulfonate accounting for 1.1% of the mass fraction of the whole electrolyte, and mixing to obtain an electrolyte 1; wherein the mass of lithium hexafluorophosphate was 14% of the total electrolyte solution 1 mass. The above steps are all carried out in a glove box filled with inert gas.
Preparing a lithium ion battery by using the electrolyte 1:
(1) preparation of positive plate
The method comprises the following steps of mixing a positive electrode active substance high nickel material NMC811, acetylene black (a conductive agent) and polyvinylidene fluoride (a binder) according to a mass ratio of NMC 811: acetylene black: polytetrafluoroethylene 96: 1.5: 2.5, adding N-methyl pyrrolidone, fully stirring and uniformly mixing, uniformly coating the formed uniform anode slurry on an aluminum foil with the thickness of 16 microns, and drying to obtain an anode plate;
(2) preparation of negative plate
Preparing the following raw materials by mass: acetylene black: styrene-butadiene rubber: thickener 96: 1.5: 1.5: 1, mixing, adding deionized water, fully stirring to form uniform negative electrode slurry, coating the uniform negative electrode slurry on a copper foil with the thickness of 8 microns, and drying to obtain a negative electrode sheet;
(3) preparation of experimental lithium battery
And controlling the dew point to be below-40 ℃ in a drying environment, stacking the prepared positive pole piece, negative pole piece and diaphragm in sequence, making a coiled core by a pole piece winding machine, encapsulating the coiled core in an aluminum plastic film with a glue tab to form a soft package battery to be injected, injecting the prepared electrolyte into the soft package battery, and sequentially sealing, forming, aging and grading to obtain the experimental lithium battery for testing.
Example 2
A preparation method of a lithium ion battery electrolyte suitable for a high-nickel material system comprises the steps of firstly weighing ethylene carbonate, diethyl carbonate and methyl ethyl carbonate according to the mass ratio of 30:30:40, uniformly mixing to obtain an organic solvent, fully dissolving lithium hexafluorophosphate in the organic solvent, adding vinylene carbonate accounting for 2% of the mass fraction of the whole electrolyte, adding benzotriazole propyl lithium sulfonate accounting for 1.3% of the mass fraction of the whole electrolyte, and mixing to obtain an electrolyte 2; wherein the mass of lithium hexafluorophosphate was 14% of the mass of the entire electrolyte solution 2. The above steps are all carried out in a glove box filled with inert gas.
An experimental lithium cell was prepared using electrolyte 2, in the same manner as in example 1.
Example 3
A preparation method of a lithium ion battery electrolyte suitable for a high-nickel material system comprises the steps of firstly weighing ethylene carbonate, diethyl carbonate and methyl ethyl carbonate according to the mass ratio of 30:30:40, uniformly mixing to obtain an organic solvent, fully dissolving lithium hexafluorophosphate in the organic solvent, adding vinylene carbonate accounting for 2% of the mass fraction of the whole electrolyte, adding benzotriazole propyl lithium sulfonate accounting for 1.5% of the mass fraction of the whole electrolyte, and mixing to obtain an electrolyte 3; wherein the mass of lithium hexafluorophosphate was 14% of the mass of the entire electrolyte solution 3. The above steps are all carried out in a glove box filled with inert gas.
Experimental lithium cells were prepared using electrolyte 3 in the same manner as in example 1.
Example 4
A preparation method of a lithium ion battery electrolyte suitable for a high-nickel material system comprises the steps of firstly weighing ethylene carbonate, diethyl carbonate and methyl ethyl carbonate according to the mass ratio of 30:30:40, uniformly mixing to obtain an organic solvent, fully dissolving lithium hexafluorophosphate in the organic solvent, adding vinylene carbonate accounting for 2% of the mass fraction of the whole electrolyte, adding benzotriazole fluoropropyl lithium sulfonate accounting for 1.1% of the mass fraction of the whole electrolyte, and mixing to obtain an electrolyte 4; wherein the mass of lithium hexafluorophosphate was 14% of the total electrolyte 4 mass. The above steps are all carried out in a glove box filled with inert gas.
An experimental lithium cell was prepared using electrolyte 4, in the same manner as in example 1.
Comparative example 1
A preparation method of lithium ion battery electrolyte comprises the steps of firstly weighing ethylene carbonate, diethyl carbonate and ethyl methyl carbonate according to the mass ratio of 30:30:40, uniformly mixing to obtain an organic solvent, fully dissolving lithium hexafluorophosphate in the organic solvent, adding vinylene carbonate accounting for 2% of the mass fraction of the whole electrolyte, and mixing to obtain an electrolyte 5; wherein the mass of lithium hexafluorophosphate was 14% of the total electrolyte 5 mass. The above steps are all carried out in a glove box filled with inert gas.
An experimental lithium cell was prepared using electrolyte 5, in the same manner as in example 1.
Comparative example 2
A preparation method of lithium ion battery electrolyte comprises the steps of firstly weighing ethylene carbonate, diethyl carbonate and ethyl methyl carbonate according to the mass ratio of 30:30:40, uniformly mixing to obtain an organic solvent, fully dissolving lithium hexafluorophosphate in the organic solvent, adding vinylene carbonate accounting for 1% of the mass fraction of the whole electrolyte, adding tris (trimethylsilane) phosphate accounting for 1% of the mass fraction of the whole electrolyte, and mixing to obtain an electrolyte 6; wherein the mass of lithium hexafluorophosphate was 14% of the total electrolyte 5 mass. The above steps are all carried out in a glove box filled with inert gas.
An experimental lithium cell was prepared using electrolyte 6, in the same manner as in example 1.
And (3) testing the conductivity of the electrolyte and the cycle performance of the battery:
(1) and detecting the conductivity of the electrolyte: conductivity tests were performed on the electrolyte samples prepared in examples 1 to 4 and comparative examples 1 to 2 using a conductivity meter at 25 ℃ and 45 ℃, 3 parallel tests were performed for each sample measurement, and the average value was taken as a result, and the relevant comparative data are shown in the following table;
(2) and testing charge-discharge cycle: the experimental lithium batteries prepared in examples 1 to 4 and comparative examples 1 to 2 were subjected to 1C constant volume at room temperature, and then placed in a thermostat at 25 ℃ to perform 1C charge and discharge tests, wherein the voltage interval was 3.0 to 4.2V, the rest time was 60min, the discharge capacity was recorded, and the cell capacity retention rates at 100 weeks and 500 weeks were calculated, respectively, and the specific test results are shown in the following table.
Figure BDA0002742090000000061
Figure BDA0002742090000000071
From the comparison data and the test results, the electrolyte prepared by the invention is added with the benzotriazole alkyl sulfonic acid lithium hexafluorophosphate compound, so that the ionic conductivity of the electrolyte at normal temperature and high temperature can be effectively improved, the cycle performance of the lithium ion battery is improved, the addition amount is small, and the cost can be well controlled, so that the electrolyte is a novel multifunctional film forming additive.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. The lithium ion battery electrolyte suitable for the high nickel material system is characterized in that: the lithium ion battery electrolyte comprises an organic solvent, a lithium salt electrolyte, an additive and a film forming additive, wherein the film forming additive is a benzotriazole alkyl sulfonic acid lithium hexafluorophosphate compound, and the chemical structural formula of the lithium ion battery electrolyte is as follows:
Figure FDA0002742089990000011
wherein in the chemical structural formula, R1 and R2 are respectively and independently selected from F or C1-5Alkyl group of (1).
2. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 1, wherein: the mass of the lithium salt electrolyte accounts for 9-15% of the total mass of the lithium ion battery electrolyte.
3. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 1, wherein: the mass ratio of the additive to the film forming additive is 1: (0.5-1), wherein the total mass of the forming additive and the film forming additive accounts for 0.1-5% of the total mass of the lithium ion battery electrolyte.
4. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 1, wherein: the lithium compound of benzotriazole alkyl sulfonate hexafluorophosphate is lithium benzotriazole propyl sulfonate hexafluorophosphate or lithium benzotriazole fluoropropyl sulfonate hexafluorophosphate.
5. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 1, wherein: the organic solvent is at least one of ethylene carbonate, propylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, 1, 4-butyrolactone, methyl ethyl carbonate, dimethyl ether, diphenyl sulfide, acetonitrile, glutaronitrile, sulfolane and methyl propionate.
6. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 5, wherein: the organic solvent is prepared from ethylene carbonate, diethyl carbonate and methyl ethyl carbonate according to the mass ratio of (20-30) to (30-50): (30-50) a mixed solvent.
7. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 1, wherein: the lithium salt electrolyte is at least one of lithium hexafluorophosphate, lithium difluorooxalato borate, lithium tetrafluoroborate and lithium bis-fluorosulfonylimide.
8. The lithium ion battery electrolyte suitable for the high nickel material system according to claim 1, wherein: the additive is at least one of tris (trimethylsilane) phosphate, vinylene carbonate and fluoroethylene carbonate.
9. The method of preparing the lithium ion battery electrolyte of claim 1, wherein: firstly, weighing the organic solvent according to the weight ratio, mixing and stirring uniformly, then weighing the lithium salt electrolyte according to the weight ratio, fully dissolving the lithium salt electrolyte in the organic solvent, finally weighing the additive and the film-forming additive according to the weight ratio, and sequentially adding the additives and the film-forming additive into the organic solvent to be mixed to obtain the lithium ion battery electrolyte.
CN202011153892.0A 2020-10-26 2020-10-26 Lithium ion battery electrolyte suitable for high-nickel material system and preparation method thereof Pending CN112290095A (en)

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