CN112331920A - Formation method of lithium ion battery - Google Patents
Formation method of lithium ion battery Download PDFInfo
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- CN112331920A CN112331920A CN202011256629.4A CN202011256629A CN112331920A CN 112331920 A CN112331920 A CN 112331920A CN 202011256629 A CN202011256629 A CN 202011256629A CN 112331920 A CN112331920 A CN 112331920A
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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
- 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
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
- H01M10/446—Initial charging measures
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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
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- Condensed Matter Physics & Semiconductors (AREA)
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- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a formation method of a lithium ion battery, wherein electrolyte of the lithium ion battery comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and alpha, alpha-dimethyl-gamma-butyrolactone; injecting the electrolyte into a battery to be injected, charging to a first preset voltage at a constant current, then performing pulse charge-discharge circulation for a plurality of times between the first preset voltage and a second preset voltage, vacuumizing and exhausting during the pulse charge-discharge circulation, then charging to a charge cut-off voltage at the constant current, standing, then performing charge-discharge circulation for a plurality of times at the charge cut-off voltage and the discharge cut-off voltage, vacuumizing and exhausting, and sealing to obtain the battery; the lithium ion battery obtained by the formation method has good high-temperature performance and low-temperature performance.
Description
Technical Field
The invention relates to a formation method of a lithium ion battery.
Background
The lithium ion battery has good safety performance and cycle life, but the use temperature window is not very wide, the low-temperature performance of the common high-temperature battery is poor, and the high-temperature capacity retention rate of the low-temperature battery is poor, because of the limitation of the battery electrolyte, the high-temperature performance and the low-temperature performance are difficult to be considered. The invention provides an electrolyte of a battery and a corresponding formation method, which can enable a lithium ion battery to have good high-temperature performance and low-temperature performance.
Disclosure of Invention
The invention provides a formation method of a lithium ion battery, wherein electrolyte of the lithium ion battery comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone, wherein the volume concentration of the additives satisfies the following relationship, (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone): volume of linear carbonate ═ k ═ divinyl sulfone ═ volume of cyclic carbonate, wherein k ═ 1.62 to 1.65; injecting the electrolyte into a battery to be injected, charging to a first preset voltage at a constant current, then performing pulse charge-discharge circulation for a plurality of times between the first preset voltage and a second preset voltage, vacuumizing and exhausting during the pulse charge-discharge circulation, then charging to a charge cut-off voltage at the constant current, standing, then performing charge-discharge circulation for a plurality of times at the charge cut-off voltage and the discharge cut-off voltage, vacuumizing and exhausting, and sealing to obtain the battery; the lithium ion battery obtained by the formation method has good high-temperature performance and low-temperature performance.
The specific scheme is as follows:
the invention relates to a formation method of a lithium ion battery, which comprises the following steps:
1) injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone, wherein the volume concentration of the additives satisfies the following relationship, (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone): volume of linear carbonate ═ k ═ divinyl sulfone ═ volume of cyclic carbonate, wherein k ═ 1.62 to 1.65;
2) charging to a first preset voltage by constant current;
3) performing charge-discharge cycle for several times between a first preset voltage and a second preset voltage, and vacuumizing and exhausting gas during the charge-discharge cycle;
4) charging at constant current to a charge cut-off voltage;
5) standing the mixture for a while,
6) performing charge-discharge cycles at the charge cut-off voltage and the discharge cut-off voltage for several times;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Further, the volume concentration of the fluoroethylene carbonate is: the volume concentration of α, α -dimethyl- γ -butyrolactone was 1: 1.6.
Further, the volume concentration of the divinyl sulfone is 2.4-2.6%.
Further, the linear carbonate accounts for 50-55% of the total electrolyte volume, and the remainder is cyclic carbonate.
Further, the first predetermined voltage is 3.72V, and the second predetermined voltage is 3.85V.
Further, the step 3 is to perform pulse charge-discharge cycle 3-5 times between a first predetermined voltage and a second predetermined voltage, wherein the pulse current is 0.1-0.2C, the pulse action time is 120-200s, the interval is 20-30s, and the battery is evacuated and exhausted during the interval.
Further, the linear carbonate is selected from dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate.
Further, the cyclic carbonate is selected from ethylene carbonate and propylene carbonate.
Further, the discharge cut-off voltage is 2.75V; the charge cut-off voltage was 4.20V.
The invention has the following beneficial effects:
1) the inventors found that when fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone are contained in the electrolyte and the volume concentrations thereof satisfy the following relationship, (the volume concentration of fluoroethylene carbonate + the volume concentration of α, α -dimethyl- γ -butyrolactone) — the volume of linear carbonate ═ k ═ divinyl sulfone ═ cyclic carbonate volume, where k ═ 1.62 to 1.65, the cell can have both good high-temperature cycle performance and low-temperature cycle performance;
2) and, when a specific additive is formed in a specific voltage interval, sufficient exhaust is possible to form a stable SEI film, thereby further improving the cycle performance of the battery;
3) the formation process is simple, the formation process can be completed only by carrying out charge-discharge circulation in two voltage intervals, the formation process is simplified, and the formation time is shortened.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples. The linear carbonate used in the present invention is selected from ethyl methyl carbonate; the cyclic carbonate is selected from ethylene carbonate. The electrolyte salt is 1mol/L lithium hexafluorophosphate.
Example 1
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone, wherein the volume concentration of the additives satisfies the following relationship, (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone): volume of linear carbonate ═ k ═ divinyl sulfone ═ volume of cyclic carbonate, wherein k ═ 1.62; volume concentration of fluoroethylene carbonate: the volume concentration of alpha, alpha-dimethyl-gamma-butyrolactone is 1:1.6, the volume concentration of divinyl sulfone is 2.4%, the volume concentration of fluoroethylene carbonate is 1.50%, and the volume concentration of alpha, alpha-dimethyl-gamma-butyrolactone is 2.39%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 3 times, wherein the pulse current is 0.1C, the pulse action time is 120s, the interval is 20s, and vacuumizing and exhausting are performed on the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing;
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Example 2
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 55% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone, wherein the volume concentration of the additives satisfies the following relationship, (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone): volume of linear carbonate ═ k ═ divinyl sulfone ═ volume of cyclic carbonate, wherein k ═ 1.65; volume concentration of fluoroethylene carbonate: the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 1:1.6, the volume concentration of the divinyl sulfone is 2.6%, the volume concentration of the fluoroethylene carbonate is 1.35%, and the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 2.16%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 5 times, wherein the pulse current is 0.2C, the pulse action time is 200s, the interval is 30s, and vacuumizing and exhausting are performed on the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing;
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Example 3
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone, wherein the volume concentration of the additives satisfies the following relationship, (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone): volume of linear carbonate ═ k ═ divinyl sulfone ═ volume of cyclic carbonate, wherein k ═ 1.64; volume concentration of fluoroethylene carbonate: the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 1:1.6, the volume concentration of the divinyl sulfone is 2.5%, the volume concentration of the fluoroethylene carbonate is 1.58%, and the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 2.52%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Comparative example 1
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additives are divinyl sulfone and alpha, alpha-dimethyl-gamma-butyrolactone, wherein the volume concentration of the divinyl sulfone is 2.5%, and the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 2.52%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Comparative example 2
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additive is fluoroethylene carbonate and alpha, alpha-dimethyl-gamma-butyrolactone, wherein the volume concentration of fluoroethylene carbonate is 1.58%, and the volume concentration of alpha, alpha-dimethyl-gamma-butyrolactone is 2.52%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Comparative example 3
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additive is fluoroethylene carbonate and divinyl sulfone, wherein the volume concentration of the divinyl sulfone is 2.5%, and the volume concentration of the fluoroethylene carbonate is 1.58%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Comparative example 4
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additive comprises fluoroethylene carbonate, divinyl sulfone and alpha, alpha-dimethyl-gamma-butyrolactone, wherein the volume concentration of the divinyl sulfone is 2.5%, the volume concentration of the fluoroethylene carbonate is 1%, and the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 3%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Comparative example 5
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additive comprises fluoroethylene carbonate, divinyl sulfone and alpha, alpha-dimethyl-gamma-butyrolactone, wherein the volume concentration of the divinyl sulfone is 2%, the volume concentration of the fluoroethylene carbonate is 1.58%, and the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 2.52%;
2) charging to 3.72V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.72V and 3.85V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Comparative example 6
1) Injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; the linear carbonate accounts for 50% of the total volume of the electrolyte, and the rest is cyclic carbonate; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and alpha, alpha-dimethyl-gamma-butyrolactone, wherein the volume concentration of the divinyl sulfone is 2.5%, the volume concentration of the fluoroethylene carbonate is 1.58%, and the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 2.52%;
2) charging to 3.4V at 0.1C constant current;
3) performing pulse charge-discharge cycle at 0.1C between 3.4V and 3.5V for 4 times, wherein the pulse current is 0.15C, the pulse action time is 150s, the interval is 25s, and vacuumizing and exhausting the battery during the interval;
4) charging to 4.20V at 0.1C constant current;
5) standing the mixture for a while,
6)0.2C was cycled 3 times at 4.20V and 2.75V;
7) and vacuumizing, exhausting and sealing to obtain the battery.
Test and results
The batteries formed in examples 1 to 3 and comparative examples 1 to 6 were tested, and the capacity retention rate was measured after 300 cycles of charge and discharge at 1C rate in low-temperature and high-temperature environments of 0 ℃ and 50 ℃, respectively. As can be seen from table 1, when fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone are contained in the electrolyte and the volume concentrations thereof satisfy the following relationship (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone) × volume of linear carbonate ═ volume of divinyl sulfone cyclic carbonate, where k ═ 1.62 to 1.65, volume concentration of fluoroethylene carbonate: the volume concentration of the alpha, alpha-dimethyl-gamma-butyrolactone is 1:1.6, and the battery has good high-temperature cycle performance and low-temperature cycle performance; when the formation is performed in a specific voltage range, the cycle performance of the battery is further improved.
TABLE 1
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.
Claims (8)
1. A formation method of a lithium ion battery is characterized by comprising the following steps:
1) injecting electrolyte into a battery to be injected, wherein the electrolyte comprises linear carbonate, cyclic carbonate, electrolyte salt and an additive; wherein the additives comprise fluoroethylene carbonate, divinyl sulfone and α, α -dimethyl- γ -butyrolactone, wherein the volume concentration of the additives satisfies the following relationship, (volume concentration of fluoroethylene carbonate + volume concentration of α, α -dimethyl- γ -butyrolactone): volume of linear carbonate ═ k ═ divinyl sulfone ═ volume of cyclic carbonate, wherein k ═ 1.62 to 1.65;
2) charging to a first preset voltage by constant current;
3) performing charge-discharge cycle for several times between a first preset voltage and a second preset voltage, and vacuumizing and exhausting gas during the charge-discharge cycle;
4) charging at constant current to a charge cut-off voltage;
5) standing the mixture for a while,
6) performing charge-discharge cycles at the charge cut-off voltage and the discharge cut-off voltage for several times;
7) and vacuumizing, exhausting and sealing to obtain the battery.
2. The method of the preceding claim, wherein the volume concentration of fluoroethylene carbonate is: the volume concentration of α, α -dimethyl- γ -butyrolactone was 1: 1.6.
3. The process of the preceding claim, wherein the volume concentration of divinyl sulfone is from 2.4 to 2.6%.
4. The method of the preceding claim, wherein the linear carbonate comprises 50-55% by volume of the total electrolyte, with the remainder being cyclic carbonate.
5. The method of the preceding claim, wherein the first predetermined voltage is 3.72V and the second predetermined voltage is 3.85V.
6. The method as claimed in the above claim, wherein the step 3 is to perform a pulse charge-discharge cycle between a first predetermined voltage and a second predetermined voltage for 3-5 times, wherein the pulse current is 0.1-0.2C, the pulse duration is 120-200s, and the interval is 20-30s, and the battery is evacuated during the interval.
7. The process of the preceding claim, wherein the linear carbonate is selected from the group consisting of dimethyl carbonate, diethyl carbonate, and ethyl methyl carbonate.
8. The process according to the preceding claim, wherein the cyclic carbonate is selected from ethylene carbonate, propylene carbonate.
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| CN202011256629.4A CN112331920A (en) | 2020-11-11 | 2020-11-11 | Formation method of lithium ion battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112909317A (en) * | 2021-02-06 | 2021-06-04 | 苏州酷卡环保科技有限公司 | Aging method of lithium ion battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112909317A (en) * | 2021-02-06 | 2021-06-04 | 苏州酷卡环保科技有限公司 | Aging method of lithium ion battery |
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