CN110416626B - Formation method of lithium ion battery - Google Patents
Formation method of lithium ion battery Download PDFInfo
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- CN110416626B CN110416626B CN201910717550.8A CN201910717550A CN110416626B CN 110416626 B CN110416626 B CN 110416626B CN 201910717550 A CN201910717550 A CN 201910717550A CN 110416626 B CN110416626 B CN 110416626B
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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
- H01M10/058—Construction or manufacture
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a formation method of a lithium ion battery, the lithium ion battery can be stored for a long time in a high-temperature environment after the formation method provided by the invention, and the high-temperature cyclicity is better.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery formation method.
Background
With the acceleration of globalization and the increasing popularity of electronic products, the developing electric vehicles and the like have higher requirements on battery energy, especially energy density, rate capability and cycle performance. Lithium ion batteries are considered to be the most ideal energy storage element because they have the advantages of high energy density, long cycle life, no memory effect, and the like. The lithium ion battery is subjected to a formation process after liquid injection, gas is generated in the formation process, electrolyte loss is caused, and meanwhile, the battery needs to be replenished with liquid after the formation, so that the cost is increased; meanwhile, in the existing lithium ion battery, the activity of the positive active material is high, and the electrolyte is easy to decompose on the surface of the positive electrode to generate gas in a high-temperature environment, so that the high-temperature storage and the cycle life of the battery are influenced.
Disclosure of Invention
In view of the above problems, the present invention provides a formation method for a lithium ion battery, which can store the lithium ion battery for a long time in a high temperature environment after the formation method provided by the present invention, and has a good high temperature cyclicity, the method includes injecting a first electrolyte, then performing pre-formation in a range of a higher potential, injecting a second electrolyte after exhausting, and then performing charge and discharge cycles in a full voltage range.
The inventor finds that, after long-term research, before formal formation process, the battery is placed in a high-temperature environment, and charge and discharge cycles are performed under high potential, so that deposition of an SEI film on the surface of a positive electrode is increased, and further finds that even tiny electrode polarization can cause easy excessive decomposition of an electrolyte in a cycle process of a high potential interval under the high-temperature environment, so that a large amount of gas is generated and film forming conditions of the SEI film are influenced.
The specific scheme is as follows:
a method of formation of a lithium ion battery, the method comprising:
1) injecting the first electrolyte into a battery to be formed;
2) charging to a charging cut-off voltage by a small current constant current;
3) placing the battery at 45-55 ℃, and performing pulse charge-discharge circulation between a charge cut-off voltage and a first preset voltage, wherein the first preset voltage is lower than the charge cut-off voltage by 0.1-0.2V;
4) constant voltage charging is carried out under the charging cut-off voltage until the current is less than the first preset current;
5) standing, and then performing constant voltage charging under the charging cut-off voltage until the current is less than a first preset current;
6) repeating the step 4-5 for a plurality of times;
7) vacuumizing and exhausting, and then injecting a second electrolyte;
8) discharging at constant current till the discharge cut-off voltage;
9) standing, and then performing constant current charge-discharge circulation between a discharge cut-off voltage and a second preset voltage, wherein the second preset voltage is 0.2-0.4V higher than the discharge cut-off voltage;
10) and performing constant current circulation for several times between the discharge cut-off voltage and the charge cut-off voltage.
Further, the nonaqueous solvent in the first electrolyte is a cyclic carbonate, and the nonaqueous solvent in the second electrolyte is a chain carbonate; the volume ratio of the first electrolyte to the second electrolyte is 7:3-6: 4.
Further, the charging current in the step 2 is 0.01-0.1C.
Further, the pulse charge-discharge cycle in the step 3 is carried out in a process of pulse charging to a charge cut-off voltage, then pulse discharging to the first preset voltage, wherein the pulse current is 0.1-1C, the action time is 5-10s, and the interval time is 1/5 of the action time of the pulse.
Further, the first predetermined current is 0.02C or less.
Further, the charge cut-off voltage is 4.2-4.3V.
Further, the discharge cut-off voltage is 2.7-2.8V.
Further, the non-aqueous solvent of the first electrolyte is selected from ethyl carbonate, propyl carbonate, butyl carbonate; the non-aqueous solvent of the second electrolyte is selected from ethyl methyl carbonate, dimethyl carbonate and diethyl carbonate.
Further, the current in the step 9 is 0.1-0.5C.
The invention has the following beneficial effects:
1) before the formal formation process, the battery is placed in a high-temperature environment, and the pre-formation of charge-discharge cycle is carried out at a high potential, so that the deposition of an SEI film on the surface of the anode is increased;
2) in a barren solution state, the formation is carried out through pulse current, so that the polarization of an electrode and the decomposition condition of electrolyte can be effectively relieved, and a better SEI film is formed;
3) multiple times of constant voltage stable charging is beneficial to improving the density of an SEI film, and the stability of the battery is enhanced;
4) the cycle of the low voltage interval is beneficial to the formation of a negative electrode SEI film;
5) the non-aqueous solvent in the first electrolyte is composed of cyclic carbonate, so that the stability of the electrolyte in a high voltage range can be improved, and the chain carbonate of the second electrolyte is beneficial to adjusting the conductivity of the whole electrolyte to obtain lower internal resistance;
6) the battery prepared by the method has good high-temperature storage performance, and can keep higher cycle life and capacity retention performance after storage.
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 positive electrode of the battery adopted by the invention is (433) nickel cobalt lithium manganate, and the negative electrode is artificial graphite and natural graphite; the first electrolyte includes: 1M LiPF6Ethyl carbonate and additive VC 3% (by volume); the second electrolyte comprises 1M LiPF6Ethyl methyl carbonate and diethyl carbonate, wherein the volume ratio of ethyl methyl carbonate: diethyl carbonate 1: 1.
Example 1
1) Injecting the first electrolyte into a battery to be formed;
2) charging to 4.2V by a current of 0.01C in a constant current manner;
3) placing the battery at 55 ℃, and performing pulse charge-discharge circulation between 4.2V and 4.1V, wherein the pulse charge-discharge circulation process comprises the steps of pulse charging to 4.2V, then pulse discharging to 4.1V, pulse current of 0.1C, action time of 10s and interval time of 2s of pulse action time;
4) charging at constant voltage of 4.2V until the current is less than 0.02C;
5) standing for 2h, and then charging at constant voltage of 4.2V until the current is less than 0.02C;
6) repeating the step 4-5) for 3 times;
7) vacuumizing and exhausting, and then injecting a second electrolyte, wherein the volume ratio of the first electrolyte to the second electrolyte is 7: 3;
8) discharging the mixture to 2.7V at a constant current of 0.1C;
9) standing for 2h, and then performing constant-current charge-discharge circulation for 5 times at a current of 0.1C between 2.7V and 2.9V;
10) constant current cycle at 0.1C between 2.7V and 4.2V 5 times.
Example 2
1) Injecting the first electrolyte into a battery to be formed;
2) charging to 4.3V by a current of 0.1C in a constant current manner;
3) placing the battery at 45 ℃, and performing pulse charge-discharge circulation between 4.3V and 4.1V, wherein the pulse charge-discharge circulation process comprises the steps of pulse charging to 4.3V, then pulse discharging to 4.1V, the pulse current is 1C, the action time is 5s, and the interval time is 1s of the action time of the pulse;
4) charging at constant voltage of 4.3V until the current is less than 0.02C;
5) standing for 2h, and then charging at constant voltage of 4.3V until the current is less than 0.02C;
6) repeating the step 4-5) for 3 times;
7) vacuumizing and exhausting, and then injecting a second electrolyte, wherein the volume ratio of the first electrolyte to the second electrolyte is 6: 4;
8) discharging the mixture to 2.8V at a constant current of 0.2C;
9) standing for 1h, and then performing constant current charge-discharge circulation for 3 times at a current of 0.5C between 2.8V and 3.2V;
10) cycling 3 times between 2.8V and 4.3V with a constant current of 0.5C.
Example 3
1) Injecting the first electrolyte into a battery to be formed;
2) charging to 4.2V by a current of 0.05C in a constant current manner;
3) placing the battery at 50 ℃, and performing pulse charge-discharge circulation between 4.2V and 4.1V, wherein the pulse charge-discharge circulation process comprises the steps of pulse charging to 4.2V, then pulse discharging to 4.1V, pulse current of 0.1C, action time of 10s and interval time of 2s of pulse action time;
4) charging at constant voltage of 4.2V until the current is less than 0.01C;
5) standing for 2h, and then charging at constant voltage of 4.2V until the current is less than 0.01C;
6) repeating the step 4-5) for 3 times;
7) vacuumizing and exhausting, and then injecting a second electrolyte, wherein the volume ratio of the first electrolyte to the second electrolyte is 6: 4;
8) discharging the mixture to 2.7V at a constant current of 0.2C;
9) standing for 2h, and then performing constant-current charge-discharge circulation for 5 times at a current of 0.2C between 2.7 and 3.0V;
10) cycling 3 times between 2.7 and 4.2V with a constant current of 0.2C.
Comparative example 1
1) Injecting the first electrolyte into a battery to be formed;
2) charging to 4.2V by a current of 0.05C in a constant current manner;
3) charging at constant voltage of 4.2V until the current is less than 0.01C;
4) vacuumizing and exhausting, and then injecting a second electrolyte, wherein the volume ratio of the first electrolyte to the second electrolyte is 6: 4;
5) discharging the mixture to 2.7V at a constant current of 0.2C;
6) cycling 3 times between 2.7 and 4.2V with a constant current of 0.2C.
Comparative example 2
1) Injecting the first electrolyte into a battery to be formed;
2) charging to 4.2V by a current of 0.05C in a constant current manner;
3) charging at constant voltage of 4.2V until the current is less than 0.01C;
4) standing for 2h, and then charging at constant voltage of 4.2 until the current is less than 0.01 ℃;
5) repeating the step 3-4) for 3 times;
6) vacuumizing and exhausting, and then injecting a second electrolyte, wherein the volume ratio of the first electrolyte to the second electrolyte is 6: 4;
7) discharging the mixture to 2.7V at a constant current of 0.2C;
8) cycling 3 times between 2.7 and 4.2V with a constant current of 0.2C.
Comparative example 3
1) Injecting the first electrolyte into a battery to be formed;
2) charging to 4.2V by a current of 0.05C in a constant current manner;
3) placing the battery at 50 ℃, and performing pulse charge-discharge circulation between 4.2V and 4.1V, wherein the pulse charge-discharge circulation process comprises the steps of pulse charging to 4.2V, then pulse discharging to 4.1V, pulse current of 0.1C, action time of 10s and interval time of 2s of pulse action time;
4) vacuumizing and exhausting, and then injecting a second electrolyte, wherein the volume ratio of the first electrolyte to the second electrolyte is 6: 4;
5) discharging the mixture to 2.7V at a constant current of 0.2C;
6) standing for 2h, and then performing constant-current charge-discharge circulation for 5 times at a current of 0.2C between 2.7 and 3.0V;
7) cycling 3 times between 2.7 and 4.2V with a constant current of 0.2C.
Comparative example 4
1) Injecting the first electrolyte and the second electrolyte into a battery to be formed; the volume ratio of the first electrolyte to the second electrolyte is 6: 4;
2) charging to 4.2V by a current of 0.05C in a constant current manner;
3) placing the battery at 50 ℃, and performing pulse charge-discharge circulation between 4.2V and 4.1V, wherein the pulse charge-discharge circulation process comprises the steps of pulse charging to 4.2V, then pulse discharging to 4.1V, pulse current of 0.1C, action time of 10s and interval time of 2s of pulse action time;
4) charging at constant voltage of 4.2V until the current is less than 0.01C;
5) standing for 2h, and then charging at constant voltage of 4.2 until the current is less than 0.01 ℃;
6) repeating the step 4-5) for 3 times;
7) discharging the mixture to 2.7V at a constant current of 0.2C;
8) standing for 2h, and then performing constant-current charge-discharge circulation for 5 times at a current of 0.2C between 2.7 and 3.0V;
9) cycling 3 times between 2.7 and 4.2V with a constant current of 0.2C.
Experiment and data
The batteries of examples 1 to 3 and comparative examples 1 to 4 were stored at 55 ℃ for 60 days, then the capacity after cycling at a current of 0.1C for 3 times and 100 times was measured, and the capacity was divided by the capacity measured before storage to obtain the storage capacity retention rate and the cycle capacity retention rate, respectively. As can be seen from table 1, the pulse formation in the high potential interval, the constant voltage charge formation at high potential for a plurality of times, the fractional injection of the electrolyte, and the cycle process at low potential have different degrees of influence on the high temperature storage performance and the capacity retention rate of the battery.
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 (6)
1. A lithium ion battery formation method is provided, wherein a non-aqueous solvent of a first electrolyte is cyclic carbonate, and a non-aqueous solvent of a second electrolyte is chain carbonate; the volume ratio of the first electrolyte to the second electrolyte is 7:3-6: 4; the method comprises the following steps:
1) injecting the first electrolyte into a battery to be formed;
2) charging to a charging cut-off voltage by a small current constant current;
3) placing the battery at 45-55 ℃, and performing pulse charge-discharge circulation between a charge cut-off voltage and a first preset voltage, wherein the first preset voltage is lower than the charge cut-off voltage by 0.1-0.2V; the pulse charging and discharging cycle comprises the steps of pulse charging to a charging cut-off voltage, then pulse discharging to the first preset voltage, wherein the pulse current is 0.1-1C, the action time is 5-10s, and the interval time is 1/5 of the action time of the pulse;
4) constant voltage charging is carried out under the charging cut-off voltage until the current is less than the first preset current;
5) standing, and then performing constant voltage charging under the charging cut-off voltage until the current is less than a first preset current;
6) repeating the step 4-5 for a plurality of times;
7) vacuumizing and exhausting, and then injecting a second electrolyte;
8) discharging at constant current till the discharge cut-off voltage;
9) standing, and then performing constant current charge-discharge circulation between a discharge cut-off voltage and a second preset voltage, wherein the second preset voltage is 0.2-0.4V higher than the discharge cut-off voltage;
10) and performing constant current circulation for several times between the discharge cut-off voltage and the charge cut-off voltage.
2. The method of claim 1, wherein the charging current in step 2) is 0.01-0.1C.
3. The method of claim 1, wherein the first predetermined current is 0.02C or less.
4. The method of claim 1, wherein the charge cutoff voltage is 4.2-4.3V.
5. The method of claim 1, wherein the discharge cutoff voltage is 2.7-2.8V.
6. The method of claim 1, wherein the current in step 9) is 0.1-0.5C.
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| CN111082149A (en) * | 2019-12-18 | 2020-04-28 | 江苏智泰新能源科技有限公司 | Formation method of lithium ion battery |
| CN111162335B (en) * | 2020-01-02 | 2021-05-28 | 广州明美新能源股份有限公司 | Formation method of lithium ion battery |
| CN111129604B (en) * | 2020-01-02 | 2021-03-23 | 萧县鑫辉源电池有限公司 | Formation method of power lithium ion battery |
| CN111180794B (en) * | 2020-02-18 | 2021-01-12 | 苏州梵洁结构设计有限公司 | Storage method of power lithium ion battery |
| CN111342128B (en) * | 2020-02-18 | 2021-08-31 | 江西金晖锂电材料股份有限公司 | Formation method of low-temperature lithium ion battery |
| CN111293349B (en) * | 2020-02-19 | 2021-07-02 | 江西迪比科股份有限公司 | Formation method of lithium ion battery |
| CN111276758B (en) * | 2020-02-21 | 2021-06-29 | 江西迪比科股份有限公司 | Preparation method of lithium ion battery |
| CN111293377B (en) * | 2020-03-12 | 2021-08-24 | 江西金晖锂电材料股份有限公司 | Formation method of power battery |
| CN111342028B (en) * | 2020-03-20 | 2021-07-20 | 吉林中溢炭素科技有限公司 | Formation method of lithium ion battery with graphite-based cathode |
| CN111313118B (en) * | 2020-04-13 | 2021-07-06 | 东方醒狮储能电池有限公司 | Formation method of lithium ion battery |
| CN111313098B (en) * | 2020-04-13 | 2021-05-28 | 广州明美新能源股份有限公司 | Preparation method of lithium ion battery |
| CN111916837B (en) * | 2020-08-14 | 2021-11-30 | 江苏中奕和创智能科技有限公司 | Formation method of lithium-nickel-based composite compound battery |
| CN111916841A (en) * | 2020-09-24 | 2020-11-10 | 昆山宝创新能源科技有限公司 | Method for improving electrolyte infiltration effect of lithium battery and reducing diaphragm wrinkles and lithium battery |
| CN112103581B (en) * | 2020-09-30 | 2022-07-26 | 苏州精诚智造智能科技有限公司 | Preparation method of lithium ion battery |
| 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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