CN110911767A - Formation method of lithium ion battery with composite anode - Google Patents

Formation method of lithium ion battery with composite anode Download PDF

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Publication number
CN110911767A
CN110911767A CN201911227299.3A CN201911227299A CN110911767A CN 110911767 A CN110911767 A CN 110911767A CN 201911227299 A CN201911227299 A CN 201911227299A CN 110911767 A CN110911767 A CN 110911767A
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voltage
charging
constant current
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constant
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王现思
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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
    • H01M10/4242—Regeneration of electrolyte or reactants
    • 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
    • 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
    • H01M10/448—End of discharge regulating measures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a formation method of a lithium ion battery with a composite positive electrode, wherein an active material of the composite positive electrode comprises LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2Wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (1) is 8-12:6-15:2-3: 4-6; the formation method comprises opening pre-formation, wherein the pre-formation comprises injecting electrolyte, and the electrolyte comprises 3-5% of fluoroethylene carbonate FEC by volume; discharging to a discharge cutoff voltage; lowering battery temperatureA low current charge-discharge cycle between a discharge cutoff voltage and a first predetermined voltage; charging the constant current pulse to a second preset voltage, and charging the constant current pulse at the second preset voltage; charging the battery at a constant current to a third preset voltage, and charging the battery at a constant voltage of the third preset voltage; charging the battery at a constant current to a fourth preset voltage and charging the battery at a constant voltage of the fourth preset voltage; charging the battery at a constant current to a fifth preset voltage, and charging the battery at a constant voltage of the fifth preset voltage; charging the constant current pulse to a charge cut-off voltage, and charging the constant current pulse at the charge cut-off voltage; and discharging at constant current to a fifth preset voltage, adjusting the current to continue discharging at constant current to a second preset voltage, adjusting the current to continue discharging at constant current to a discharge cut-off voltage, sealing, and finishing the pre-formation process.

Description

Formation method of lithium ion battery with composite anode
Technical Field
The invention relates to a formation method of a lithium ion battery with a composite positive electrode.
Background
In order to meet the requirements of high-power electric devices on power supplies of electric automobiles, lithium ion batteries with composite anodes have been produced, the lithium ion batteries with composite anodes have high energy density, good rate capability, high working voltage and lower cost, and are favored by manufacturers.
Disclosure of Invention
In view of the above problems, the present invention provides a method for forming a lithium ion battery having a composite positive electrode whose active material includes LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2Wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (1) is 8-12:6-15:2-3: 4-6; the formation method is opening pre-formation, and the pre-formation comprises the steps of injecting electrolyte, wherein the electrolyte comprises 3-5% of fluoroethylene carbonate FEC by volume; discharging to a discharge cutoff voltage, then reducing the battery temperature, and performing a low-current charge-discharge cycle between the discharge cutoff voltage and a first predetermined voltage; charging the constant current pulse to a second preset voltage, and charging the constant current pulse at the second preset voltage; charging the battery at a constant current to a third preset voltage, and charging the battery at a constant voltage of the third preset voltage; charging the battery at a constant current to a fourth preset voltage and charging the battery at a constant voltage of the fourth preset voltage; charging the battery at a constant current to a fifth preset voltage, and charging the battery at a constant voltage of the fifth preset voltage; charging the constant current pulse to a charge cut-off voltage, and charging the constant current pulse at the charge cut-off voltage; discharging the constant current to a fifth predetermined voltage,and adjusting the current to continue constant current discharge to a second preset voltage, adjusting the current to continue constant current discharge to a discharge cut-off voltage, sealing, and finishing the pre-formation process.
The specific scheme is as follows:
a formation method of a lithium ion battery with a composite positive electrode, wherein an active material of the composite positive electrode comprises LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2Wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (1) is 8-12:6-15:2-3: 4-6; the formation method is opening pre-formation, and the pre-formation comprises the steps of injecting electrolyte, wherein the electrolyte comprises 3-5% of fluoroethylene carbonate FEC by volume; discharging to a discharge cutoff voltage, then reducing the battery temperature, and performing a low-current charge-discharge cycle between the discharge cutoff voltage and a first predetermined voltage; charging the constant current pulse to a second preset voltage, and charging the constant current pulse at the second preset voltage; charging the battery at a constant current to a third preset voltage, and charging the battery at a constant voltage of the third preset voltage; charging the battery at a constant current to a fourth preset voltage and charging the battery at a constant voltage of the fourth preset voltage; charging the battery at a constant current to a fifth preset voltage, and charging the battery at a constant voltage of the fifth preset voltage; charging the constant current pulse to a charge cut-off voltage, and charging the constant current pulse at the charge cut-off voltage; and discharging at constant current to a fifth preset voltage, adjusting the current to continue discharging at constant current to a second preset voltage, adjusting the current to continue discharging at constant current to a discharge cut-off voltage, sealing, and finishing the pre-formation process.
The chemical conversion method according to claim 1, wherein the discharge cutoff voltage is 2.75V, the first predetermined voltage is 2.85V, and the charge cutoff voltage is 4.25V.
The formation method according to claim 2, wherein the second predetermined voltage is 3.60V, the third predetermined voltage is 3.67V, the fourth predetermined voltage is 3.72V, the fifth predetermined voltage is 3.80V,
a method of formation according to claims 1-3, the pre-formation consisting of the steps of:
1) injecting an electrolyte comprising 3-5% by volume fluoroethylene carbonate FEC;
2) discharging at 0.01-0.02 deg.C to discharge cut-off voltage;
3) adjusting the temperature of the battery to be 5-10 ℃, and performing constant current charge-discharge circulation at 0.01-0.02 ℃ between the discharge cut-off voltage and a first preset voltage;
4) charging to a second preset voltage by constant current pulse at 0.1-0.2C, wherein the pulse time is 30-60s, the interval is 3-5s, and charging at a second preset voltage and constant voltage until the charging current is lower than 0.01C;
5) charging to a third preset voltage by a constant current of 0.1-0.2C, and charging to a constant voltage by the third preset voltage until the charging current is lower than 0.01C;
6) charging to a fourth preset voltage by a constant current of 0.1-0.2C, and charging to a constant voltage by the fourth preset voltage until the charging current is lower than 0.01C;
7) charging to a fifth preset voltage by a constant current of 0.1-0.2C, and charging to a constant voltage by the fifth preset voltage until the charging current is lower than 0.01C;
8) charging to a charge cut-off voltage by constant current pulse of 0.1-0.2C, wherein the pulse time is 30-60s, the interval is 3-5s, and charging to a constant voltage by the charge cut-off voltage until the charge current is lower than 0.01C;
9) discharging at constant current of 0.02-0.09 deg.C to fifth preset voltage, regulating current to 0.1-0.2, continuing to discharge at constant current to second preset voltage, and regulating current to 0.02-0.1 deg.C, continuing to discharge at constant current to discharge cut-off voltage;
10) and (7) sealing.
The method of the preceding claim, the electrolyte comprising EC, DEC, EMC as an organic solvent in a volume ratio of 2:1: 1.
The method as claimed in the preceding claim, wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (1) to (2) is 9:12:2: 5;
the method of claim, further comprising a constant current charge-discharge cycle between a charge cutoff voltage and a discharge cutoff voltage after capping.
The method of the preceding claim, said electrolyte comprising 4% by volume fluoroethylene carbonate FEC.
The invention has the following beneficial effects:
1) different constant voltage charging platforms are arranged aiming at specific active substances, wherein the second to fifth preset voltages correspond to different voltage platforms of the four materials, the reaction power of the materials is high under the voltage, the reaction speed at the electrode can be slowed down by adopting constant voltage charging, so that an SEI film can be formed smoothly, meanwhile, the electrode polarization of the materials can be reduced by constant voltage under the voltage, and the battery materials can be activated fully;
2) in a specific voltage interval at the initial formation stage, the low-current formation is adopted, so that a stable SEI film can be formed at the initial formation stage under a low potential, and the overflow of a large amount of gas caused by an excessively high gas generation speed is avoided;
3) in the voltage range outside the working voltage platform of the active material, the electrode polarization is avoided by adopting the pulse formation, so that a more stable SEI film is formed; in the discharging process, the discharging current is designed according to the range of the discharging voltage platform, so that the voltage can be stably reduced, and the speed of the pre-formation is improved.
4) The formation method of the present invention can improve the cycle life of the composite electrode of the present invention only for the specific composite electrode of the present invention, and does not have an obvious improvement effect for other electrodes.
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 active material of the composite positive electrode comprises LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2Wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (a) to (b) in example 1 is 8:6:2: 4; 12:15:3:6 in example 2; example 3 was 9:12:2: 5; the electrolyte for injection contains 1M lithium hexafluorophosphate and EC, DEC and EMC in a volume ratio of 2:1:1 as organic solvents; the negative electrode is an artificial graphite negative electrode.
Example 1
1) Injecting an electrolyte, the electrolyte further comprising 3% by volume fluoroethylene carbonate FEC;
2)0.01C to 2.75V;
3) regulating the temperature of the battery to 5 ℃, and performing charge-discharge circulation for 3 times at a constant current of 0.01 ℃ between 2.75 and 2.85V;
4) charging to 3.60V by 0.1C constant current pulse, wherein the pulse time is 30s, the interval is 3s, and charging at 3.60V constant voltage until the charging current is lower than 0.01C;
5) charging to 3.67V at a constant current of 0.1C and charging at a constant voltage of 3.67V until the charging current is lower than 0.01C;
6) charging to 3.72V at constant current of 0.1C and charging at constant voltage of 3.72V until the charging current is lower than 0.01C;
7) charging to 3.80V at constant current of 0.1C and charging at constant voltage of 3.80V until the charging current is lower than 0.01C;
8) charging to 4.25V with 0.1C constant current pulse, pulse time 30s, interval 3s, and charging with 4.25V constant voltage until the charging current is lower than 0.01C;
9) discharging to 3.80V at constant current of 0.02C, adjusting current to 0.1, continuing to discharge to 3.60V at constant current, and adjusting current to 0.02C, continuing to discharge to 2.75V at constant current;
10) sealing;
11) charging and discharging 3 times at 0.2C constant current between 2.75-4.25V.
Example 2
1) Injecting an electrolyte, the electrolyte further comprising 5% by volume fluoroethylene carbonate FEC;
2)0.02C to 2.75V;
3) regulating the temperature of the battery to 10 ℃, and performing charge-discharge circulation for 3 times at a constant current of 0.02 ℃ between 2.75 and 2.85V;
4) charging to 3.60V by 0.2C constant current pulse, wherein the pulse time is 60s, the interval is 5s, and charging at 3.60V constant voltage until the charging current is lower than 0.01C;
5) charging to 3.67V at a constant current of 0.2C and charging at a constant voltage of 3.67V until the charging current is lower than 0.01C;
6) charging to 3.72V at constant current of 0.2C and charging at constant voltage of 3.72V until the charging current is lower than 0.01C;
7) charging to 3.80V at constant current of 0.2C, and charging at constant voltage of 3.80V until the charging current is lower than 0.01C;
8) charging to 4.25V with 0.2C constant current pulse, pulse time is 60s, interval is 5s, charging with 4.25V constant voltage until charging current is lower than 0.01C;
9) discharging to 3.80V at constant current of 0.09C, adjusting current to 0.2, continuing to discharge to 3.60V at constant current, adjusting current to 0.1C, and continuing to discharge to 2.75V at constant current;
10) sealing;
11) charging and discharging 3 times at 0.2C constant current between 2.75-4.25V.
Example 3
1) Injecting an electrolyte, the electrolyte further comprising 4% by volume fluoroethylene carbonate FEC;
2)0.02C to 2.75V;
3) regulating the temperature of the battery to be 8 ℃, and performing charge-discharge circulation for 3 times at a constant current of 0.01 ℃ between 2.75 and 2.85V;
4) charging to 3.60V by 0.1C constant current pulse, wherein the pulse time is 40s, the interval is 4s, and charging at 3.60V constant voltage until the charging current is lower than 0.01C;
5) charging to 3.67V at a constant current of 0.2C and charging at a constant voltage of 3.67V until the charging current is lower than 0.01C;
6) charging to 3.72V at constant current of 0.2C and charging at constant voltage of 3.72V until the charging current is lower than 0.01C;
7) charging to 3.80V at constant current of 0.2C, and charging at constant voltage of 3.80V until the charging current is lower than 0.01C;
8) charging to 4.25V with 0.1C constant current pulse, pulse time of 40s, interval of 4s, and charging with 4.25V constant voltage until the charging current is lower than 0.01C;
9) discharging to 3.80V at constant current of 0.05C, adjusting current to 0.2, continuing to discharge to 3.60V at constant current, and adjusting current to 0.05C, continuing to discharge to 2.75V at constant current;
10) sealing;
11) charging and discharging 3 times at 0.2C constant current between 2.75-4.25V.
Comparative example 1
The battery of example 3 was used
1) Injecting the assembled battery into electrolyte, wherein the electrolyte also comprises 4% by volume of fluoroethylene carbonate FEC, and sealing;
2) charging and discharging 3 times at 0.2C constant current between 2.75-4.25V.
Comparative example 2
By using LiCo0.2Mn0.6Ni0.2O2Other parameters of the positive electrode active material were the same as those in example 3.
Comparative example 3
By using LiCo0.4Mn0.2Ni0.4O2Other parameters of the positive electrode active material were the same as those in example 3.
Comparative example 4
By using LiCo0.2Mn0.1Ni0.7O2Other parameters of the positive electrode active material were the same as those in example 3.
Comparative example 5
By using LiCo0.1Mn0.9O2Other parameters of the positive electrode active material were the same as those in example 3.
Experiment and data
The batteries obtained according to the methods of examples 1 to 3 and comparative examples 1 to 5 were subjected to charge and discharge cycles 100 times and 200 times, respectively, at 1C, and the average value of the capacity retention rates of the batteries of the respective groups was measured, and the results are shown in the following table. As can be seen from the following table, the capacity retention rate of the battery can be greatly improved by the pre-formation method of the present invention, but the formation method of the present invention is only effective for the positive electrode of the specific proportion in the present application, and for other single positive electrodes (comparative examples 2 to 5), the technical effect for the electrodes of other materials is not obvious because the voltage of the constant voltage charging does not correspond to the working platform voltage of the material.
TABLE 1
100 times (%) 200 times (%)
Example 1 98.5 96.3
Example 2 98.2 96.7
Example 3 98.6 97.2
Comparative example 1 96.2 91.2
Comparative example 2 95.1 90.1
Comparative example 3 95.4 90.4
Comparative example 4 94.9 89.6
Comparative example 5 95.3 89.9
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 with a composite positive electrode, wherein an active material of the composite positive electrode comprises LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2Wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (1) is 8-12:6-15:2-3: 4-6; the formation method comprises opening pre-formation, wherein the pre-formation comprises injecting electrolyte, and the electrolyte comprises 3-5% of fluoroethylene carbonate FEC by volume; discharging to a discharge cutoff voltage, then reducing the battery temperature, and performing a low-current charge-discharge cycle between the discharge cutoff voltage and a first predetermined voltage; charging the constant current pulse to a second preset voltage, and charging the constant current pulse at the second preset voltage; charging the battery at a constant current to a third preset voltage, and charging the battery at a constant voltage of the third preset voltage; charging the battery at a constant current to a fourth preset voltage and charging the battery at a constant voltage of the fourth preset voltage; constant current charging to the fifth stepA constant voltage, which is charged with a constant voltage of a fifth predetermined voltage; charging the constant current pulse to a charge cut-off voltage, and charging the constant current pulse at the charge cut-off voltage; and discharging at constant current to a fifth preset voltage, adjusting the current to continue discharging at constant current to a second preset voltage, adjusting the current to continue discharging at constant current to a discharge cut-off voltage, sealing, and finishing the pre-formation process.
2. The chemical conversion method according to claim 1, wherein the discharge cutoff voltage is 2.75V, the first predetermined voltage is 2.85V, and the charge cutoff voltage is 4.25V.
3. The formation method according to claim 2, wherein the second predetermined voltage is 3.60V, the third predetermined voltage is 3.67V, the fourth predetermined voltage is 3.72V, and the fifth predetermined voltage is 3.80V.
4. A method of formation according to claims 1-3, the pre-formation consisting of the steps of:
1) injecting an electrolyte comprising 3-5% by volume fluoroethylene carbonate FEC;
2) discharging at 0.01-0.02 deg.C to discharge cut-off voltage;
3) adjusting the temperature of the battery to be 5-10 ℃, and performing constant current charge-discharge circulation at 0.01-0.02 ℃ between the discharge cut-off voltage and a first preset voltage;
4) charging to a second preset voltage by constant current pulse at 0.1-0.2C, wherein the pulse time is 30-60s, the interval is 3-5s, and charging at a second preset voltage and constant voltage until the charging current is lower than 0.01C;
5) charging to a third preset voltage by a constant current of 0.1-0.2C, and charging to a constant voltage by the third preset voltage until the charging current is lower than 0.01C;
6) charging to a fourth preset voltage by a constant current of 0.1-0.2C, and charging to a constant voltage by the fourth preset voltage until the charging current is lower than 0.01C;
7) charging to a fifth preset voltage by a constant current of 0.1-0.2C, and charging to a constant voltage by the fifth preset voltage until the charging current is lower than 0.01C;
8) charging to a charge cut-off voltage by constant current pulse of 0.1-0.2C, wherein the pulse time is 30-60s, the interval is 3-5s, and charging to a constant voltage by the charge cut-off voltage until the charge current is lower than 0.01C;
9) discharging at constant current of 0.02-0.09 deg.C to fifth preset voltage, regulating current to 0.1-0.2, continuing to discharge at constant current to second preset voltage, and regulating current to 0.02-0.1 deg.C, continuing to discharge at constant current to discharge cut-off voltage;
10) and (7) sealing.
5. The method of the preceding claim, the electrolyte comprising EC, DEC, EMC as an organic solvent in a volume ratio of 2:1: 1.
6. The method as claimed in the preceding claim, wherein LiCo0.1Mn0.8Ni0.1O2，LiCo0.3Mn0.4Ni0.3O2，LiCo0.1Mn0.3Ni0.6O2And LiCo0.2Mn0.8O2The mass ratio of (A) to (B) is 9:12:2: 5.
7. The method of claim, further comprising a constant current charge-discharge cycle between a charge cutoff voltage and a discharge cutoff voltage after capping.
8. The method of the preceding claim, said electrolyte comprising 4% by volume fluoroethylene carbonate FEC.
CN201911227299.3A 2019-12-04 2019-12-04 Formation method of lithium ion battery with composite anode Withdrawn CN110911767A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112993423A (en) * 2021-02-19 2021-06-18 芜湖天弋能源科技有限公司 Method for improving capacity of lithium ion battery cell module

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112993423A (en) * 2021-02-19 2021-06-18 芜湖天弋能源科技有限公司 Method for improving capacity of lithium ion battery cell module

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