CN112259797A - Formation method of lithium ion battery - Google Patents
Formation method of lithium ion battery Download PDFInfo
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- CN112259797A CN112259797A CN202011146886.2A CN202011146886A CN112259797A CN 112259797 A CN112259797 A CN 112259797A CN 202011146886 A CN202011146886 A CN 202011146886A CN 112259797 A CN112259797 A CN 112259797A
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- voltage
- volume content
- charging
- predetermined voltage
- lithium ion
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 21
- PCYBDHWNMPLUSI-UHFFFAOYSA-N 2,2,2-trifluoroethylphosphonic acid Chemical compound OP(O)(=O)CC(F)(F)F PCYBDHWNMPLUSI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003792 electrolyte Substances 0.000 claims abstract description 30
- RBBXSUBZFUWCAV-UHFFFAOYSA-N ethenyl hydrogen sulfite Chemical compound OS(=O)OC=C RBBXSUBZFUWCAV-UHFFFAOYSA-N 0.000 claims abstract description 24
- WDXYVJKNSMILOQ-UHFFFAOYSA-N 1,3,2-dioxathiolane 2-oxide Chemical compound O=S1OCCO1 WDXYVJKNSMILOQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000007773 negative electrode material Substances 0.000 claims abstract description 5
- 238000007789 sealing Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 4
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 3
- 229910021382 natural graphite Inorganic materials 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 230000000996 additive effect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
-
- 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
-
- 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
- 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
- H01M2004/027—Negative 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a formation method of a lithium ion battery, wherein a negative active material of the lithium ion battery is graphite; the formation method comprises the following steps: injecting the assembled battery into electrolyte, wherein the organic solvent of the electrolyte is EC + PC + DMC, and the additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; charging at constant current to a first preset voltage, then charging at constant voltage under the first preset voltage, then performing constant current charge-discharge circulation between a second preset voltage and a third preset voltage, and performing charge-discharge circulation between a charge cut-off voltage and a discharge cut-off voltage; wherein the first predetermined voltage is a second predetermined voltage k + a third predetermined voltage (1-k); wherein k is the volume content of vinyl sulfite/(volume content of vinyl sulfite + volume content of trifluoroethylphosphonic acid). The formation method of the lithium ion battery can shorten the formation time, effectively form a stable SEI film and prolong the cycle life of the battery.
Description
Technical Field
The invention relates to a formation method of a lithium ion battery.
Background
The formation method of the lithium ion battery has great influence on the performance, particularly the stability of the lithium ion battery, and the research on the additive and the formation process parameters is not known in the field.
Disclosure of Invention
The invention provides a formation method of a lithium ion battery, wherein a negative active material of the lithium ion battery is graphite; the formation method comprises the following steps: injecting the assembled battery into electrolyte, wherein the organic solvent of the electrolyte is EC + PC + DMC, and the additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; charging at constant current to a first preset voltage, then charging at constant voltage under the first preset voltage, then performing constant current charge-discharge circulation between a second preset voltage and a third preset voltage, and performing charge-discharge circulation between a charge cut-off voltage and a discharge cut-off voltage; wherein the first predetermined voltage is a second predetermined voltage k + a third predetermined voltage (1-k); wherein k is the volume content of vinyl sulfite/(volume content of vinyl sulfite + volume content of trifluoroethylphosphonic acid). The formation method of the lithium ion battery can shorten the formation time, effectively form a stable SEI film and prolong the cycle life of the battery. The specific scheme is as follows:
a formation method of a lithium ion battery is characterized in that a negative active material of the lithium ion battery is graphite; the formation method comprises the following steps:
1) injecting the assembled battery into electrolyte, wherein the organic solvent of the electrolyte is EC + PC + DMC, and the additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid;
2) charging to a first preset voltage by constant current;
3) charging at a constant voltage under a first preset voltage until the charging current is lower than the cut-off current; wherein the first predetermined voltage is a second predetermined voltage k + a third predetermined voltage (1-k); wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
4) performing constant-current charge-discharge circulation between the second preset voltage and the third preset voltage for a plurality of times;
5) and carrying out charge-discharge circulation for a plurality of times between the charge cut-off voltage and the discharge cut-off voltage, and sealing to obtain the lithium ion battery.
Further, the graphite is selected from natural graphite or artificial graphite.
Further, the volume content of the ethylene sulfite is 2.4-2.8%, and the volume content of the trifluoroethyl phosphonic acid is 1.6-2.0%.
Further, the second predetermined voltage is 3.62V, and the third predetermined voltage is 3.76V.
Further, the organic solvent is 35 vol% EC +15 vol% PC +50 vol% DMC.
Further, the charging current in the step 2 is 0.05-0.1C.
Further, the charging and discharging current in the step 4 is 0.1-0.2C.
Further, the charging and discharging current in the step 5 is 0.1-0.2C.
The invention has the following beneficial effects:
1) specific additive combinations (ethylene sulfite and trifluoroethyl phosphonic acid) can greatly improve the cycle performance of the battery aiming at the graphite cathode.
2) The inventors have found that, when the content of the additive and the constant voltage forming voltage satisfy the following relational expression for the content of the different additives, the first predetermined voltage is the second predetermined voltage k + the third predetermined voltage (1-k); wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content); the stability of film formation is greatly improved;
3) the cyclic formation is carried out under the second preset voltage and the third preset voltage, so that the cyclic performance of the battery is further improved;
4) the invention adopts specific additive combination, can obtain the battery with higher cycle performance in shorter formation time, and has wide industrial application prospect.
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 active material is lithium cobaltate, and the negative electrode active material is a mixture of natural graphite and artificial graphite in a mass ratio of 1: 1; the organic solvent of the electrolyte is 35% EC + 15% PC + 50% DMC by volume, and the electrolyte salt is LiPF with 1mol/L6。
Example 1
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2.4 percent, and the volume content of the trifluoroethyl phosphonic acid is 2.0 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.62 k +3.76 (1-k) 3.68V; wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Example 2
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2.8 percent, and the volume content of the trifluoroethyl phosphonic acid is 1.6 percent;
2) charging the battery to a first preset voltage at a constant current of 0.1C; the first predetermined voltage is 3.62 k +3.76 (1-k) 3.67V; wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.2C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.2 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Example 3
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2.6 percent, and the volume content of the trifluoroethyl phosphonic acid is 1.8 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.62 k +3.76 (1-k) 3.68V; wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Comparative example 1
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2.6 percent, and the volume content of the trifluoroethyl phosphonic acid is 1.8 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.62V;
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Comparative example 2
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2.6 percent, and the volume content of the trifluoroethyl phosphonic acid is 1.8 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.76V;
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Comparative example 3
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 3 percent, and the volume content of the trifluoroethyl phosphonic acid is 1 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.62 k +3.76 (1-k) 3.66V; wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Comparative example 4
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2 percent, and the volume content of the trifluoroethyl phosphonic acid is 3 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.62 k +3.76 (1-k) 3.7V; wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Comparative example 5
1) Injecting the assembled battery into electrolyte, wherein additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid; the volume content of the ethylene sulfite is 2.6 percent;
2) charging to a first predetermined voltage at 0.05C; the first predetermined voltage is 3.62V;
3) charging at a first predetermined voltage at a constant voltage until the charging current is lower than the cutoff current by 0.01C;
4) performing constant current charge and discharge at 0.1C between 3.62V and 3.76V for 3 times;
5) and (3) carrying out charge-discharge circulation at 0.1 ℃ between 4.25V and 2.75V for 3 times, and sealing to obtain the lithium ion battery.
Test and results
The batteries of examples 1 to 3 and comparative examples 1 to 5 were tested and the capacity retention rate of the batteries was measured after 500 constant current charge and discharge cycles at a current of 1C. As can be seen from table 1, for the graphite negative electrode, the specific additive combination (vinyl sulfite and trifluoroethyl phosphonic acid) can greatly improve the cycle performance of the battery. When the contents of the additives and the constant voltage forming voltage satisfy the following relation, the first predetermined voltage is the second predetermined voltage k + the third predetermined voltage (1-k); wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content); the stability of film formation is greatly improved; the cycling under the second predetermined voltage and the third predetermined voltage is more beneficial to further improving the cycling performance of the battery.
TABLE 1
| Capacity retention (%) | |
| Example 1 | 99.1 |
| Example 2 | 99.0 |
| Example 3 | 99.3 |
| Comparative example 1 | 95.6 |
| Comparative example 2 | 95.9 |
| Comparative example 3 | 94.3 |
| Comparative example 4 | 94.1 |
| Comparative example 5 | 93.2 |
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 in that a negative active material of the lithium ion battery is graphite; the formation method comprises the following steps:
1) injecting the assembled battery into electrolyte, wherein the organic solvent of the electrolyte is EC + PC + DMC, and the additives in the electrolyte are ethylene sulfite and trifluoroethyl phosphonic acid;
2) charging to a first preset voltage by constant current;
3) charging at a constant voltage under a first preset voltage until the charging current is lower than the cut-off current; wherein the first predetermined voltage is a second predetermined voltage k + a third predetermined voltage (1-k); wherein k ═ vinyl sulfite volume content/(vinyl sulfite volume content + trifluoroethylphosphonic acid volume content);
4) performing constant-current charge-discharge circulation between the second preset voltage and the third preset voltage for a plurality of times;
5) and carrying out charge-discharge circulation for a plurality of times between the charge cut-off voltage and the discharge cut-off voltage, and sealing to obtain the lithium ion battery.
2. The method of the preceding claim, wherein the graphite is selected from natural graphite or artificial graphite.
3. The process according to the preceding claim, wherein the vinyl sulfite has a volume content of from 2.4 to 2.8% and the trifluoroethylphosphonic acid has a volume content of from 1.6 to 2.0%.
4. The method of the preceding claim, the second predetermined voltage being 3.62V and the third predetermined voltage being 3.76V.
5. The method of the preceding claim, wherein the organic solvent is 35% EC + 15% PC + 50% DMC by volume.
6. The method of the preceding claim, wherein the charging current in step 2 is 0.05-0.1C.
7. The method according to the previous claim, wherein the charging and discharging current in step 4 is 0.1-0.2C.
8. The method according to the previous claim, wherein the charging and discharging current in step 5 is 0.1-0.2C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011146886.2A CN112259797A (en) | 2020-10-23 | 2020-10-23 | Formation method of lithium ion battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011146886.2A CN112259797A (en) | 2020-10-23 | 2020-10-23 | Formation method of lithium ion battery |
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| Publication Number | Publication Date |
|---|---|
| CN112259797A true CN112259797A (en) | 2021-01-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011146886.2A Withdrawn CN112259797A (en) | 2020-10-23 | 2020-10-23 | Formation method of lithium ion battery |
Country Status (1)
| Country | Link |
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| CN (1) | CN112259797A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112864466A (en) * | 2021-01-28 | 2021-05-28 | 苏州酷卡环保科技有限公司 | Preparation method of lithium ion battery |
| CN113036246A (en) * | 2021-03-05 | 2021-06-25 | 惠州亿纬锂能股份有限公司 | Method for improving performance of lithium ion battery and lithium ion battery |
| CN113948778A (en) * | 2021-10-12 | 2022-01-18 | 远景动力技术(江苏)有限公司 | Lithium ion battery cell and formation method and application thereof |
-
2020
- 2020-10-23 CN CN202011146886.2A patent/CN112259797A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112864466A (en) * | 2021-01-28 | 2021-05-28 | 苏州酷卡环保科技有限公司 | Preparation method of lithium ion battery |
| CN113036246A (en) * | 2021-03-05 | 2021-06-25 | 惠州亿纬锂能股份有限公司 | Method for improving performance of lithium ion battery and lithium ion battery |
| CN113948778A (en) * | 2021-10-12 | 2022-01-18 | 远景动力技术(江苏)有限公司 | Lithium ion battery cell and formation method and application thereof |
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Application publication date: 20210122 |