CN109786875B - Formation method for prolonging storage time of lithium ion battery - Google Patents
Formation method for prolonging storage time of lithium ion battery Download PDFInfo
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- CN109786875B CN109786875B CN201910062860.0A CN201910062860A CN109786875B CN 109786875 B CN109786875 B CN 109786875B CN 201910062860 A CN201910062860 A CN 201910062860A CN 109786875 B CN109786875 B CN 109786875B
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- voltage
- current
- charging
- electrolyte
- lithium ion
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 23
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 14
- 239000003792 electrolyte Substances 0.000 claims abstract description 31
- 239000000654 additive Substances 0.000 claims abstract description 10
- 230000000996 additive effect Effects 0.000 claims abstract description 10
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 8
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007774 positive electrode material Substances 0.000 claims abstract description 5
- 238000007600 charging Methods 0.000 claims description 42
- 238000007599 discharging Methods 0.000 claims description 8
- 238000010277 constant-current charging Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 230000006866 deterioration Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- -1 lithium hexafluorophosphate Chemical compound 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- CQDGTJPVBWZJAZ-UHFFFAOYSA-N monoethyl carbonate Chemical compound CCOC(O)=O CQDGTJPVBWZJAZ-UHFFFAOYSA-N 0.000 description 1
- 239000011356 non-aqueous organic solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- 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
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- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a formation method for improving the standing time of a lithium ion battery, wherein a positive active material in the lithium ion battery is mainly composed of lithium iron phosphate, an electrolyte of the lithium ion battery comprises an additive composed of fluoroethylene carbonate FEC and NaF, the FEC accounts for 0.5-1.5% of the electrolyte and the NaF accounts for 0.001-0.02% of the electrolyte according to the proportion of the total mass of the electrolyte, and the formation method forms a stable SEI film by controlling current, voltage and formation time, so that the performance deterioration of the battery caused by over-discharge due to self-discharge of the battery in the storage process is avoided.
Description
Technical Field
The invention relates to the technical field of flexible package lithium ion batteries, in particular to a formation method for prolonging the placement time of a lithium ion battery.
Background
Lithium ion batteries are becoming increasingly popular in a relatively high proportion as a means for reducing weight and increasing energy. The new policy of the new energy automobile releases signals for promoting the performance of the battery and increasing the energy density. Along with the continuous promotion of subsidy threshold, lithium ion battery can the more battery enterprises of helping improve energy density and product competitiveness. Lithium iron phosphate has the characteristics of safety, long cycle life, low toxicity and low price, and is one of the research targets of power lithium ion batteries, but batteries made of the material have obvious overdischarge conditions caused by self-discharge after long-term storage, and lithium is dissolved out of the surface of a positive electrode caused by overdischarge to cause battery degradation.
Disclosure of Invention
The invention provides a formation method for improving the standing time of a lithium ion battery, wherein a positive active material in the lithium ion battery is mainly composed of lithium iron phosphate, an electrolyte of the lithium ion battery comprises an additive composed of fluoroethylene carbonate FEC and NaF, the FEC accounts for 0.5-1.5% of the electrolyte and the NaF accounts for 0.001-0.02% of the electrolyte according to the proportion of the total mass of the electrolyte, and the formation method forms a stable SEI film by controlling current, voltage and formation time, so that the performance deterioration of the battery caused by over-discharge due to self-discharge of the battery in the storage process is avoided.
The specific scheme is as follows:
a formation method for improving the standing time of a lithium ion battery is characterized in that a positive active material in the lithium ion battery is mainly composed of lithium iron phosphate, an electrolyte of the lithium ion battery comprises an additive composed of fluoroethylene carbonate FEC and NaF, wherein the FEC accounts for 0.5-1.5% of the electrolyte and the NaF accounts for 0.001-0.02% of the electrolyte according to the proportion of the total mass of the electrolyte, and the formation method comprises the following steps:
1) standing the lithium ion battery after liquid injection for more than 6 hours;
2) charging the battery to a first voltage with a constant current, wherein the current is 0.02-0.04C;
3) standing for 1-6 h;
4) charging with a first voltage constant voltage until the charging current is reduced to below 0.01C;
5) discharging at constant current to a second voltage, wherein the current is 0.1-0.2C;
6) carrying out small current charge-discharge circulation for a plurality of times near a second voltage, wherein the small current is 0.005-0.01C;
7) charging the battery to the first voltage by constant current charging at a current of 0.02-0.04C;
8) carrying out small current charge-discharge circulation for a plurality of times near the first voltage, wherein the small current is 0.005-0.01C;
9) charging with a constant current of 0.02-0.04C to a charge cut-off voltage, and then charging at a constant voltage under the voltage until the charge current is reduced to below 0.01C;
10) and carrying out constant-current charge-discharge circulation for a plurality of times between the charge cut-off voltage and the discharge cut-off voltage, and sealing.
Further, the first voltage is 3.9-4.0V, and the second voltage is 3.1-3.2V.
Further, the charging cut-off voltage is 4.2-4.3V, and the discharging cut-off voltage is 2.7-2.8V.
In step 6, the voltage near the second voltage is within plus-minus 0.02V of the second voltage.
Further, in the step 8, the voltage is within plus or minus 0.02V of the first voltage in the vicinity of the first voltage.
Further, the steps 6 and 8 are cycled for more than 5 times.
Furthermore, according to the proportion of the total mass of the electrolyte, FEC accounts for 1-1.2% of the electrolyte, and NaF accounts for 0.01-0.012%.
The invention has the following beneficial effects:
1) the inventor finds that the self-discharge phenomenon of the battery in the storage process can be effectively reduced and the storage life of the battery can be prolonged by adding the additive formed by combining the fluoroethylene carbonate FEC into the battery electrolyte of which the positive electrode active material is lithium iron phosphate.
2) The inventors have found that, in a battery using an FEC additive, the battery resistance can be reduced by adding a small amount of NaF, presumably because the major component in the SEI film is LiF due to the FEC additive, NaF is partially co-deposited in the SEI during chemical conversion, and the Na ion radius is higher than the F ion, and therefore, a lithium ion path can be formed in the SEI film, and the conductivity of lithium ions can be improved.
3) The formation process adopts a small-current charge-discharge cycle before, which is beneficial to gas discharge and forms a stable SEI film, and for the lithium iron phosphate material, a very small current is adopted to perform the charge-discharge cycle near a specific voltage point, so that a more compact SEI film can be generated on the surfaces of a positive electrode and a negative electrode, and the self-discharge efficiency of the battery is reduced.
4. The compact SEI film generally causes the increase of the internal resistance of the battery, and due to the synergistic effect of the additive combination added in the invention and FEC and NaF, the SEI film can keep certain ionic conductivity while being more compact, thereby avoiding the increase of the internal resistance and keeping the multiplying power performance.
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 lithium ion battery used in the invention, (5% carbon-coated) lithium iron phosphate (anode)/artificial graphite (cathode); the electrolyte includes: 1.0M lithium hexafluorophosphate as an electrolyte salt, a mixed solution of dimethyl carbonate, ethyl methyl carbonate, and ethyl carbonate in a volume ratio of 1:1:2 as a nonaqueous organic solvent, and an additive consisting of fluoroethylene carbonate FEC and NaF.
Example 1
According to the proportion of the total mass of the electrolyte, FEC accounts for 0.5 percent of the electrolyte, NaF accounts for 0.005 percent, and the method comprises the following steps:
1) standing the lithium ion battery after liquid injection for 6 hours;
2) charging to 3.9V at constant current, wherein the current is 0.02C;
3) standing for 1 h;
4) charging at a constant voltage of 3.9V until the charging current is reduced to below 0.01C;
5) discharging to 3.1V at constant current, wherein the current is 0.1C;
6) carrying out small current charge-discharge circulation for 5 times at 3.08-3.12V, wherein the small current is 0.005C;
7) charging the battery to 3.9V by constant current charging with the current of 0.02C;
8) carrying out small current charge-discharge circulation for 5 times at 3.88-3.92V, wherein the small current is 0.005C;
9) charging to 4.2V with a constant current of 0.02C, and then charging at a constant voltage under the voltage until the charging current is reduced to below 0.01C;
10) and performing 0.2C constant current charge-discharge circulation between 4.2V and 2.7V for 3 times, and sealing.
Example 2
According to the proportion of the total mass of the electrolyte, FEC accounts for 1.5 percent of the electrolyte, NaF accounts for 0.02 percent, and the method comprises the following steps:
1) standing the lithium ion battery after liquid injection for 6 hours;
2) charging to 4.0V by constant current, wherein the current is 0.04C;
3) standing for 6 hours;
4) charging at a constant voltage of 4.0V until the charging current is reduced to below 0.01C;
5) discharging to 3.2V at constant current, wherein the current is 0.2C;
6) carrying out small current charge-discharge circulation for 5 times at 3.18-3.22V, wherein the small current is 0.01C;
7) charging the battery to 4.0V by constant current charging at the current of 0.02-0.04C;
8) carrying out small current charging and discharging circulation for 5 times at 3.98-4.02V, wherein the small current is 0.01C;
9) charging to 4.3V with a constant current of 0.04C, and then charging at a constant voltage under the voltage until the charging current is reduced to below 0.01C;
10) and performing 0.2C constant current charge-discharge circulation between 4.3V and 2.8V for 3 times, and sealing.
Example 3
According to the proportion of the total mass of the electrolyte, FEC accounts for 1 percent of the electrolyte, NaF accounts for 0.01 percent, and the method comprises the following steps:
1) standing the lithium ion battery after liquid injection for 8 hours;
2) charging to 3.9V at constant current, wherein the current is 0.02C;
3) standing for 6 hours;
4) charging at a constant voltage of 3.9V until the charging current is reduced to below 0.01C;
5) discharging to 3.1V at constant current, wherein the current is 0.1C;
6) carrying out small current charge-discharge circulation for 10 times at 3.08-3.12V, wherein the small current is 0.005C;
7) charging the battery to 3.9V by constant current charging with the current of 0.02C;
8) carrying out small current charge-discharge circulation for 10 times at 3.88-3.92V, wherein the small current is 0.005C;
9) charging to 4.2V with a constant current of 0.02C, and then charging at a constant voltage under the voltage until the charging current is reduced to below 0.01C;
10) and performing 0.2C constant current charge-discharge cycle between 4.2V and 2.7V for 5 times, and sealing.
Example 4
According to the proportion of the total mass of the electrolyte, FEC accounts for 1-1.2% of the electrolyte, NaF accounts for 0.01-0.012%, and the method comprises the following steps:
1) standing the lithium ion battery after liquid injection for 8 hours;
2) charging to 4.0V by constant current, wherein the current is 0.04C;
3) standing for 6 hours;
4) charging at a constant voltage of 4.0V until the charging current is reduced to below 0.01C;
5) discharging to 3.2V at constant current, wherein the current is 0.2C;
6) carrying out small current charge-discharge circulation for 10 times at 3.18-3.22V, wherein the small current is 0.01C;
7) charging the battery to 4.0V by constant current charging at the current of 0.02-0.04C;
8) carrying out small current charge-discharge circulation for 10 times at 3.98-4.02V, wherein the small current is 0.01C;
9) charging to 4.3V with a constant current of 0.04C, and then charging at a constant voltage under the voltage until the charging current is reduced to below 0.01C;
10) and performing 0.2C constant current charge-discharge circulation between 4.3V and 2.8V for 5 times, and sealing.
Comparative example
The same lithium ion battery as in examples 1-4 was charged with the same electrolyte of lithium salt and organic solvent, except that the additive in the comparative example was 1% fluoroethylene carbonate FEC.
The cells of the comparative examples were cycled between 2.7-4.2V 3 times at 0.1C, 3 times at 0.2C, and 3 times at 0.5C.
Experiment and data
The batteries of examples 1 to 4 and comparative example were left to stand for 90 days after being fully charged, and then the remaining capacity SOC and the internal resistance of the battery were measured. As can be seen from table 1, the batteries of examples and comparative examples, which were stored for 90 days, underwent different degrees of self-discharge, but the storage life of the battery in the example of the present invention was significantly longer than that of the battery in the comparative example, self-discharge was significantly suppressed, and the internal resistance of the battery was significantly lower than that of the battery in the comparative example.
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 (5)
1. A formation method for improving the standing time of a lithium ion battery is characterized in that a positive active material in the lithium ion battery is mainly composed of lithium iron phosphate, an electrolyte of the lithium ion battery comprises an additive composed of fluoroethylene carbonate FEC and NaF, wherein the FEC accounts for 0.5-1.5% of the electrolyte and the NaF accounts for 0.001-0.02% of the electrolyte according to the proportion of the total mass of the electrolyte, and the formation method comprises the following steps:
1) standing the lithium ion battery after liquid injection for more than 6 hours;
2) charging the battery to a first voltage with a constant current, wherein the current is 0.02-0.04C;
3) standing for 1-6 h;
4) charging with a first voltage constant voltage until the charging current is reduced to below 0.01C;
5) discharging at constant current to a second voltage, wherein the current is 0.1-0.2C;
6) carrying out small current charge-discharge circulation for a plurality of times near a second voltage, wherein the small current is 0.005-0.01C, and the second voltage is plus or minus 0.02V near the second voltage;
7) charging the battery to the first voltage by constant current charging at a current of 0.02-0.04C;
8) carrying out small current charge-discharge circulation for a plurality of times near the first voltage, wherein the small current is 0.005-0.01C, and the voltage near the first voltage is within plus or minus 0.02V of the first voltage;
9) charging with a constant current of 0.02-0.04C to a charge cut-off voltage, and then charging at a constant voltage under the voltage until the charge current is reduced to below 0.01C;
10) and carrying out constant-current charge-discharge circulation for a plurality of times between the charge cut-off voltage and the discharge cut-off voltage, and sealing.
2. The method of claim 1, wherein the first voltage is 3.9-4.0V and the second voltage is 3.1-3.2V.
3. The method of claim 1, wherein the charge cutoff voltage is 4.2-4.3V and the discharge cutoff voltage is 2.7-2.8V.
4. The method of claim 1, wherein steps 6 and 8 are cycled more than 5 times.
5. The method of claim 1, wherein the FEC is 1-1.2% and the NaF is 0.01-0.012% of the total electrolyte mass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910062860.0A CN109786875B (en) | 2019-01-23 | 2019-01-23 | Formation method for prolonging storage time of lithium ion battery |
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| CN201910062860.0A CN109786875B (en) | 2019-01-23 | 2019-01-23 | Formation method for prolonging storage time of lithium ion battery |
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| CN110416626B (en) * | 2019-08-05 | 2020-12-22 | 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 |
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| CN101635376A (en) * | 2009-05-28 | 2010-01-27 | 广州丰江电池新技术股份有限公司 | Performing method of flexible-packaging lithium-iron-phosphate aqueous positive-pole lithium battery |
| CN103151527A (en) * | 2012-12-28 | 2013-06-12 | 中银（宁波）电池有限公司 | Alkaline battery additive |
| US9735445B2 (en) * | 2015-09-14 | 2017-08-15 | Nanotek Instruments, Inc. | Alkali metal or alkali-ion batteries having high volumetric and gravimetric energy densities |
| CN105489943A (en) * | 2015-11-25 | 2016-04-13 | 百顺松涛（天津）动力电池科技发展有限公司 | Lithium-ion battery formation method |
| CN106654427B (en) * | 2017-01-22 | 2019-10-22 | 珠海格力电器股份有限公司 | A kind of chemical synthesizing method of lithium ion battery |
| CN107275671A (en) * | 2017-07-07 | 2017-10-20 | 东莞市航盛新能源材料有限公司 | A kind of electrolyte and preparation method and lithium battery for suppressing Li dendrite |
| CN108054452A (en) * | 2017-11-30 | 2018-05-18 | 山西长征动力科技有限公司 | A kind of rapid forming method of lithium titanate battery |
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Effective date of registration: 20201225 Address after: Room 322, 319 Shenjia Road, Xiacheng District, Hangzhou, Zhejiang 310000 Patentee after: HANGZHOU DOLAY ELECTRONIC TECHNOLOGY Co.,Ltd. Patentee after: STATE GRID ZHEJIANG INTEGRATED ENERGY SERVICE Co.,Ltd. Address before: 215004 room 207, building 104, sanyuaner village, Suzhou City, Jiangsu Province Patentee before: Cao Yijun |
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Inventor after: Cao Yijun Inventor after: Ye Guobin Inventor after: Wen Jianyang Inventor after: Nie Jianbo Inventor after: Chen Xiuhai Inventor before: Cao Yijun |
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