CN114335770A - Cold and hot alternate aging method for lithium battery - Google Patents
Cold and hot alternate aging method for lithium battery Download PDFInfo
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- CN114335770A CN114335770A CN202111676167.6A CN202111676167A CN114335770A CN 114335770 A CN114335770 A CN 114335770A CN 202111676167 A CN202111676167 A CN 202111676167A CN 114335770 A CN114335770 A CN 114335770A
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- 230000032683 aging Effects 0.000 title claims abstract description 30
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 18
- 238000012546 transfer Methods 0.000 claims abstract description 7
- 230000007704 transition Effects 0.000 claims 1
- 238000002407 reforming Methods 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract description 2
- 230000006798 recombination Effects 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract description 2
- 238000011105 stabilization Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 230000014759 maintenance of location Effects 0.000 description 10
- 238000003860 storage Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003880 polar aprotic solvent Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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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Abstract
The invention belongs to the field of lithium polymer batteries, and provides a cold and hot alternate aging method for a lithium battery, which comprises the following steps of: placing the battery in a high-temperature area for a period of time, and then transferring the battery to a low-temperature area for a period of time; or, the battery is placed in a low temperature region for a period of time, and then the battery is transferred to a high temperature region for a period of time; the battery undergoes two placements and one transfer into one cycle; the battery is cycled at least 5 times; the temperature difference between the high temperature zone and the low temperature zone is greater than 55 ℃. The invention provides an aging method of cold-hot alternating impact by combining the advantages of short high-temperature aging period, good SEI film reforming performance, better stability of the normal-temperature aged SEI film and good cycle performance; rapid recombination and stabilization of the SEI film; and thus the cycle life performance of the battery.
Description
Technical Field
The invention belongs to the field of lithium polymer batteries, and particularly relates to a cold and hot alternate aging method for a lithium battery.
Background
Lithium ion batteries are widely used in electric vehicles and consumer electronics because of their advantages of high energy density, high output power, long cycle life, and low environmental pollution. The current demands for lithium ion batteries are: high voltage, high power, long cycle life, long storage life and excellent safety performance.
The preparation process of the lithium ion battery comprises the following steps: preparing materials such as a positive electrode, a negative electrode, a diaphragm and the like; assembling; injecting electrolyte; formation; aging; and finally packaging and selling.
Formation refers to the first charge and discharge of a lithium battery; the positive and negative electrode substances in the battery core are activated, and the self-discharge, charge and discharge performance and storage performance of the battery are improved.
Aging refers to a placing process after the battery is assembled and injected with liquid and is charged and formed for the first time; the first activation charging in formation is generally 50% -70% of capacity, and after formation, all materials in the battery are in an active state, and the voltage is also in an unstable state, so that aging is needed to stabilize the performance of all materials in the battery.
There are two methods of normal temperature aging and high temperature aging in general; the room temperature is 25 ℃ under normal temperature aging, and the time is three weeks to one month generally; the high-temperature aging is different according to different manufacturers, but is generally within 38-45 ℃ for 48-72 hours.
At present, in order to shorten the whole production period of the battery, lithium battery manufacturers generally age the battery for 48 to 72 hours at a temperature of between 40 and 50 ℃ after formation. In addition, the process is mainly used for optimizing the SEI film on the surface of the negative electrode after aging for 48-72 hours at 40-50 ℃, so that the properties and the composition of the SEI film formed after primary charging can be stabilized, and the phenomenon that the negative electrode generates solvent co-insertion during subsequent charging to damage the layered structure of the negative electrode is avoided.
The SEI film is an interfacial film with the thickness of about 100-120nm generated by the reduction reaction of a small amount of polar aprotic solvent in the electrolyte after partial electrons are obtained and combined with lithium ions when the lithium/sodium ion battery is charged and discharged for the first time. The SEI film is generally formed at a solid-liquid interface between an electrode material and an electrolyte. The quality of the SEI film and the stability and integrity of the formed film are very important for the capacity and the performance of the battery in the later period.
But the purely high temperature aging easily destroys the SEI film already formed, which is not favorable for battery cycle.
Disclosure of Invention
Aiming at the defect that the formed SEI is easy to decompose and damage by high-temperature aging in the production process of the battery in the prior method, the invention provides a cold and hot alternate aging method for a lithium battery.
A cold and hot alternate aging method for a lithium battery comprises the following steps:
placing the battery in a high-temperature area for a period of time, and then transferring the battery to a low-temperature area for a period of time;
or, the battery is placed in a low temperature region for a period of time, and then the battery is transferred to a high temperature region for a period of time;
the battery undergoes two placements and one transfer into one cycle; the battery is cycled at least 5 times;
the temperature difference between the high temperature zone and the low temperature zone is greater than 55 ℃.
Specifically, the temperature difference between the high-temperature region and the low-temperature region is 55 ℃ to 90 ℃.
More specifically, the temperature of the high temperature zone ranges from 55 ℃ to 70 ℃; the temperature range of the low-temperature zone is-20 ℃ to 0 ℃.
Specifically, each transfer time is less than or equal to 30 min.
Specifically, the standing time is 3h or more.
Specifically, the temperature fluctuation ranges of the high-temperature region and the low-temperature region are less than or equal to 2 ℃.
The invention discovers that when the temperature difference is less than 55 ℃, the stability improvement effect of the SEI film is not obvious; when the temperature difference is more than 90 ℃, the performance of the SEI film is not improved except for increasing energy consumption; and may even lead to performance degradation.
The invention discovers that when the temperature of a low-temperature region is lower than-20 ℃, the electrolyte can be separated out, and the electrolyte can not be completely recovered after the temperature rises; although the stability of the SEI film is better as the temperature is lower, it may negatively affect other structures of the battery. When the temperature of the high temperature region is more than 70 ℃, the reforming rate of the SEI film is less than the decomposition rate, so that the effect of the reforming rate of the previous cycle of the SEI film is offset.
The invention finds that each transfer time needs to be controlled within 30min, and when the transfer time is more than 30min, the temperature is easy to slowly rise/fall, thereby having negative effects on the low-temperature formed SEI film or the high-temperature SEI film reformed into Zhao.
The invention discovers that when the standing time in a high temperature area/a low temperature area is within 3h, the quality of an SEI film is in direct proportion to the time; when the time exceeds 3 hours, the quality of the SEI film is not further improved.
The present invention has found that when a lithium battery is placed in a high temperature region/a low temperature region for aging, when the temperature fluctuation is more than 2 ℃, the negative effects on the performance of the SEI film are caused; the negative effects are negligible in the fluctuation range of 2 ℃ or less.
The invention has the beneficial effects that:
the invention provides an aging method of cold-hot alternating impact by combining the advantages of short high-temperature aging period, good SEI film reforming performance, better stability of the normal-temperature aged SEI film and good cycle performance; rapid recombination and stabilization of the SEI film; and thus the cycle life performance of the battery.
Detailed Description
The present invention will be further illustrated in detail with reference to the following specific examples, which are not intended to limit the present invention but are merely illustrative thereof. The experimental methods used in the following examples are not specifically described, and the materials, reagents and the like used in the following examples are generally commercially available under the usual conditions without specific descriptions.
In the specific embodiment, the steps, material selection and numerical parameters which are not described in detail are all conventional choices in the prior art, such as the safety requirements for lithium ion batteries and battery packs for portable electronic products in GB 31241-2014, or any prior art which is disclosed in the prior art.
1) After the lithium battery is prepared, formation is carried out, and the specific steps of the formation of the battery are shown in the following table 1:
TABLE 1
2) Placing the battery in a high-temperature area for 3 hours, wherein the environmental temperature of the high-temperature area is set to be constant at 55 ℃/62 ℃/70 ℃;
3) transferring the battery from the high-temperature area to the low-temperature area, and standing the battery in the low-temperature area for 3h, wherein the environmental temperature of the low-temperature area is-20 ℃ to-10 ℃/0 ℃;
4) repeating the step 2) and the step 3) for 5 times, wherein the transfer time of the battery in different temperature areas of the temperature area is within 30min each time;
5) the specific steps of capacity grading are shown in the following table 2:
TABLE 2
6) The capacity grading is the same as the preparation steps of the conventional battery.
Experiment-battery life (cycle performance) test
Test conditions and methods: at 25 ℃, the batteries after capacity grading are charged to 4.2V at constant current and constant voltage of 1C, the current is cut off at 0.1C, and then the batteries are discharged to 3.0V at constant current of 1C. And circulating for 500 weeks. The first capacity of the cycle is recorded as C1, the 100 capacities as C100, and so on, C200, C300, C400, C500. Calculating the comparison of the capacity retention rate corresponding to the cycle number; the results are shown in Table 3. Shown in table 4.
Experiment two Charge and Capacity recovery with 30 days storage at 60 deg.C
The battery is charged to 4.2V at constant current and constant voltage according to 1C, the current is cut off to 0.1C, then the battery is discharged to 3.0V at constant current according to 1C, the standard capacity C1 of the battery is obtained by charging and discharging, then the battery is charged, the battery is charged to 4.2V at constant current and constant voltage according to 1C, the current is cut off to 0.1C, and the charging voltage at the moment is recorded as U1. Storing at 60 ℃ for 30 days after charging, then discharging at a constant current of 1C until the final voltage is 3.0V to obtain a discharge capacity C2, wherein the charge retention rate is C2/C1, and recording the charging voltage U2 (calculating the K value is (U2-U1)/U1); finally, the battery is charged to 4.2V at constant current and constant voltage of 1C, the cut-off current is 0.1C, and then the battery is discharged to the end voltage of 3.0V at constant current of 1C, so that the discharge capacity C3 is obtained, and the capacity recovery rate is C3/C1. The results are shown in tables 3 and 4.
TABLE 3
TABLE 4
In table 4, the unit of discharge capacity is mAh; the ratio units are%, where the ratio of the battery cycle initial discharge capacity is calculated as: C1/C1; the rate of discharge capacity after 100 cycles of the battery was calculated as: C100/C1; the rate of discharge capacity after 200 cycles of the battery was calculated as: C200/C1; the rate of discharge capacity after 300 cycles of the battery was calculated as: C300/C1; the rate of discharge capacity after 400 cycles of the battery was calculated as: C400/C1; the rate of discharge capacity after 500 cycles of the battery was calculated as: C500/C1.
As can be seen from table 4, the initial cycle discharge capacity of the battery produced in the comparative example was 887.8mAh, which reached 104.4% of the nominal capacity; after the circulation is carried out for 300 times, the capacity is 849.9mAh, and the capacity retention rate reaches 95.7 percent of the initial discharge capacity; after 500 times of circulation, the capacity is 808.5mAh, and the capacity retention rate reaches 91.1 percent of the initial discharge capacity. Calculating according to the standard quality requirement that the service life of 500 weeks after circulation reaches 90% of the initial discharge capacity, namely the end of the circulation service life, wherein the battery produced in the comparative example just reaches the standard quality requirement but is close to the critical point of the standard quality requirement;
the batteries produced in the examples 1-9 have initial discharge capacity of 879-899mAh, and the highest capacity reaches 105.8 percent of the nominal capacity; after circulating for 300 times, the capacity range is 850.5-871.1mAh, 96.4% -97.0% of the initial discharge capacity is achieved, the average value is 96.7%, and the ratio is 1% higher than 95.7%; after the battery is cycled for 500 times, the capacity range is 825.7-845.0mAh, the initial discharge capacity is 93.4% -94.1%, the average value is 93.75%, the discharge capacity is 2.65% higher than the proportion of 91.1%, the discharge capacity is 3.75% higher than the standard quality requirement that the service life of the battery reaches 90% of the initial discharge capacity after the battery is cycled for 500 weeks, and the discharge capacity far exceeds the standard quality requirement, so that the hidden danger that the battery possibly does not reach the standard at a detection mechanism is reduced; it can also be seen that the cycle life of examples 1-9 is significantly better than the comparative example.
Comparison of storage performance at 60 ℃ for 30 days: examples 1-9& comparative example
As can be seen from Table 1, the initial cycle discharge capacity of the battery produced in the comparative example was 888.3mAh, which reached 104.5% of the nominal capacity; the fully charged state is placed into an oven at 60 ℃ for storage for 30 days and then taken out, and after the fully charged state is naturally cooled to room temperature, the capacity retention rate is 86.04%. The battery produced by the comparative example is just up to the critical point of the standard quality requirement when the battery is close to the critical point of the standard quality requirement calculated according to the capacity retention rate of the standard quality requirement of more than or equal to 85 percent. The capacity can be recovered after the charge and the discharge are carried out again at normal temperature (the recovery rate is 99.72 percent).
The batteries produced in examples 1-9 had an initial cyclic discharge capacity of 878.8-899.3mAh, which reached 103.4-105.8% of the nominal capacity; the full-charge state is placed into an oven at 60 ℃ for storage for 30 days and then taken out, after the full-charge state is naturally cooled to room temperature, the capacity retention rate is 89.44-90.85%, the average value is 90.15%, the capacity retention rate is 4.11% higher than 86.04%, the capacity retention rate is 5.15% higher than that of the standard quality requirement which is more than or equal to 85%, and the capacity retention rate far exceeds the standard quality requirement, so that the hidden danger that the battery possibly does not reach the standard at a detection mechanism is reduced; it can also be seen that the storage performance at 60 ℃ for 30 days of examples 1-9 is significantly better than that of the comparative example. The capacity can be recovered after the charge and the discharge are carried out again at normal temperature (the recovery rate is 99.66-99.88%).
In addition, from the K value, the K value of the battery produced in the comparative example was 2.33%, and the K values of the batteries produced in examples 1 to 9 ranged from 2.28 to 2.33%. Meanwhile, the voltage before and after the high-temperature storage at 60 ℃ was both high, the voltage before and after the batteries produced in the comparative examples was 4.166V and 4.069V, respectively, while the voltage before and after the batteries produced in examples 1 to 9 were 4.168V to 4.171V and 4.072V to 4.076V, respectively. It can also be seen that the cells produced in examples 1-9 had lower K values and higher cell voltages before and after high temperature storage than the comparative examples. The lower K values and higher voltage values before and after testing for the batteries produced in examples 1-9 also mean better self-discharge performance of the batteries, and thus the batteries produced in examples 1-9 are more durable.
In the embodiment, the shortest aging time is 5 cycles, and the interval time of each time is 30 min; the standing time is 3h each time; namely, the whole aging time is 3h multiplied by 5 multiplied by 2+30min multiplied by 5 which is 32.5 h. The comparative example had an aging time of 48 hours; i.e. the inventive example saves the aging time by 15.5h compared to the comparative example.
Claims (6)
1. The cold and hot alternate aging method for the lithium battery is characterized in that after the battery is formed:
placing the battery in a high-temperature area for a period of time, and then transferring the battery to a low-temperature area for a period of time;
or, the battery is placed in a low temperature region for a period of time, and then the battery is transferred to a high temperature region for a period of time;
the battery undergoes two placements and one transfer into one cycle; the battery is cycled at least 5 times;
the temperature difference between the high temperature zone and the low temperature zone is greater than 55 ℃.
2. The cold-hot alternating aging method for a lithium battery as claimed in claim 1, wherein the temperature difference between the high temperature region and the low temperature region is 55 ℃ to 90 ℃.
3. The cold-hot alternating aging method for the lithium battery as claimed in claim 2, wherein the temperature of the high temperature region is in a range of 55 ℃ to 70 ℃; the temperature range of the low-temperature zone is-20 ℃ to 0 ℃.
4. The cold-hot alternating aging method for a lithium battery as claimed in claim 1, wherein each transition time is less than or equal to 30 min.
5. The cold-hot alternating aging method for the lithium battery as claimed in claim 1, wherein each standing time is 3 hours or more.
6. The cold-hot alternating aging method for lithium batteries according to any one of claims 1 to 5, wherein the temperature fluctuation ranges of the high-temperature region and the low-temperature region are 2 ℃ or less.
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| CN202111676167.6A CN114335770A (en) | 2021-12-31 | 2021-12-31 | Cold and hot alternate aging method for lithium battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115377536A (en) * | 2022-09-14 | 2022-11-22 | 江苏正力新能电池技术有限公司 | Battery charging and discharging method, battery module, battery pack and power supply device |
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| CN102646852A (en) * | 2012-04-01 | 2012-08-22 | 广州丰江电池新技术股份有限公司 | Lithium ion battery aging method |
| CN103985911A (en) * | 2014-05-29 | 2014-08-13 | 上虞安卡拖车配件有限公司 | Lithium ion battery aging method |
| CN107658504A (en) * | 2017-09-14 | 2018-02-02 | 合肥国轩高科动力能源有限公司 | Formation aging method for inhibiting lithium titanate battery flatulence |
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2021
- 2021-12-31 CN CN202111676167.6A patent/CN114335770A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004179009A (en) * | 2002-11-27 | 2004-06-24 | Sony Corp | Battery aging method and aging device |
| CN101714673A (en) * | 2009-11-18 | 2010-05-26 | 中国科学院上海微系统与信息技术研究所 | Method for improving storage/shelving performance of lithium ion battery |
| CN102646852A (en) * | 2012-04-01 | 2012-08-22 | 广州丰江电池新技术股份有限公司 | Lithium ion battery aging method |
| CN103985911A (en) * | 2014-05-29 | 2014-08-13 | 上虞安卡拖车配件有限公司 | Lithium ion battery aging method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115377536A (en) * | 2022-09-14 | 2022-11-22 | 江苏正力新能电池技术有限公司 | Battery charging and discharging method, battery module, battery pack and power supply device |
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Application publication date: 20220412 |