CN114373997A - Method for infiltrating pole piece with electrolyte - Google Patents
Method for infiltrating pole piece with electrolyte Download PDFInfo
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- CN114373997A CN114373997A CN202210118592.1A CN202210118592A CN114373997A CN 114373997 A CN114373997 A CN 114373997A CN 202210118592 A CN202210118592 A CN 202210118592A CN 114373997 A CN114373997 A CN 114373997A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The application discloses a method for enabling electrolyte to infiltrate a pole piece. In the present application, the method comprises the steps of: standing at high temperature for the first time: taking the battery after liquid injection, and standing at the temperature of 40-50 ℃; charging: charging the battery subjected to the first high-temperature standing treatment; and standing at high temperature for the second time: standing the battery subjected to the charging treatment at 40-50 ℃; wherein the magnitude of the charging current used in the charging step is 0.005C to 0.1C. Compared with the prior art, the method for infiltrating the pole piece with the electrolyte can effectively accelerate infiltration of the electrolyte into the pole piece, can consume residual water in the pole piece, accelerates diffusion dynamic performance of the electrolyte, reduces infiltration time by more than half while not losing infiltration effect, shortens production period of the battery, and reduces manufacturing cost; the pole piece is soaked by the method provided by the application, so that the stable performance of the battery at the initial circulation stage is facilitated, and the capacity rebound of the first-time circulation battery is reduced.
Description
Technical Field
The invention relates to the field of secondary batteries, in particular to a method for infiltrating a pole piece with electrolyte.
Background
In the production process of the lithium iron phosphate battery, the energy density of the battery is further improved on the battery with the same size by improving the compaction density of the lithium iron phosphate pole piece. However, with the improvement of pole piece compaction, the manufacturability of pole pieces and batteries is more and more prominent, for example, with the improvement of positive pole piece compaction, the porosity of the pole piece is relatively reduced, the pole piece becomes more and more brittle, the infiltration of electrolyte is also difficult, and the negative pole also has the problems of unstable pole piece thickness rebound, insufficient electrolyte infiltration, lithium precipitation and the like. In the prior art, after the battery liquid injection is completed, the electrolyte infiltration is accelerated by adopting a high-temperature standing mode, and the infiltration effect of the electrolyte is ensured by prolonging the infiltration time. However, with the increase of the soaking time, the energy consumption in the battery manufacturing process is increased, and meanwhile, the process period is long, the factory space requirement is large, and the manufacturing cost of the battery is greatly increased. In addition, along with the extension of high-temperature standing time, the chemical reaction in the battery is more obvious in the high-temperature storage process, the consistency of the battery is also influenced to a certain extent, meanwhile, the requirement on the stability of the electrolyte is further increased, and the design cost of the battery is increased.
Therefore, there is still a need in the art to find a method for rapidly infiltrating the electrode plate with the electrolyte.
Disclosure of Invention
The invention aims to provide a method for infiltrating a pole piece with electrolyte, so that the pole piece is quickly infiltrated with the electrolyte, the infiltration time is saved, the manufacturing period is saved, and side reactions caused by long-time infiltration are avoided.
In order to solve the above technical problem, a first aspect of the present invention provides a method for infiltrating an electrolyte into a pole piece, the method comprising the steps of:
standing at high temperature for the first time: taking the battery after liquid injection, and standing at the temperature of 40-50 ℃;
charging: charging the battery subjected to the first high-temperature standing treatment; and
standing at high temperature for the second time: standing the battery subjected to the charging treatment at 40-50 ℃;
wherein the magnitude of the charging current used in the charging step is 0.005C to 0.1C.
In some preferred schemes, the time of the first high-temperature standing is not less than 10 hours and not more than 30 hours; more preferably, not less than 15 hours and not more than 25 hours; more preferably, not less than 18 hours and not more than 24 hours; for example: 18 hours or 24 hours.
In some preferred schemes, the time of the second high-temperature standing is not less than 5 hours and not more than 30 hours; more preferably not less than 8 hours and not more than 24 hours, for example: 23 hours, 11 hours, or 17 hours.
In some preferred schemes, the time of the second high-temperature standing is not less than 10 hours and not more than 20 hours; more preferably not less than 10 hours and not more than 15 hours, for example 11 hours.
In some preferred embodiments, the magnitude of the charging current is 0.01C to 0.08C; more preferably 0.02C to 0.06C, e.g. 0.02C, 0.05C.
In some preferred embodiments, the number of charging is not less than 2 times, and more preferably 2 to 3 times.
In some preferred aspects, the time for each of said charging is not less than 1 minute and not more than 30 minutes; more preferably the time per said charging is not less than 3 minutes and not more than 25 minutes; more preferably, the time per said charge is not less than 5 minutes and not more than 15 minutes; for example 5 minutes or 10 minutes.
In some preferred aspects, when the charging current is 0.01C to 0.03C, the time per one charge is not less than 8 minutes and not more than 15 minutes, for example: when the charging current is 0.02C, the time of each charging is 10 minutes.
In some preferred aspects, when the charging current is 0.04C to 0.06C, the time per one charge is not less than 2 minutes and not more than 7 minutes; for example: when the charging current is 0.05C, the time for each charging is 5 minutes.
In some preferred aspects, the battery is a hard-shell battery, more preferably a prismatic metal-shell battery or a cylindrical metal-shell battery.
In some preferred aspects, the battery is a hard-shell battery, and the charging is performed under negative pressure; more preferably, the charging is carried out at a pressure of-70 Kpa to-90 Kpa, for example 85 Kpa.
In other embodiments, the battery is a pouch battery and the charging step is performed at an elevated pressure, such as 0.2 to 0.5Mpa, for example 0.3 Mpa.
In other embodiments, the battery is a pouch battery, and a rolling step is further included between the charging step and the second high-temperature standing step. In some embodiments, the pressure of the rolling is 0.05 to 0.15MPa, such as 0.08 MPa.
In some preferred schemes, the number of times of charging is not less than 2, and 2 times of charging are separated by at least 10 minutes; preferably 2 said charges are separated by a time interval of 15 minutes to 30 minutes; for example 20 minutes or 25 minutes.
In still other embodiments of the present invention, there is provided a method for preparing a lithium ion battery, including the steps of:
taking the lithium ion battery packaged by the injection liquid to sequentially carry out pole piece infiltration, formation, aging and capacity calibration;
wherein the pole piece is soaked by the method for soaking the pole piece with the electrolyte according to the first aspect of the invention.
In some preferred embodiments, the formation is carried out under negative pressure.
In some preferred embodiments, the lithium ion battery is a lithium iron phosphate battery.
In some preferred embodiments, the lithium ion battery is a hard shell battery.
Compared with the prior art, the embodiment of the invention has at least the following advantages:
(1) the method for infiltrating the pole piece with the electrolyte can effectively accelerate the infiltration of the electrolyte into the pole piece, can consume residual water in the pole piece, accelerates the diffusion dynamic performance of the electrolyte, reduces the infiltration time by more than half without losing the infiltration effect, shortens the production period of the battery and reduces the manufacturing cost;
(2) the pole piece is infiltrated by the method provided by the invention, so that the stable performance of the battery at the initial cycle stage is favorably exerted, and the rebound proportion of the battery capacity at the initial cycle stage is favorably reduced.
It is to be understood that within the scope of the present invention, the above-described features of the present invention and those specifically described below (e.g., in the examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.
Drawings
One or more embodiments are illustrated by the corresponding figures in the drawings, which are not meant to be limiting.
Fig. 1 is a graph of battery capacity as a function of cycle number in an embodiment in accordance with the invention.
Detailed Description
In the prior art, the time for soaking the pole piece with the electrolyte is prolonged to realize full soaking, and in the aging step before formation, the pole piece is usually required to be kept still for 3 to 4 days or even more, so that the preparation efficiency is low, and the consistency of the obtained battery is poor. Through a large number of experimental researches, the inventor finds that the electrolyte can be accelerated to infiltrate the pole piece by using a mode of combining two times of high-temperature standing with small current charging, the battery preparation time is saved, redundant water and active functional groups are consumed, and the battery consistency is improved.
In some embodiments of the present invention, there is provided a method of wetting a pole piece with an electrolyte, the method comprising the steps of:
standing at high temperature for the first time: taking the battery after liquid injection, and standing at the temperature of 40-50 ℃;
charging: charging the battery subjected to the first high-temperature standing treatment; and
standing at high temperature for the second time: standing the battery subjected to the charging treatment at 40-50 ℃;
wherein the magnitude of the charging current used in the charging step is 0.005C to 0.1C.
Through further research, the inventor finds that the first high-temperature standing, the charging and the second high-temperature standing are necessary steps for accelerating the electrolyte to infiltrate the pole piece, if the step of the first high-temperature standing is omitted, the charging is carried out after the first high-temperature standing is directly placed at normal temperature, the effect of accelerating the electrolyte to infiltrate the pole piece cannot be realized, and the capacity exertion of the obtained battery (corresponding to comparative example 3) is close to the capacity exertion data in comparative example 2, which indicates that the first high-temperature standing, the charging and the second high-temperature standing are necessary steps for realizing the effect of the invention.
In addition, the magnitude of the charging current, the number of times of charging and the length of the charging time also have a significant influence on the wetting effect. As the charging current in the charging step, the charging step between two times of high-temperature standing is carried out at the charging current of less than 0.1C (preferably 0.005C to 0.1C), and the excessive current causes the gas generation to be faster at the initial stage of charging, so that the crystallization of the electrolyte is easy to occur or the infiltration of the electrolyte is influenced.
As the number of times of charging in the charging step described in the present invention, preferably two or more, more preferably two to three times, the number of times of charging is too large, promotion of the wetting efficiency of the electrolyte is not significant, and the excessive number of times of charging reduces the efficiency of battery production and consumption at the negative electrode.
As the charging time in the charging step described in the present invention, it is preferably not less than 1 minute and not more than 30 minutes, and an excessively long charging time will cause the battery capacity to exert a deterioration, and an excessively short charging time will reduce the effect of promoting wetting.
Of course, the magnitude of the charging current, the number of times of charging and the charging time are matched with each other, for example, the number of times of charging is 2, each time of charging is not less than 1 minute and not more than 30 minutes, the interval between two times of charging is 10 to 30 minutes, the magnitude of the charging current is 0.02 to 0.05C, and the obtained battery capacity is exerted more stably.
In some preferred schemes, the time of the first high-temperature standing is not less than 10 hours and not more than 30 hours; more preferably, not less than 15 hours and not more than 25 hours; more preferably, not less than 18 hours and not more than 24 hours; for example: 18 hours or 24 hours.
In some preferred schemes, the time of the second high-temperature standing is not less than 5 hours and not more than 30 hours; more preferably not less than 8 hours and not more than 24 hours, for example: 23 hours, 11 hours, or 17 hours.
In some preferred schemes, the time of the second high-temperature standing is not less than 10 hours and not more than 20 hours; more preferably not less than 10 hours and not more than 15 hours, for example 11 hours.
In some preferred embodiments, the magnitude of the charging current is 0.01C to 0.08C; more preferably 0.02C to 0.06C, e.g. 0.02C, 0.05C.
In some preferred embodiments, the number of charging is not less than 2 times, and more preferably 2 to 3 times.
In some preferred aspects, the time for each of said charging is not less than 1 minute and not more than 30 minutes; more preferably the time per said charging is not less than 3 minutes and not more than 25 minutes; more preferably, the time per said charge is not less than 5 minutes and not more than 15 minutes; for example 5 minutes or 10 minutes.
In some preferred aspects, when the charging current is 0.01C to 0.03C, the time per one charge is not less than 8 minutes and not more than 15 minutes, for example: when the charging current is 0.02C, the time of each charging is 10 minutes.
In some preferred aspects, when the charging current is 0.04C to 0.06C, the time per one charge is not less than 2 minutes and not more than 7 minutes; for example: when the charging current is 0.05C, the time for each charging is 5 minutes.
In some preferred aspects, the battery is a hard-shell battery, more preferably a prismatic metal-shell battery or a cylindrical metal-shell battery.
In some preferred aspects, the battery is a hard-shell battery, and the charging is performed under negative pressure; more preferably, the charging is carried out at a pressure of-70 Kpa to-90 Kpa, for example 85 Kpa.
In other embodiments, the battery is a pouch battery and the charging step is performed at an elevated pressure, such as 0.2 to 0.5Mpa, for example 0.3 Mpa.
In other embodiments, the battery is a pouch battery, and a rolling step is further included between the charging step and the second high-temperature standing step. In some embodiments, the pressure of the rolling is 0.05 to 0.15MPa, such as 0.08 MPa.
In some preferred schemes, the number of times of charging is not less than 2, and 2 times of charging are separated by at least 10 minutes; preferably 2 said charges are separated by a time interval of 15 minutes to 30 minutes; for example 20 minutes or 25 minutes.
In still other embodiments of the present invention, there is provided a method for preparing a lithium ion battery, including the steps of:
taking the lithium ion battery packaged by the injection liquid to sequentially carry out pole piece infiltration, formation, aging and capacity calibration;
wherein the pole piece is soaked by the method for soaking the pole piece with the electrolyte according to the first aspect of the invention.
In some preferred embodiments, the formation is carried out under negative pressure.
In some preferred embodiments, the lithium ion battery is a lithium iron phosphate battery.
The formation, aging, and capacity calibration steps described in the present invention can be performed by experimental means known to those skilled in the art. In some embodiments, the formation step can be performed with reference to the battery formation flow in table 1.
TABLE 1
| Number of steps | Time/min | Type (B) | Current (A) | Cutoff current (A) |
| 1 | 5 | Standing still | ||
| 2 | 7 | Cross current charging | 3 | Time cut-off |
| 3 | 5 | Standing still | ||
| 4 | 180 | Cross current charging | 3 | Time cut-off |
| 5 | 5 | Standing still |
In some embodiments, the step of capacity calibration may be performed with reference to the battery capacity calibration flow of table 2.
TABLE 2
| Number of steps | Time/min | Type (B) | Voltage (V) | Current (A) | Cutoff current (A) |
| 1 | 5 | Standing still | |||
| 2 | 200 | Constant current charging | 3.65 | 10 | Voltage cut-off |
| 3 | 60 | Constant voltage charging | 3.65 | Off current 1.5A | |
| 4 | 5 | Standing still | |||
| 5 | 200 | Constant current discharge | 2.5 | 30 | Voltage cut-off |
| 6 | 5 | Standing still | |||
| 7 | 200 | Constant current discharge | 2.0 | 10 | Voltage cut-off |
| 8 | 5 | Standing still | |||
| 9 | 60 | Constant current charging | 3.0 | 10 | Voltage cut-off |
| 10 | 30 | Constant voltage charging | 3.0 | Off current 1.5A | |
| 11 | 5 | Standing still |
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the present invention is further described below with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers. Unless otherwise indicated, percentages and parts are percentages and parts by weight. The test materials and reagents used in the following examples are commercially available without specific reference.
Unless otherwise defined, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs, and it is to be noted that the terms used herein are merely for describing particular embodiments and are not intended to limit example embodiments of the present application.
Example 1
The high-compaction lithium iron phosphate positive pole piece and the conventional compaction negative pole piece are assembled into a 30Ah square metal shell battery, and the compaction density of the lithium iron phosphate positive pole piece is 2.7g/cm3The compacted density of the negative pole piece is 1.55g/cm3. And after the battery is subjected to vacuum drying, filling electrolyte, and then sealing the liquid injection hole by using a sealing rubber plug. Standing at a high temperature of 45 +/-3 ℃ for 24h, then carrying out negative pressure charging on the battery, wherein the charging current is 0.02C, the negative pressure is-85 Kpa, the charging time is 10min, standing for 20min after the charging is finished, carrying out next charging, repeating the charging for 2 times, and then continuously standing the battery at a high temperature for 23 h. After the negative pressure charging is finished, pulling out the rubber plug, and performing high-temperature negative pressure formation on the battery through the liquid injection hole, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charging and discharging cycle test on the battery after the capacity calibration.
Example 2
The high-compaction lithium iron phosphate positive pole piece and the conventional compaction negative pole piece are assembled into the 30Ah square metal shell battery, and the compaction density of the lithium iron phosphate positive pole piece is 2.7g/cm3The compacted density of the negative pole piece is 1.55g/cm3. After the battery is subjected to vacuum drying, electrolyte is filled, then a sealing rubber plug is used for sealing a liquid filling hole, the battery is kept stand at a high temperature of 45 +/-3 ℃ for 24 hours, then the battery is charged at a negative pressure, the charging current is 0.02C, the negative pressure is-85 Kpa, the charging time is 10min, the battery is kept stand for 20min after the charging is finished, the next charging is carried out, the charging is repeated for 2 times, and then the battery is kept stand at a high temperature for 11 hours. After the negative pressure charging is finished, pulling out the rubber plug, and performing high-temperature negative pressure formation on the battery through the liquid injection hole, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charging and discharging cycle test on the battery after the capacity calibration.
Example 3
The high-compaction lithium iron phosphate positive pole piece and the conventional compaction negative pole piece are assembled into the 30Ah square metal shell battery, and the compaction density of the lithium iron phosphate positive pole piece is 2.7g/cm3The compacted density of the negative pole piece is 1.55g/cm3. After the battery is subjected to vacuum drying, electrolyte is filled, then a sealing rubber plug is used for sealing a liquid filling hole, the battery is placed at a high temperature of 45 +/-3 ℃ for 24 hours, then negative pressure charging is carried out on the battery, the charging current is 0.05C, the negative pressure is-85 Kpa, the charging time is 5min, the battery is placed at a position of 25min after the charging is finished for next charging, the charging is repeated for 2 times, and then the battery is continuously placed at a high temperature for 11 hours. After the negative pressure charging is finished, pulling out the rubber plug, and performing high-temperature negative pressure formation on the battery through the liquid injection hole, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charging and discharging cycle test on the battery after the capacity calibration.
Example 4
The high-compaction lithium iron phosphate positive pole piece and the conventional compaction negative pole piece are assembled into the 30Ah square metal shell battery, and the compaction density of the lithium iron phosphate positive pole piece is 2.7g/cm3The compacted density of the negative pole piece is 1.55g/cm3. After the battery is subjected to vacuum drying, electrolyte is filled, then a sealing rubber plug is used for sealing a liquid filling hole, the battery is placed at a high temperature of 45 +/-3 ℃ for 18 hours, then negative pressure charging is carried out on the battery, the charging current is 0.05C, the negative pressure is-85 Kpa, the charging time is 5min, the battery is placed at a position of 25min after the charging is finished for next charging, the charging is repeated for 2 times, and then the battery is continuously placed at a high temperature for 17 hours. After the negative pressure charging is finished, pulling out the rubber plug, and performing high-temperature negative pressure formation on the battery through the liquid injection hole, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charging and discharging cycle test on the battery after the capacity calibration.
Example 5
The high-compaction lithium iron phosphate positive pole piece and the conventional compaction negative pole piece are assembled into the 30Ah square metal shell battery, and the compaction density of the lithium iron phosphate positive pole piece is 2.7g/cm3The compacted density of the negative pole piece is 1.55g/cm3. After the battery is subjected to vacuum drying, electrolyte is filled, then a sealing rubber plug is used for sealing a liquid filling hole, the battery is placed at a high temperature of 45 +/-3 ℃ for 12 hours, then negative pressure charging is carried out on the battery, the charging current is 0.02C, the negative pressure is-85 Kpa, the charging time is 10 minutes, the battery is placed at a position of 20 minutes after the charging is finished for next charging, the charging is repeated for 2 times, and then the battery is continuously placed at a high temperature for 11 hours. After the negative pressure charging is finished, pulling out the rubber plug, and performing high-temperature negative pressure formation on the battery through the liquid injection hole, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charging and discharging cycle test on the battery after the capacity calibration.
Comparative example 1
The high-compaction lithium iron phosphate positive pole piece and the conventional compaction negative pole piece are assembled into the 30Ah square metal shell battery, and the compaction density of the lithium iron phosphate positive pole piece is 2.7g/cm3The compacted density of the negative pole piece is 1.55g/cm3. After the battery is vacuum-dried, electrolyte is filled, then a sealing rubber plug is used for sealing the liquid filling hole, the battery is kept stand at a high temperature of 45 +/-3 ℃ for 48 hours, and then the rubber is pulled outAnd (3) performing high-temperature negative pressure formation on the battery through the liquid injection hole by using the plug, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charge-discharge cycle test on the battery after the capacity calibration.
Comparative example 2
The method for preparing the battery in comparative example 2 is substantially the same as that of comparative example 1, except that the battery is left standing at a high temperature of 45 +/-3 ℃ for 84h after being packaged, then subjected to negative pressure formation, high temperature aging and capacity calibration, and subjected to a 1C/1C charge-discharge cycle test.
Comparative example 3
The method for manufacturing the battery in the comparative example 3 is substantially the same as that of the example 1, except that the battery is vacuum-dried, electrolyte is injected, the injection hole is sealed by using a sealing rubber plug, then the battery is charged under negative pressure, the charging current is 0.02C, the negative pressure is-85 Kpa, the charging time is 10min, the battery is placed still for 20min after the charging is finished for the next charging, the charging is repeated for 2 times, and then the battery is continuously placed still for 60h at high temperature. After the negative pressure charging is finished, pulling out the rubber plug, and performing high-temperature negative pressure formation on the battery through the liquid injection hole, wherein the negative pressure is-85 Kpa, the charging current is 0.1C, the battery is charged to 30% SOC, then performing high-temperature aging and capacity calibration, and performing 1C/1C charging and discharging cycle test on the battery after the capacity calibration.
[ volatilization test for Battery Positive electrode Material Capacity ]
The batteries prepared in the examples were subjected to a positive electrode capacity volatilization test in accordance with the procedure shown in table 2, and the gram capacity exertion data of the obtained battery 1C cycle positive electrode material is shown in table 3 and fig. 1.
TABLE 3
According to table 3 and fig. 1, the battery capacity was stably exerted in the initial stage of the cycle in the example, the battery capacity rebound ratio after a long-term cycle was low, while the gram capacity of the positive electrode material in the first cycle of the cycle in the comparative example was relatively low exerted, and the battery capacity in the comparative example was highly rebounded in the initial stage of the cycle. The electrolyte in the comparative example does not fully infiltrate the pole piece, so that the positive electrode material cannot be fully exerted, while the electrolyte in the example fully infiltrates the pole piece, so that the water in the pole piece is consumed, and the diffusion dynamic performance of the electrolyte is accelerated. The electrolyte soaks the pole piece is accelerated, and the battery capacity is more stably exerted.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.
Claims (10)
1. A method for infiltrating an electrolyte into a pole piece is characterized by comprising the following steps:
standing at high temperature for the first time: taking the battery after liquid injection, and standing at the temperature of 40-50 ℃;
charging: charging the battery subjected to the first high-temperature standing treatment; and
standing at high temperature for the second time: standing the battery subjected to the charging treatment at 40-50 ℃;
wherein the magnitude of the charging current used in the charging step is 0.005C to 0.1C.
2. The method of claim 1, wherein the number of charges is not less than 2.
3. The method of claim 2, wherein the time for each of the charging is not less than 1 minute and not more than 30 minutes.
4. The method of claim 2, wherein the magnitude of the charging current is 0.01C to 0.08C.
5. The method according to claim 4, wherein when the charging current is 0.01C to 0.03C, the time per charging is not less than 8 minutes and not more than 15 minutes.
6. The method of claim 4, wherein when the charging current is 0.04C to 0.06C, the time per charging is not less than 2 minutes and not more than 7 minutes.
7. The method of claim 1, wherein the battery is a hard-shell battery and the charging is performed under negative pressure.
8. The method according to claim 1, wherein the time of the first high-temperature standing is not less than 10 hours and not more than 30 hours;
and/or the time of the second high-temperature standing is not less than 5 hours and not more than 30 hours.
9. The method according to claim 1, wherein the time of the second high-temperature standing is not less than 5 hours and not more than 30 hours.
10. A method of making a lithium ion battery, the method comprising the steps of:
taking the lithium ion battery after liquid injection, and sequentially carrying out pole piece infiltration, formation, aging and capacity calibration;
the pole piece soaking is carried out by the method for soaking the pole piece with the electrolyte according to any one of claims 1 to 8.
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