CN112216889B - Formation method of polymer lithium ion battery - Google Patents

Formation method of polymer lithium ion battery Download PDF

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CN112216889B
CN112216889B CN202011087586.1A CN202011087586A CN112216889B CN 112216889 B CN112216889 B CN 112216889B CN 202011087586 A CN202011087586 A CN 202011087586A CN 112216889 B CN112216889 B CN 112216889B
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lithium ion
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CN112216889A (en
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刘亚明
左志良
杨纪荣
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Shenzhen Qiming New Energy Technology Co ltd
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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
    • 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
    • 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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    • 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
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Abstract

The invention belongs to the field of polymer lithium ion batteries, and particularly relates to a formation method of a polymer lithium ion battery, which comprises the following steps: (1) aging the battery with liquid injection and vacuum pumping at 50-85 ℃; (2) setting the temperature and pressing the battery; (3) forming the battery, namely charging by adopting 2 stages of steps and discharging by adopting 3 rd steps, and totally adopting 4 stages of different pressures; (4) taking down the battery, rapidly cooling, sealing in vacuum, aging and picking out unqualified products to obtain the product. The invention can improve the displacement of the electrode core and the aluminum plastic film generated when the lithium ion battery is formed by using pressure, improve the hardness and the thickness of the battery and the peeling phenomenon of a negative electrode active material and a matrix copper foil, and pick out the battery with bad problems in time by using a high-temperature and high-humidity means, thereby not only improving the performance of the battery, but also ensuring the product shipment quality.

Description

Formation method of polymer lithium ion battery
Technical Field
The invention belongs to the field of polymer lithium ion battery manufacturing, and particularly relates to a formation method capable of improving the hardness, thickness and cycle performance of a high-energy density polymer lithium ion battery.
Background
With the demand of high energy density and portability of the market, the lithium ion battery is developed from the original steel shell and aluminum shell battery to the polymer lithium ion battery, and the polymer lithium ion battery has the advantages of high energy density, small volume, good safety performance, flexible appearance design and the like, and is widely applied to 3C digital products. Particularly, in recent years, with the rapid development of 4G and 5G, people have demanded more experience of mobile phones, and not only higher energy density but also faster charging are required. This puts higher demands on the manufacture of lithium ion batteries.
In the production process of the polymer lithium ion battery, a formation process is a very critical process, and plays a vital role in the thickness, hardness and electrical property of the polymer lithium ion battery. The formation of the lithium ion battery has two main functions: firstly, active substances in the battery are converted into normal electrochemical action by virtue of first charging; but the effective SEI film is generated on the surface of the electrode, mainly the negative electrode. The SEI film plays a very important role in the electrochemical reaction of the lithium ion battery for the stability of the battery system. During the formation of the battery, the initial charge and discharge of the battery are caused by irreversible reactions of the battery system, so that the discharge capacity of the battery is attenuated in the initial stage, and the battery tends to have stable capacity after the electrochemical state of the battery is stabilized. The current method commonly used in the industry adopts a pressure formation mode to form.
The chinese invention patent CN109301335B discloses a formation method of a flexible package lithium ion battery, which adopts a three-stage pressure pulse type variation method to form the lithium ion battery. The pressure pulse type variation selects a specific pulse pressure waveform and time of triangular wave, trapezoidal wave or half sine wave to carry out pulse pressure massage. The method improves the efficiency of the formation process, the stability of the SE1 film, the efficiency of the formation process and the cycle performance of lithium ions, but the pressure setting is more complex and has certain requirements on the technology.
Chinese patent application CN109560337A discloses a formation method of a lithium ion battery, which adopts three times of constant current charging, the first time of charging, the current is 0.05-0.15C, the pressure is 0.05-0.35MPa, the standing is carried out for 3-8 minutes, the second time of constant current charging is carried out, the current is 0.2-0.4C, the pressure is 0.05-0.35MPa, the standing is carried out for 3-7 minutes, the third time of constant current charging is carried out, the current is 0.4-0.7C, the pressure is 0.5-0.8MPa, the standing is carried out for 5 minutes, and the formation is finished. The formation method of the lithium ion battery can improve the stability of the SE1 film, improve the production efficiency and improve the cycle performance of the lithium ion battery.
However, when the pressure formation is used, due to the unreasonable design of pressure and temperature in each stage, the displacement between the electrode winding core and the aluminum plastic film of the battery is easily caused, and the battery is scrapped. Meanwhile, as the production efficiency is pursued, the formation voltage is reduced and the formation time is shortened, the battery becomes soft after formation, and even the negative active material and the matrix copper foil are peeled off (more seriously after circulation), the surface of the battery is bulged, the thickness is poor, the battery cannot be installed in a mobile phone cabin, or the mobile phone screen is pushed open in the use process of installing the battery in the mobile phone cabin, so that the mobile phone is scrapped. The phenomenon is particularly remarkable in the aspect of lithium ion batteries with high energy density, quick charge and quick discharge.
Disclosure of Invention
The invention aims to provide a formation process method which can improve the displacement of an electrode core and an aluminum plastic film generated when a lithium ion battery is formed by using pressure and improve the hardness and the thickness of the battery and the stripping phenomenon of a negative electrode active material and a matrix copper foil.
The technical problem of the invention is solved by the following technical scheme:
a formation method of a polymer lithium ion battery comprises the following steps:
(1) after vacuumizing the battery liquid injection, aging;
(2) after the temperature of the pressure formation cabinet reaches 50-70 ℃, the battery is compressed, the closing speed between the layers of the pressure formation cabinet is less than 1cm/s, and the closing pressure is less than or equal to 1kg/cm2；
(3) The battery is formed by adopting 2-stage step charging and 1-stage step discharging, and adopting 4-stage different pressures; wherein, the cut-off voltage of the 2 nd stage step charging is within 0.15V from full charge to full charge;
(4) cooling;
(5) vacuumizing and sealing the cooled battery;
(6) and aging the battery after vacuum sealing to obtain the battery.
Preferably, the aging temperature of step (1) is from 50 ℃ to 85 ℃.
Preferably, the aging time of step (1) is 3h to 24 h.
Preferably, the pressure in stage 1 in step (3) is less than or equal to 3kg/cm2The pressure of the 2 nd to 4 th sections is 4 to 15kg/cm2。
Preferably, in the step (3), the charging current of the 1 st step charging is 0.2C-0.5C, and the cut-off voltage is less than 3.70V.
Preferably, in the step (3), the charging current of the 2 nd step charging is 0.2C-1.5C.
Preferably, in the step (3), the step discharge current is 0.2C-0.5C, and the discharge voltage is 3.90V.
Preferably, the cooling in the step (4) is that the battery is cooled in an environment with the temperature lower than 18 ℃, and the cooling time is more than 1 h.
Preferably, after the vacuum pumping in the step (5), the retention amount of the electrolyte in the battery is 1.5g/Ah-1.9 g/Ah.
Preferably, the environmental conditions for aging the battery in the step (6) in the technical scheme are that the temperature is 30-50 ℃, the relative humidity of air is greater than 70% RH, and the aging time is greater than 48 h.
The invention has the beneficial effects that:
(1) according to the pressurization formation process, the closing speed between the laminates is low, the first section of pressurization pressure is low, the displacement generated between the electrode core and the aluminum-plastic film is effectively improved, and the service life of the battery is prolonged;
(2) the invention is charged in steps, the film forming uniformity and stability of the SEI film are better controlled by controlling the charging current and voltage, the charging dissatisfaction caused by the polarization voltage is effectively eliminated, the stress between the negative electrode and the matrix copper foil is eliminated, the negative electrode material and the matrix copper foil are prevented from being stripped when the battery is subjected to capacity grading or recycling, and the thickening and the recycling performance of the battery are effectively improved;
(3) the pressurization formation process can ensure that the battery has better hardness by controlling temperature, pressure, voltage and the like;
(4) according to the invention, through aging in a high-temperature and high-humidity environment, products with peeling, bulging, liquid leakage and poor side voltage can be effectively selected, and the quality hidden danger of the discharged battery is ensured;
(5) the process technology of the invention is simple and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a diagram of a polymer lithium ion battery formed according to example 1;
FIG. 2 is a diagram of a polymer lithium ion battery formed in example 2;
FIG. 3 is a diagram of a polymer lithium ion battery formed according to example 3;
FIG. 4 is a diagram of a polymer lithium ion battery formed according to example 4;
FIG. 5 is a diagram of a polymer lithium ion battery formed in comparative example 1;
FIG. 6 is a diagram of a polymer lithium ion battery formed according to example 2;
FIG. 7 is a diagram of a polymer lithium ion battery formed according to example 3;
FIG. 8 shows a defective cell detected by high temperature and high humidity techniques after formation in example 1;
FIG. 9 is a graph comparing the cycle performance of different formation modes;
fig. 10 shows the bottom case of the different formation modes, and the bottom of the comparative example 1 is spiral due to the cell shift.
Detailed Description
The invention will now be further described with reference to the accompanying drawings and examples.
356290PL300FY 4.4.4V cell pressure was calculated as follows:
effective area of pressure (cm)2) Width of the cell (mm) height of the cell (mm)/100;
356290PL300FY model cell effective area 62 x 90/100cm2＝55.8cm2
Calculating the battery charging current as the nominal capacity of the battery and the battery charging multiplying power;
a charging current of 0.1C 3000 × 0.1(mA) 300mA
Example 1
High-temperature formation process of 356290PL300FY 4.4.4V battery
(1) After battery liquid injection and vacuumizing, aging at the high temperature of 50 +/-5 ℃ for 24 hours, and putting the battery on a cabinet to a pressure forming cabinet;
(2) after the temperature of the pressure formation cabinet reaches 50 ℃ of the set temperature, the battery is compressed, the interlayer spacing of the pressure formation cabinet is reduced, the closing speed between the laminates is 0.5cm/s, and the closing pressure is 0.50kg/cm2The closing time is 10 min.
(3) Sending parameter formation, adopting 2-stage step charging and 3 rd-stage step discharging, adopting 4-stage different pressures, and setting specific formation pressure and formation parameters as shown in tables 1-1 and 1-2.
(4) After the pressure formation is finished, immediately taking down the battery, and rapidly cooling the battery for 3 hours at a low temperature of 0 ℃;
(5) vacuumizing and sealing the cooled battery, wherein the preservation amount of the electrolyte after vacuumizing is 1.5 g/Ah;
(6) and (3) aging the battery cell after vacuum sealing for 72h in an environment with high temperature of 40 +/-3 ℃ and high humidity of 70% RH, selecting products with leakage, bulging and poor side voltage, and finishing formation.
Table 1-1 example 1 formation pressure parameters
Figure BDA0002720852740000041
Table 1-2 example 1 formation parameters
Figure BDA0002720852740000042
Example 2
High-temperature formation process of 356290PL300FY 4.4.4V battery
(1) Vacuumizing the injection liquid, aging at the high temperature of 85 +/-5 ℃ for 4 hours, and loading the battery cell on a pressure forming cabinet;
(2) after the temperature of the pressure formation cabinet reaches 70 ℃, the battery is compressed, the interlayer spacing of the pressure formation cabinet is reduced, the closing speed between the laminates is 0.5cm/s, and the closing pressure is 0.50kg/cm2The closing time is 10 min.
(3) Sending parameter formation, adopting 2-stage charging and 3 rd-stage discharging, adopting 4-stage different pressures, and setting specific formation pressure and formation parameters as shown in tables 2-1 and 2-2.
(4) After the pressure formation pressing is finished, immediately taking down the battery, and rapidly cooling the battery for 3 hours at a low temperature of 0 ℃;
(5) vacuumizing and sealing the cooled battery, wherein the preservation amount of the electrolyte after vacuumizing is 1.7 g/Ah;
(6) and (3) aging the battery cell after vacuum sealing for 72h in an environment with high temperature of 40 +/-3 ℃ and high humidity of 70% RH, selecting products with leakage, bulging and poor side voltage, and finishing formation.
Table 2-1 example 2 formation pressure parameters
Figure BDA0002720852740000051
Table 2-2 example 2 formation parameters
Figure BDA0002720852740000052
Example 3
High-temperature formation process of 356290PL300FY 4.4.4V battery
(1) Vacuumizing the injection liquid, aging at the high temperature of 50 +/-5 ℃ for 4 hours, and loading the battery cell on a pressure forming cabinet;
(2) after the temperature of the pressure formation cabinet reaches 70 ℃, the battery is compressed, the interlayer spacing of the pressure formation cabinet is reduced, the closing speed between the laminates is 0.5cm/s, and the closing pressure is 0.50kg/cm2The closing time is 10 min. .
(3) Sending parameter formation, adopting 2-stage charging and 3 rd-stage discharging, adopting 4-stage different pressures, and setting specific formation pressure and formation parameters as shown in tables 3-1 and 3-2.
(4) After the pressure formation pressing is finished, immediately taking down the battery, and rapidly cooling the battery for 3 hours at a low temperature of 0 ℃;
(5) vacuumizing and sealing the cooled battery, wherein the preservation amount of the electrolyte after vacuumizing is 1.7 g/Ah;
(6) and (3) aging the battery cell after vacuum sealing for 72h in an environment with high temperature of 40 +/-3 ℃ and high humidity of 70% RH, selecting products with leakage, bulging and poor side voltage, and finishing formation.
Table 3-1 example 3 formation pressure parameters
Figure BDA0002720852740000053
Figure BDA0002720852740000061
Table 3-2 example 3 formation parameters
Figure BDA0002720852740000062
Example 4
High-temperature formation process of 356290PL300FY 4.4.4V battery
(1) Vacuumizing the injection liquid, aging at the high temperature of 50 +/-5 ℃ for 24 hours, and loading the battery cell on a pressure forming cabinet;
(2) after the temperature of the pressure formation cabinet reaches 70 ℃, the battery is compressed, the interlayer spacing of the pressure formation cabinet is reduced, the closing speed between the laminates is 1cm/s, and the closing pressure is 0.50kg/cm2The closing time is 10 min.
(3) Sending parameter formation, adopting 2-stage charging and 3 rd-stage discharging, adopting 4-stage different pressures, and setting specific formation pressure and formation parameters in tables 4-1 and 4-2.
(4) After the pressure formation pressing is finished, immediately taking down the battery, and rapidly cooling the battery for 3 hours at a low temperature of 0 ℃;
(5) vacuumizing and sealing the cooled battery, wherein the preservation amount of the electrolyte after vacuumizing is 1.7 g/Ah;
(6) and (3) aging the battery cell after vacuum sealing for 72h in an environment with high temperature of 40 +/-3 ℃ and high humidity of 70% RH, selecting products with leakage, bulging and poor side voltage, and finishing formation.
Table 4-1 example 4 formation pressure parameters
Figure BDA0002720852740000063
Figure BDA0002720852740000071
Table 4-2 example 4 formation parameters
Figure BDA0002720852740000072
Comparative example 1
356290PL300FY 4.4.4V battery common formation process
(1) Vacuumizing the injection liquid, aging at 25 ℃ for 24 hours, and loading the battery on a cabinet to a pressure forming cabinet;
(3) sending parameter formation, wherein the first constant current charging current is 0.05C, the cut-off voltage is 3.5V, and the time is 120 min; and (3) performing constant current charging for the second time, wherein the current is 0.1C, the cut-off voltage is 3.9V, the time is 300min, and the specific formation parameters are shown in Table 5.
(4) Vacuumizing and sealing the cooled battery, wherein the preservation amount of the electrolyte after vacuumizing is 1.5 g/Ah;
(5) and (3) aging the battery cell after vacuum sealing for 72h in an environment with high temperature of 40 +/-3 ℃ and high humidity of 70% RH, selecting products with leakage, bulging and poor side voltage, and finishing formation.
TABLE 5-1 formation parameters for comparative example 1
Serial number Working steps Current (mA) Cut-off voltage (V) Time (min)
1 Constant current charging 150 3.5V 120
2 Constant current charging 300 3.9V 300
Comparative example 2
High-temperature formation process of 356290PL300FY 4.4.4V battery
The closing pressure in example 1 was adjusted to 2.00kg/cm2The second stage pressure was adjusted to 2.00kg/cm2The first step charging current was adjusted to 0.1C (300mA), and the rest remained unchanged from the condition of example 1. Specific formation parameters are shown in tables 6-1 and 6-2.
TABLE 6-1 formation pressure parameter for comparative example 2
Figure BDA0002720852740000081
TABLE 6-2 formation parameters for comparative example 2
Figure BDA0002720852740000082
Comparative example 3
High-temperature formation process of 356290PL300FY 4.4.4V battery
The first stage pressure in example 1 was adjusted to 5.00kg/cm2And the pressure of the fourth stage is adjusted to 20.00kg/cm2The charging current of the middle step was adjusted to 2C (6000mA), and the charging current of the last step was adjusted to 1C (3000mA), and the rest remained unchanged from the conditions of example 1. Specific formation parameters are shown in tables 7-1 and 7-2.
TABLE 7-1 formation pressure parameter for comparative example 3
Figure BDA0002720852740000083
TABLE 7-2 formation parameters for comparative example 3
Figure BDA0002720852740000084
Figure BDA0002720852740000091
Examples of effects
1. Confirmation of battery formation effect
Through comparison tests, the results show that the examples 1 to 4 obviously improve the stripping phenomenon of the negative pole piece of the battery of the comparative example 1, and the results of the examples 1 to 4 and the comparative examples 1 to 3 are respectively shown in the figures 1, 2, 3, 4, 5, 6 and 7.
2. Detection of defective battery
The battery cell after vacuum sealing is placed in an environment with the high temperature of 40 +/-3 ℃ and the high humidity of 70% RH for aging for 72h, so that products with liquid leakage, bulging and poor edge voltage can be quickly and accurately selected, and the figure 8 shows.
3. Battery rate capability test
It was found by comparison that examples 1 to 4 were significantly better in discharge capacity and rate capability than comparative examples 1 to 4, and the film formation uniformity and stability of the SEI film were better. The specific results are shown in Table 8.
TABLE 8 Battery Rate Performance test
Figure BDA0002720852740000092
Figure BDA0002720852740000101
4. Cycle performance test
As can be seen by comparison in fig. 9, the cycling performance of the example 1, example 2, example 3 and example 4 is significantly better than that of the comparative example 1, with the best cycling performance of the example 2 cell.
Comparative example 2 changes the closing pressure, the second stage pressure and the first step charging current compared with example 1, and comparative example 3 changes the 1 st stage pressure, the 4 th stage pressure, the 2 nd step current and the final step current compared with example 1, and the cycle performance is not as good as that of the example.
5. The use of high-temperature pressurization improves the displacement between the electrode core and the aluminum plastic film, and improves the movement of the battery, and the result is shown in fig. 10.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.

Claims (8)

1. A formation method of a polymer lithium ion battery is characterized by comprising the following steps:
(1) after vacuumizing the battery liquid injection, aging;
(2) after the temperature of the pressure formation cabinet reaches 50-70 ℃, the battery is compressed, the closing speed between the layers of the pressure formation cabinet is less than 1cm/s, and the closing pressure is less than or equal to 1kg/cm 2;
(3) the battery is formed by adopting 2-stage step charging and 1-stage step discharging, and adopting 4-stage different pressures; wherein, the cut-off voltage of the 2 nd stage step charging is within 0.15V from full charge to full charge;
(4) cooling;
(5) vacuumizing and sealing the cooled battery;
(6) aging the battery after vacuum sealing to obtain the battery;
wherein, in the step (3), the pressure of the 1 st section is less than or equal to 3kg/cm2The pressure of the 2 nd to 4 th sections is 4 to 15kg/cm2(ii) a The charging current of the 1 st stage of the step charging is 0.2-0.5C; the charging current of the 2 nd step charging is 0.2-1.5C; the step discharge current is 0.2-0.5C.
2. The formation method of the polymer lithium ion battery according to claim 1, wherein the aging temperature in the step (1) is 50 ℃ to 85 ℃.
3. The formation method of the polymer lithium ion battery according to claim 1, wherein the aging time in the step (1) is 3h-24 h.
4. The method for forming a polymer lithium ion battery according to claim 1, wherein in the step (3), the cut-off voltage is less than 3.70V.
5. The method for forming the polymer lithium ion battery according to claim 1, wherein in the step (3), the discharge voltage is 3.90V.
6. The formation method of the polymer lithium ion battery according to claim 1, wherein the cooling in (4) is that the battery is cooled in an environment with the temperature lower than 18 ℃, and the cooling time is more than 1 h.
7. The formation method of the polymer lithium ion battery according to claim 1, wherein in the step (5), after the vacuum pumping, the retention amount of the electrolyte in the battery is 1.5g/Ah-1.9 g/Ah.
8. The formation method of the polymer lithium ion battery according to any one of claims 1 to 7, wherein in the step (6), the environmental conditions for aging the battery are that the temperature is 30 ℃ to 50 ℃, the relative humidity of air is more than 70% RH, and the aging time is more than 48 h.
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