CN111987376A - Lithium iron battery and formation aging and capacity grading process thereof - Google Patents
Lithium iron battery and formation aging and capacity grading process thereof Download PDFInfo
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- CN111987376A CN111987376A CN202010716762.7A CN202010716762A CN111987376A CN 111987376 A CN111987376 A CN 111987376A CN 202010716762 A CN202010716762 A CN 202010716762A CN 111987376 A CN111987376 A CN 111987376A
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- 230000032683 aging Effects 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 34
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 19
- 230000004913 activation Effects 0.000 claims abstract description 22
- 238000007731 hot pressing Methods 0.000 claims abstract description 22
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 12
- 238000001994 activation Methods 0.000 claims description 24
- 238000007600 charging Methods 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 20
- 238000010277 constant-current charging Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 abstract description 5
- 238000007493 shaping process Methods 0.000 abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052744 lithium Inorganic materials 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005086 pumping Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007784 solid electrolyte Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—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
-
- 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
-
- 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
Abstract
A lithium iron battery and a formation aging and capacity grading process thereof belong to the technical field of lithium battery manufacturing. The lithium iron battery formation aging and capacity grading process comprises the steps of firstly carrying out hot pressing on a positive electrode plate, a negative electrode plate and a diaphragm to obtain a battery core, carrying out low-rate activation while carrying out hot pressing, then carrying out primary aging on the battery core, carrying out cyclic activation after the primary aging is finished, then carrying out secondary aging, carrying out vacuum pumping and exhaust on the battery core after the secondary aging, shaping and sealing, and finally carrying out capacity grading to obtain the battery. The battery core can greatly prolong the cycle service life of the battery core and the safety and stability of the battery core, and reduce the bulging degree of the battery core in the use process.
Description
Technical Field
The invention relates to a technology in the field of lithium battery manufacturing, in particular to a lithium iron battery and a formation aging and capacity grading process thereof.
Background
In the first charge and discharge process of the liquid lithium ion battery, the electrode material and the electrolyte react on a solid-liquid phase interface to form a passivation film layer covering the surface of the electrode material. The passivation film layer is effective in preventing the passage of solvent molecules, but Li+But can be freely inserted and extracted, and has the characteristics of a solid electrolyte, and thus this passivation film layer is referred to as a "solid electrolyte interface film (SEI film)". But the SEI film formed in the current lithium battery manufacturing process has not yet reached an ideal state.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the lithium iron battery and the formation aging grading process thereof, which can greatly prolong the cycle service life of the battery cell, improve the safety and stability of the battery cell and reduce the bulging degree of the battery cell in the using process.
The invention relates to a formation aging and capacity grading process for a lithium iron battery, which comprises the steps of firstly carrying out hot pressing on positive and negative pole pieces and a diaphragm to obtain a battery core, carrying out low-rate activation while carrying out hot pressing, then carrying out primary aging on the battery core, carrying out cyclic activation after the primary aging is finished, then carrying out secondary aging, carrying out vacuum pumping and exhausting on the battery core after the secondary aging, shaping and sealing, and finally carrying out capacity grading to obtain the battery.
Preferably, the hot pressing is carried out under a pressure of 0.5 to 3kN and with heating at 30 to 55 ℃.
Preferably, the low-rate activation is constant current charging for 1-10h at a rate of 0.01-0.2C under a hot-pressing condition, and standing after the low-rate activation. Further preferably, the mixture is left standing for 0.5 h.
Preferably, the primary aging is aging at 40-55 ℃ for 12-72 h.
Preferably, the cyclic activation process is as follows: charging with constant current and voltage of 0.2-1C until cut-off voltage is 3.45-3.6V and cut-off current is 0.01-0.05C, standing for 1-10min, discharging with constant current of 0.2-1C until cut-off voltage is 2.0-2.8V, and standing for 1-10 min; repeating the above operation for 2-5 times.
Preferably, the secondary aging is aging at 40-55 deg.C for 12-72 h.
Preferably, the capacity grading process is as follows: charging with 0.2-1C constant current and constant voltage until cut-off voltage is 3.65V and cut-off current is 0.02C, standing for 5min, discharging with 0.2-1C constant current until cut-off voltage is 2.5V, and standing for 5 min; and repeating the charging and discharging steps for 1 time to complete the capacity grading.
The invention relates to a lithium iron battery which is manufactured by adopting the process.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) in the low-rate activation process, the uniform compactness of the SEI film at the interface of the lithium iron cell can be promoted by the low activation current and a certain pressure, and the reaction of a negative interface and an electrolyte can be effectively reduced in the later charging and discharging period of the cell, so that the stability, safety and cyclic usability of the cell are improved;
2) the prepared battery SEI film is more compact and uniform on a microscopic level, is more complete and stable on a macroscopic level, has more sufficient infiltration effect of positive and negative active particulate matters and electrolyte and has better interface reaction effect;
3) the prepared battery has better cycle performance and safety and stability; specifically, on one hand, the normal-temperature cycle life of the battery cell is prolonged to 1500 times of 3700-3800 times on the basis of the original cycle life, and on the other hand, the expansion rate of the battery cell in the cycle process is about 4% -6%, which is far lower than the expansion rate of 11% -14% in the existing process.
Drawings
FIG. 1 is a graph showing the charge-discharge cycle capacity retention ratio of 50Ah cells at room temperature and 1C in example 1.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
According to the embodiment of the invention, the positive and negative pole pieces and the diaphragm are hot-pressed to obtain the battery core, low-rate activation is carried out while hot pressing is carried out, then the battery core is aged for the first time, cyclic activation is carried out after the first aging is finished, then secondary aging is carried out, the battery core is vacuumized and exhausted after the secondary aging, shaped and sealed, and finally capacity grading is carried out to obtain the battery.
Preferably, the hot pressing is carried out under a pressure of 0.5 to 3kN and with heating at 30 to 55 ℃.
Preferably, the low-rate activation is constant current charging for 1 to 8 hours at a rate of 0.01 to 0.15C under a hot-pressing condition, and standing for 0.5 hour after the low-rate activation;
preferably, the primary aging is aging at 40-55 ℃ for 12-72 h.
Preferably, the cyclic activation process is as follows: charging with constant current and voltage of 0.2-1C until cut-off voltage is 3.45-3.6V and cut-off current is 0.01-0.05C, standing for 1-10min, discharging with constant current of 0.2-1C until cut-off voltage is 2.0-2.8V, and standing for 1-10 min; repeating the above operation for 2-5 times.
Preferably, the secondary aging is aging at 40-55 deg.C for 12-72 h.
Preferably, the capacity grading process is as follows: charging with 0.2-1C constant current and constant voltage until cut-off voltage is 3.65V and cut-off current is 0.02C, standing for 5min, discharging with 0.2-1C constant current until cut-off voltage is 2.5V, and standing for 5 min; and repeating the charging and discharging steps for 1 time to complete the capacity grading.
Example 1
In this embodiment, a preparation of a 50Ah square lithium iron cell with an aluminum shell is described as an example, which includes the following steps:
s1, placing the positive and negative pole pieces and the diaphragm in a hot-pressing fixture for hot pressing, wherein the pressure is 2kN, and the temperature is 45 ℃; performing hot pressing and low-rate activation for 8h by constant current charging of 0.5A or 2h by constant current charging of 7.5A, and then standing for 0.5 h;
s2, taking out the battery cell standing in the S1, placing the battery cell in an aging room, and aging for 24 hours at 45 ℃;
s3, after the aging is finished in the S2, the battery cell is taken out and placed in a formation cabinet for cyclic activation, wherein the cycle number is 3; the single procedure was as follows: charging with 25A constant current and constant voltage until cut-off voltage is 3.6V and cut-off current is 1A, standing for 5min, discharging with 25A constant current until cut-off voltage is 2.5V, and standing for 5 min;
s4, taking out the cell in the S3, placing the cell in an aging room, and aging for 36h at 45 ℃;
s5, taking out the battery cell after the aging is finished in the S4, vacuumizing and exhausting the battery cell, shaping and sealing the battery cell, and then placing the battery cell on a grading cabinet for grading; the capacity grading process is as follows: charging with 10A constant current and constant voltage, stopping current at 3.65V and 1A, standing for 5min, discharging with 25A constant current, stopping voltage at 2.5V, and standing for 5 min; then charging with 25A constant current and constant voltage, stopping current at 3.65V and 1A, standing for 5min, discharging with 25A constant current, stopping voltage at 2.5V, and standing for 5 min;
and S6, finally, carrying out capacity internal resistance screening and electrical property spot check test.
In the embodiment, the battery is activated at low multiplying power while hot pressing, the positive and negative pole pieces are effectively and tightly contacted with the diaphragm, the heat conduction efficiency is increased, the battery is activated at high temperature, the rapid formation of the SEI film is promoted, the volume expansion of the battery cell in the formation process is inhibited, and the formed SEI film is more compact and more stable, so that the problems of rapid capacity attenuation and gas generation expansion of the battery cell caused by the rupture and the generation of the SEI film in the initial stage of the charge-discharge cycle process of the battery are solved; subsequent cyclic activation is carried out for a plurality of times, so that the formed SEI film is more sufficient and complete, and the capacity fading rate of the battery cell at the initial stage is obviously reduced; meanwhile, the process can form a good cathode interface, and potential safety hazards and capacity attenuation caused by spot lithium deposition on the cathode interface in the charging and discharging process are avoided.
In the electrical property test, the charge-discharge cycle capacity retention rate of the battery 1C is shown in FIG. 1, and according to the prediction, the normal-temperature cycle life of the final battery core is improved by 1000-3800 times on the original basis to reach 3700-3800 times.
Example 2
In this embodiment, a preparation of a 50Ah square lithium iron cell with an aluminum shell is described as an example, which includes the following steps:
s1, placing the positive and negative pole pieces and the diaphragm in a hot-pressing fixture for hot pressing, wherein the pressure is 0.5kN, and the temperature is 50 ℃; performing hot pressing and simultaneously performing low-rate activation for 1 hour by constant current charging of 5A, and then standing for 0.5 hour;
s2, taking out the battery cell standing in the S1, placing the battery cell in an aging room, and aging for 24 hours at 45 ℃;
s3, after the aging is finished in the S2, the battery cell is taken out and placed in a formation cabinet for cyclic activation, wherein the cycle number is 5; the single procedure was as follows: charging with 40A constant current and constant voltage until cut-off voltage is 3.5V and cut-off current is 2.4A, standing for 5min, discharging with 40A constant current until cut-off voltage is 2.5V, and standing for 5 min;
s4, taking out the cell in the S3, placing the cell in an aging room, and aging for 36h at 45 ℃;
s5, taking out the battery cell after the aging is finished in the S4, vacuumizing and exhausting the battery cell, shaping and sealing the battery cell, and then placing the battery cell on a grading cabinet for grading; the capacity grading process is as follows: charging with 45A constant current and constant voltage, stopping current at 3.65V and 1A, standing for 5min, discharging with 45A constant current, stopping voltage at 2.5V, and standing for 5 min; then charging with a constant current and a constant voltage of 45A, stopping the voltage at 3.65V, stopping the current at 1A, standing for 5min, then discharging with a constant current of 45A, stopping the voltage at 2.5V, and standing for 5 min;
and S6, finally, carrying out capacity internal resistance screening and electrical property spot check test.
Example 3
In this embodiment, a preparation of a 50Ah square lithium iron cell with an aluminum shell is described as an example, which includes the following steps:
s1, placing the positive and negative pole pieces and the diaphragm in a hot-pressing fixture for hot pressing, wherein the pressure is 3kN, and the temperature is 35 ℃; performing hot pressing and simultaneously performing low-rate activation for 5h by 3A constant current charging, and then standing for 0.5 h;
s2, taking out the battery cell standing in the S1, placing the battery cell in an aging room, and aging for 24 hours at 45 ℃;
s3, after the aging is finished in the S2, the battery cell is taken out and placed in a formation cabinet for cyclic activation, wherein the cycle number is 2; the single procedure was as follows: charging with 20A constant current and constant voltage until cut-off voltage is 3.5V and cut-off current is 2.0A, standing for 5min, discharging with 20A constant current until cut-off voltage is 2.3V, and standing for 5 min;
s4, taking out the cell in the S3, placing the cell in an aging room, and aging for 36h at 45 ℃;
s5, taking out the battery cell after the aging is finished in the S4, vacuumizing and exhausting the battery cell, shaping and sealing the battery cell, and then placing the battery cell on a grading cabinet for grading; the capacity grading process is as follows: charging with 30A constant current and constant voltage, stopping current at 3.65V and 1A, standing for 5min, discharging with 30A constant current, stopping voltage at 2.5V, and standing for 5 min; then charging with 30A constant current and constant voltage, stopping current at 3.65V and 1A, standing for 5min, discharging with 30A constant current, stopping voltage at 2.5V, and standing for 5 min;
and S6, finally, carrying out capacity internal resistance screening and electrical property spot check test.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (8)
1. A lithium iron battery formation aging and capacity grading process is characterized in that positive and negative pole pieces and a diaphragm are hot-pressed to obtain a battery core, low-rate activation is carried out while hot pressing is carried out, then primary aging is carried out on the battery core, cyclic activation is carried out after the primary aging is completed, then secondary aging is carried out, the battery core is vacuumized and exhausted after the secondary aging, shaped and sealed, and finally capacity grading is carried out to obtain the battery.
2. The lithium iron battery formation aging capacity grading process as recited in claim 1, wherein the hot pressing is performed under a pressure of 0.5 to 3kN and under a heating condition of 30 to 55 ℃.
3. The formation, aging and capacity grading process for the lithium iron battery as claimed in claim 1, wherein the low-rate activation is constant current charging at a rate of 0.01-0.2C for 1-10h under a hot-pressing condition, and standing after the low-rate activation.
4. The formation, aging and capacity grading process for the lithium iron battery as recited in claim 1, wherein the primary aging is performed for 12-72 hours at 40-55 ℃.
5. The formation, aging and capacity grading process for the lithium iron battery according to claim 1, wherein the cyclic activation process comprises the following steps: charging with constant current and voltage of 0.2-1C until cut-off voltage is 3.45-3.6V and cut-off current is 0.01-0.05C, standing for 1-10min, discharging with constant current of 0.2-1C until cut-off voltage is 2.0-2.8V, and standing for 1-10 min; repeating the above operation for 2-5 times.
6. The formation, aging and capacity grading process for the lithium iron battery according to claim 1, wherein the secondary aging is performed for 12-72 hours at 40-55 ℃.
7. The formation, aging and capacity grading process for the lithium iron battery according to claim 1, wherein the capacity grading process comprises the following steps: charging with 0.2-1C constant current and constant voltage until cut-off voltage is 3.65V and cut-off current is 0.02C, standing for 5min, discharging with 0.2-1C constant current until cut-off voltage is 2.5V, and standing for 5 min; and repeating the charging and discharging steps for 1 time to complete the capacity grading.
8. An iron-lithium battery, characterized in that it is manufactured by the process of any one of claims 1 to 7.
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| CN202010716762.7A CN111987376A (en) | 2020-07-23 | 2020-07-23 | Lithium iron battery and formation aging and capacity grading process thereof |
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| CN202010716762.7A CN111987376A (en) | 2020-07-23 | 2020-07-23 | Lithium iron battery and formation aging and capacity grading process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113036226A (en) * | 2021-03-04 | 2021-06-25 | 昆山兴能能源科技有限公司 | Solid-state battery manufacturing method |
| CN114628791A (en) * | 2022-01-29 | 2022-06-14 | 北京新能源汽车股份有限公司 | Battery cell, method for improving high-temperature performance of battery cell, battery and new energy vehicle |
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| CN109037815A (en) * | 2018-09-21 | 2018-12-18 | 合肥国轩高科动力能源有限公司 | A kind of chemical synthesizing method of ferric phosphate lithium cell |
| CN109713387A (en) * | 2018-12-27 | 2019-05-03 | 肇庆遨优动力电池有限公司 | A method of improving lithium-rich manganese-based lithium ion battery cyclical stability |
| CN110896154A (en) * | 2018-09-13 | 2020-03-20 | 深圳格林德能源有限公司 | Formation process of polymer lithium ion battery |
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- 2020-07-23 CN CN202010716762.7A patent/CN111987376A/en active Pending
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| KR20000042002A (en) * | 1998-12-24 | 2000-07-15 | 김순택 | Formation and aging method of a secondary lithium battery |
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