CN110137585A - A kind of chemical synthesis technology of long-life lithium-ion energy storage battery - Google Patents
A kind of chemical synthesis technology of long-life lithium-ion energy storage battery Download PDFInfo
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- CN110137585A CN110137585A CN201910457477.5A CN201910457477A CN110137585A CN 110137585 A CN110137585 A CN 110137585A CN 201910457477 A CN201910457477 A CN 201910457477A CN 110137585 A CN110137585 A CN 110137585A
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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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Abstract
The present invention provides a kind of chemical synthesis technologies of long-life lithium-ion energy storage battery.Chemical synthesis technology provided by the invention can guarantee the consistency of carbon material used as anode surface filming, the tightness between pole piece effectively being generated when formation SEI film when chemical conversion in amount gas discharge using vacuum plant by gas is discharged twice.Secondary vacuum pumping technique provided by the invention can significantly improve battery cycle life under the conditions of no negative pressure formation cabinet, to meet the needs of low cost and long-life batteries simultaneously.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of chemical conversion work of long-life lithium-ion energy storage battery
Skill.
Background technique
Lithium battery has the advantages that a variety of, the quilts such as energy density is high, light-weight, safety is good, memory-less effect, flexible design
It is widely used in new-energy automobile, mobile power source, energy-accumulating power station etc. product.The lithium battery of part of specification, such as square shell lithium
Battery, partial cylinder lithium battery, the large capacities size battery such as soft-package battery need that negative pressure technique is added in formation process, keep away
Exempt from bulging, excess electrolyte is discharged in size modification.In formation process, battery can generate bulk gas in forming SEI film,
Gas is discharged the uniformity that will affect film forming not in time, and SEI film will affect the internal resistance of finished battery, capacity, cycle life, from
The multiple parameters such as discharge level, maximum discharge current, and the formation of SEI film is a kind of irreversible state, therefore negative pressure
Superiority and inferiority at technique not just to guarantee that the gas that generates in battery forming process is sucked out, to avoid battery core oxygen blast cyanidation,
The factors such as compactness variation between pole piece；Also determine compactness, uniformity and the consistency of the formation of SEI film.
Existing technical solution mostly uses negative pressure formation cabinet so that the gas generated in formation process, such as patent No. to be discharged in time
CN201010226552.6, CN201520109286.7 etc..But negative pressure formation device is at high cost, be not suitable for energy storage etc. at
This more demanding industry.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of chemical conversion of long-life lithium-ion energy storage battery
Technique, secondary vacuum pumping technique provided by the invention can significantly improve battery cycle life under the conditions of no negative pressure formation cabinet, with
Meets the needs of low cost and long-life batteries simultaneously.
The present invention provides a kind of chemical synthesis technologies of long-life lithium-ion energy storage battery, comprising the following steps:
A the battery after fluid injection is shelved) is subjected to initial charge, is suspended after the completion, the battery after being suspended is described
The voltage of initial charge is the 10~20% of rated capacity；
B) battery after pause that step A) is obtained is placed in vacuum plant and vacuumize for the first time, is carried out after the completion
Second of charging, suspends, the battery after being suspended after charging complete；
The time vacuumized for the first time is 1~2 hour, and vacuum values are -50~-60KPa；
The voltage of second of charging is the 65~85% of rated capacity；
C the battery after pause that step B) is obtained is vacuumized for the second time), third time charging is carried out after the completion, obtains
Battery after to chemical conversion；
The time vacuumized for the second time is 1~2 hour, and vacuum values are -50~-60KPa.
Preferably, the initial charge electric current, second of charging current and third time charging current is independent is selected from
0.01C~0.3C.
Preferably, the battery is selected from ferric phosphate lithium cell or ternary lithium battery.
Preferably, the battery is ferric phosphate lithium cell, step A) in, the method that carries out initial charge are as follows:
0.01C~0.1C constant-current charge, time are 1~3 hour, and voltage is 3.2~3.3V, shelve 5~after ten minutes, then
In 0.05~0.15C constant-current charge, voltage limits 3.2~3.3V, suspends after the completion.
Preferably, the battery is ferric phosphate lithium cell, step B) in, it vacuumizes for the first time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is stopped when being evacuated to -30kpa
Only, it keeps being vacuumized again for 5~10 minutes, until stopping when -50Kpa~-60Kpa, is kept for 1~2 hour, be put into after the completion dry
Dry nitrogen takes out battery；
Second of charging are as follows: electric current 0.05~0.15C constant-current charge, time restriction 30~60 minutes, voltage limitation 3.4~
3.45V is shelved 5~10 minutes, turns 0.15~0.2C constant-current charge, and voltage is 3.4~3.5V, is suspended after the completion.
Preferably, the battery is ferric phosphate lithium cell, step C) in, the method that vacuumizes for the second time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is evacuated to -30~40kpa
When stop, keeping being vacuumized again for 5~10 minutes, when -50~-60Kpa stops, and is kept for 1~2 hour, is put into after the completion dry
Dry nitrogen takes out battery；
Third time charges are as follows: the battery after vacuumizing for the second time will be completed in electric current 0.2~0.3C constant-current constant-voltage charging, when
Between 200~300 minutes, voltage 3.65V, shelve 5~10 minutes, complete chemical conversion.
Preferably, the battery is ternary lithium battery, step A) in, the method that carries out initial charge are as follows:
0.01C~0.1C constant-current charge, time restriction 1~3 hour, voltage was 3.6~3.8V, was shelved 5 minutes, turned 0.05
~0.1C constant-current charge, voltage limit 3.6~38V, suspend after the completion.
Preferably, the battery is ternary lithium battery, step B) in, the method that vacuumizes for the first time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is stopped when being evacuated to -30kpa
Only, it keeps being vacuumized again for 5~10 minutes, when -50Kpa~-60Kpa stops, and is kept for 1~2 hour, is put into drying after the completion
Nitrogen takes out battery；
The method of second of charging are as follows:
Electric current 0.1C~0.15C constant-current charge, time are 30~60 minutes, and voltage is 3.8~4.0V, shelves 5~10 points
Clock, turns 0.15C~0.2C constant-current charge, and voltage limits 3.8~4.0V, suspends after the completion.
Preferably, the battery is ternary lithium battery, step C) in, the method that vacuumizes for the second time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is evacuated to -30~35kpa
When stop, keeping being vacuumized again for 5~10 minutes, when -50~-60Kpa stops, and is kept for 1~2 hour, is put into after the completion dry
Dry nitrogen takes out battery；
The method of third time charging are as follows:
The battery after vacuumizing for the second time will be completed in 0.2~0.3C constant-current constant-voltage charging, the time is 200~300 minutes,
Voltage is 4.2V, is shelved 5~10 minutes.
Preferably, the charging voltage of the third time charging is 100% rated capacity.
Compared with prior art, the present invention provides a kind of chemical synthesis technologies of long-life lithium-ion energy storage battery, including with
Lower step: A) by the battery progress initial charge after fluid injection is shelved, suspend after the completion, the battery after being suspended is described
The voltage of initial charge is the 10~20% of rated capacity；B) battery after the pause is placed in vacuum plant and carries out first
It is secondary to vacuumize, it carries out charging for second after the completion, suspend after charging complete, the battery after being suspended；It vacuumizes for the first time
Time is 1~2 hour, and vacuum values are -50~-60KPa；The voltage of second of charging is the 65~85% of rated capacity；C) will
Step B) battery after obtained pause vacuumized for the second time, third time charging, the electricity after being melted into are carried out after the completion
Pond；The time vacuumized for the second time is 1~2 hour, and vacuum values are -50~-60KPa.Chemical synthesis technology provided by the invention uses
Vacuum plant can guarantee by gas is discharged twice effectively being generated when formation SEI film when chemical conversion in amount gas discharge
The consistency of carbon material used as anode surface filming, the tightness between pole piece.Secondary vacuum pumping technique provided by the invention is without negative
Battery cycle life can be significantly improved under the conditions of pressure formation cabinet, to meet the needs of low cost and long-life batteries simultaneously.
Detailed description of the invention
Fig. 1 is 1 battery capacity comparison diagram of embodiment 1 and comparative example；
Fig. 2 is embodiment 1 (left figure) and comparative example 1 (right figure) negative terminal surface state vs；
Fig. 3 is 2 battery capacity comparison diagram of embodiment 1 and comparative example；
Fig. 4 is 3 battery capacity comparison diagram of embodiment 2 and comparative example；
Fig. 5 is 4 battery capacity comparison diagram of embodiment 3 and comparative example；
Fig. 6 is 4 battery cycle life comparison diagram of embodiment 3 and comparative example；
Fig. 7 is 5 battery capacity comparison diagram of embodiment 5 and comparative example；
Fig. 8 is embodiment 5 (right side) and comparative example 5 (left side) negative terminal surface state vs；
Fig. 9 is 6 battery capacity comparison diagram of embodiment 4 and comparative example；
Figure 10 is embodiment 4 (left side) and comparative example 6 (right side) negative terminal surface state vs；
Figure 11 is 7 battery capacity comparison diagram of embodiment 3 and comparative example.
Specific embodiment
The present invention provides a kind of chemical synthesis technologies of long-life lithium-ion energy storage battery, comprising the following steps:
A the battery after fluid injection is shelved) is subjected to initial charge, is suspended after the completion, the battery after being suspended is described
The voltage of initial charge is the 10-20% of rated capacity；
B) battery after the pause is placed in vacuum plant and vacuumize for the first time, is filled for the second time after the completion
Electricity, suspends after charging complete, the battery after being suspended；
The time vacuumized for the first time is 1~2 hour, and vacuum values are -50~-60KPa；
The voltage of second of charging is the 65-85% of rated capacity；
C the battery after pause that step B) is obtained is vacuumized for the second time), third time charging is carried out after the completion, obtains
Battery after to chemical conversion；
The time vacuumized for the second time is 1~2 hour, and vacuum values are -50~-60KPa.
Battery after fluid injection is shelved is melted by the present invention, wherein the battery is selected from selected from LiFePO4 electricity
Pond or ternary lithium battery.The method that the present invention shelves the fluid injection there is no specifically limited, well known to a person skilled in the art
Method.
Specifically, the battery after fluid injection is shelved is carried out initial charge, wherein the voltage of the initial charge is volume
The 10%~20% of constant volume, preferably 14%~16%.
When the battery is ferric phosphate lithium cell, step A) in, the method that carries out initial charge are as follows:
The constant-current charge of 0.01C~0.1, time are 1~3 hour, and voltage is 3.2~3.3V, shelve 5~after ten minutes, then
In 0.05~0.15C constant-current charge, voltage limits 3.2~3.3V, suspends after the completion.
When the battery is ternary lithium battery, step A) in, the method that carries out initial charge are as follows:
0.01C~0.1C constant-current charge, time restriction 1~3 hour, voltage was 3.6V~3.8V, was shelved 5~10 minutes,
Turn 0.05~0.15C constant-current charge, voltage limits 3.6~3.8V, suspends after the completion.
Suspend after the completion, the battery after being suspended；Then, the battery after the pause is placed in vacuum plant and is carried out
It vacuumizes for the first time.The time vacuumized for the first time is 1~2 hour, and vacuum values are -50~-60KPa.
When the battery is ferric phosphate lithium cell, step B) in, it vacuumizes for the first time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is stopped when being evacuated to -30kpa
Only, it keeps being vacuumized again for 5~10 minutes, until stopping when -50Kpa~-60Kpa, is kept for 1~2 hour, be put into after the completion dry
Dry nitrogen takes out battery；
When the battery is ternary lithium battery, step B) in, the method that vacuumizes for the first time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is stopped when being evacuated to -30kpa
Only, it keeps being vacuumized again for 5~10 minutes, when -50Kpa~-60Kpa stops, and is kept for 1~2 hour, is put into drying after the completion
Nitrogen takes out battery.
It carries out charging for second after the completion, suspend after charging complete, the battery after being suspended.The voltage of second of charging
It is the 65~85% of rated capacity, preferably 70%~80%.
Specifically, the battery is ferric phosphate lithium cell, second of charging are as follows: electric current 0.1C~0.15C constant-current charge, when
Between limit 30~60 minutes, voltage limits 3.4V, shelves 5~10 minutes, turns 0.15C~0.2C constant-current charge, voltage is 3.4~
3.5V suspends after the completion.
The battery is ternary lithium battery, the method for second of charging are as follows:
Electric current 0.1C~0.15C constant-current charge, time are 30~60 minutes, and voltage is 3.8~4.0V, shelves 5~10 points
Clock, turns the constant-current charge of 0.15C~0.2, and voltage limits 3.8~4.0V, suspends after the completion.
Battery after pause that step B) is obtained is vacuumized for the second time, the time vacuumized for the second time is 1~2 small
When, vacuum values are -50~-60KPa.
When the battery is ferric phosphate lithium cell, step C) in, the method that vacuumizes for the second time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is evacuated to -30~35kpa
When stop, keeping being vacuumized again for 5~10 minutes, when -50~-60Kpa stops, and is kept for 1~2 hour, is put into after the completion dry
Dry nitrogen takes out battery；
When the battery is ternary lithium battery, step C) in, the method that vacuumizes for the second time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is evacuated to -30~35kpa
When stop, keeping being vacuumized again for 5~10 minutes, when -50~-60Kpa stops, and is kept for 1~2 hour, is put into after the completion dry
Dry nitrogen takes out battery.
Third time charging, the battery after being melted into are carried out after the completion.The charging voltage of third time charging be for
100% rated capacity.
When the battery is ferric phosphate lithium cell, third time charges are as follows: will complete the battery after vacuumizing for the second time and exists
Electric current 0.2~0.3C constant-current constant-voltage charging, the time 200~300 minutes, voltage 3.65V was shelved 5 minutes, completed chemical conversion.
When the battery is ternary lithium battery, the method for third time charging are as follows:
The battery after vacuumizing for the second time will be completed in 0.2~0.3C constant-current constant-voltage charging, the time is 200~300 minutes,
Voltage is 4.2V, is shelved 5~10 minutes.
By gas is discharged twice, can guarantee effectively being generated when formation SEI film when chemical conversion in amount gas discharge
The consistency of film forming, the tightness between pole piece.
The present invention carries out the device of initial charge, second charging and third time charging there is no specifically limited to battery,
It can complete battery charging, preferably formation cabinet.
The type for the vacuum plant that the present invention vacuumizes the first time and vacuumizes for the second time is not particularly limited, energy
Vacuumize the device of substitution gas, preferably vacuum oven.In the present invention, it can be set completely without using negative pressure chemical conversion
It is standby to be vacuumized, reduce the cost of chemical conversion.
In the present invention, between charging and vacuum pumping, battery is transported through in process and vacuum plant and is needed
Whole process guarantees ambient dew point≤- 40 DEG C.
Chemical synthesis technology provided by the invention, using vacuum plant by gas is discharged twice, can effectively chemical conversion when
What is generated when forming SEI film is discharged in amount gas, guarantees the consistency of carbon material used as anode surface filming, close between pole piece
Degree.Secondary vacuum pumping technique provided by the invention can significantly improve battery cycle life under the conditions of no negative pressure formation cabinet, with same
When meet low cost and the needs of long-life batteries.
For a further understanding of the present invention, below with reference to embodiment to long-life lithium-ion energy storage battery provided by the invention
Chemical synthesis technology be illustrated, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Positive LiFePO4 LiFePO4 is main material
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.05C constant-current charge, when
Between limit 1 hour, voltage limits 3.20V, shelves 5 minutes, turns 0.1C constant-current charge, and voltage limits 3.2V, suspends after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -60Kpa stops, and is kept for 1 hour, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging, it is noted that all transport process and vacuum tank need whole process to guarantee environment at this time
Dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.1C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 3.4V, shelves 5 minutes, turned 0.15C constant-current charge, and voltage limits 3.4V, after the completion
Pause；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -60Kpa stops, and is kept for 1.5 hours, is put into after the completion dry
Dry nitrogen, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.2C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 3.65V, shelved 5 minutes, completed chemical conversion.
Comparative example 1
(10PCS battery is taken to compare) based on embodiment 1, the difference with embodiment 1 is only without for the first time
Chemical conversion is completed in the operation for vacuumizing and vacuumizing for the second time.
Battery capacity comparison, the result is shown in Figure 1 are carried out to the battery that embodiment 1 and comparative example 1 obtain, Fig. 1 is 1 He of embodiment
1 battery capacity comparison diagram of comparative example.
Negative terminal surface state observation is carried out to the battery that embodiment 1 and comparative example 1 obtain, as a result sees that Fig. 2, Fig. 2 are to implement
Example 1 (left figure) and comparative example 1 (right figure) negative terminal surface state vs.As shown in Figure 2, there is not embedding lithium on 1 negative electrode tab surface of comparative example
The blackspot that region is formed, 1 negative electrode tab color of embodiment is uniform, without not embedding lithium region.
Comparative example 2
(10PCS battery is taken to compare) based on embodiment 1, the difference with embodiment 1 is to be melted into work using negative pressure
Skill, specifically:
1) the battery restocking after fluid injection is shelved will be completed to negative pressure formation device, negative-pressure vacuum degree is set as -60Kpa；
2) initial charge is carried out, electric current 0.05C constant-current charge, time restriction 1 hour, voltage limited 3.2V, shelved 5 points
Clock, electric current 0.1C charging, voltage limit 3.2V；
3) it shelves 5 minutes, electric current 0.15C constant-current charge, time restriction 2 hours, voltage limits 3.4V；
4) it shelves 5 minutes, electric current 0.2C constant-current constant-voltage charging, time restriction 300 minutes, voltage limits 3.65V, shelves 5
Minute, complete chemical conversion.
Battery capacity comparison is carried out to the battery that embodiment 1 and comparative example 2 obtain, as a result sees that Fig. 3, Fig. 3 are 1 He of embodiment
2 battery capacity comparison diagram of comparative example.
Embodiment 2
Positive ternary lithium Li (NiCoMn) O2Trielement composite material is main material
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.05C constant-current charge, when
Between limit 1 hour, voltage limits 3.6V, shelves 5 minutes, turns 0.1C constant-current charge, and voltage limits 3.6V, suspends after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -60Kpa stops, and is kept for 1.5 hours, is put into after the completion dry
Dry nitrogen, takes out battery, and upper formation cabinet connects charging, it is noted that all transport process and vacuum tank need whole process to guarantee ring at this time
Border dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.1C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 4.0V, shelves 5 minutes, turned 0.15C constant-current charge, and voltage limits 4.0V, after the completion
Pause；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -60Kpa stops, and is kept for 2 hours, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.2C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 4.2V, shelved 5 minutes, completed chemical conversion.
Comparative example 3
(10PCS battery is taken to compare) based on embodiment 2, the difference with embodiment 2 is only without for the first time
Chemical conversion is completed in the operation for vacuumizing and vacuumizing for the second time.
Battery capacity comparison is carried out to the battery that embodiment 2 and comparative example 3 obtain, as a result sees that Fig. 4, Fig. 4 are 2 He of embodiment
3 battery capacity comparison diagram of comparative example.
Embodiment 3
Positive LiFePO4 LiFePO4Secondary vacuum pumping process the following steps are included:
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.1C constant-current charge, when
Between limit 1 hour, voltage limit 3.2V, suspend after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -60Kpa stops, and is kept for 1 hour, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging, it is noted that all transport process and vacuum tank need whole process to guarantee environment at this time
Dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.1C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 3.4V, shelves 5 minutes, turned 0.15C constant-current charge, and voltage limits 3.4V, after the completion
Pause；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -60Kpa stops, and is kept for 2 hours, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.2C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 3.65V, shelved 5 minutes, completed chemical conversion.
Comparative example 4
(10PCS battery is taken to compare) based on embodiment 3, the difference with embodiment 3 is only without for the first time
Chemical conversion is completed in the operation for vacuumizing and vacuumizing for the second time.
Battery capacity comparison is carried out to the battery that embodiment 3 and comparative example 4 obtain, as a result sees that Fig. 5, Fig. 5 are 3 He of embodiment
4 battery capacity comparison diagram of comparative example.
Battery cycle life is carried out to the battery that embodiment 3 and comparative example 4 obtain to be compared, and as a result sees that Fig. 6, Fig. 6 are
4 battery cycle life comparison diagram of embodiment 3 and comparative example.
Embodiment 4
Positive LiFePO4 LiFePO4 secondary vacuum pumping process the following steps are included:
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.03C constant-current charge, when
Between limit 2 hours, voltage limit 3.2V, shelve 10 minutes, electric current 0.1C charging, limit voltage 3.2V, suspend after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 5 minutes, and when -50Kpa stops, and is kept for 1.5 hours, is put into after the completion dry
Dry nitrogen, takes out battery, and upper formation cabinet connects charging, it is noted that all transport process and vacuum tank need whole process to guarantee ring at this time
Border dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.15C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 3.4V, shelves 5 minutes, turned 0.2C constant-current charge, and voltage limits 3.4V, after the completion temporarily
Stop；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 5 minutes, and when -50Kpa stops, and is kept for 2 hours, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.3C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 3.65V, shelved 5 minutes, completed chemical conversion.
Embodiment 5
Positive ternary lithium Li (NiCoMn) O2 trielement composite material secondary vacuum pumping process the following steps are included:
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.05C constant-current charge, when
Between limit 1 hour, voltage limit 3.7V, shelve 10 minutes, electric current 0.1C charging, limit voltage 3.7V, suspend after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -50Kpa is kept for 1.5 hours, is put into drying nitrogen after the completion, takes out battery, and upper formation cabinet connects charging, asks
Notice that all transport process at this time and vacuum tank need whole guarantee ambient dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.15C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 4.0V, shelves 5 minutes, turned 0.2C constant-current charge, and voltage limits 4.0V, after the completion temporarily
Stop；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -50Kpa is kept for 2 hours, is put into drying nitrogen after the completion, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.2C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 4.2V, shelved 5 minutes, completed chemical conversion.
Comparative example 5
Positive ternary lithium Li (NiCoMn) O2 trielement composite material secondary vacuum pumping process the following steps are included:
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.05C constant-current charge, when
Between limit 1 hour, voltage limit 3.7V, shelve 10 minutes, electric current 0.1C charging, limit voltage 3.7V, suspend after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -40Kpa is kept for 1.5 hours, is put into drying nitrogen after the completion, takes out battery, and upper formation cabinet connects charging, asks
Notice that all transport process at this time and vacuum tank need whole guarantee ambient dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.15C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 4.0V, shelves 5 minutes, turned 0.2C constant-current charge, and voltage limits 4.0V, after the completion temporarily
Stop；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -50Kpa is kept for 2 hours, is put into drying nitrogen after the completion, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.2C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 4.2V, shelved 5 minutes, completed chemical conversion.
Embodiment 5 and the difference of comparative example 5 are that it is -40kpa that comparative example 5 takes out genuine vacuum degree twice, and vacuum degree is small
A bit, inside battery gas is not discharged all, and there are gases among pole piece, influence battery capacity, equally takes 10Pcs battery with capacity
As a comparison: referring to figs. 7 and 8, Fig. 7 be 5 battery capacity comparison diagram of embodiment 5 and comparative example, Fig. 8 be embodiment 5 (left side) and
Comparative example 5 (right side) negative terminal surface state vs.
Comparative example 6
Evacuation process method of positive LiFePO4 LiFePO4 the following steps are included:
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.03C constant-current charge, when
Between limit 2 hours, voltage limit 3.2V, shelve 10 minutes, electric current 0.1C charging, limit voltage 3.2V,
2) it shelves 5 minutes, electric current 0.15C constant-current charge, time restriction 30 minutes, voltage limits 3.4V, it shelves 5 minutes,
Turn 0.2C constant-current charge, voltage limits 3.4V, suspends after the completion；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 5 minutes, and when -60Kpa stops, and is kept for 2 hours, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.3C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 3.65V, shelved 5 minutes, completed chemical conversion.
Embodiment 4 and the difference of comparative example 6 are that comparative example 6 becomes primary from vacuumizing twice, omit and take out for the first time very
Sky only stays second of suction, and vacuum number is reduced once, and inside battery gas is not discharged all, influences battery capacity, together
Sample take 10Pcs battery with capacity as a comparison: referring to Fig. 9 and Figure 10, Fig. 9 is that embodiment 4 and 6 battery capacity of comparative example compare
Figure, Figure 10 are embodiment 4 (left side) and comparative example 6 (right side) negative terminal surface state vs.
Comparative example 7
Positive LiFePO4 LiFePO4 secondary vacuum pumping process the following steps are included:
1) will complete fluid injection shelve after battery restocking to formation cabinet progress initial charge, electric current 0.1C constant-current charge, when
Between limit 1 hour, voltage limit 3.2V, suspend after the completion；
2) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -80Kpa stops, and is kept for 1 hour, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging, it is noted that all transport process and vacuum tank need whole process to guarantee environment at this time
Dew point≤- 40 DEG C；
3) the battery restocking after vacuumizing for the first time will be completed and carries out connecting charging to formation cabinet, electric current 0.1C constant current is filled
Electricity, time restriction 30 minutes, voltage limited 3.4V, shelves 5 minutes, turned 0.15C constant-current charge, and voltage limits 3.4V, after the completion
Pause；
4) the battery transfer car(buggy) undercarriage after suspending is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum
Stopping when being evacuated to -30kpa keeps being vacuumized again for 10 minutes, and when -80Kpa stops, and is kept for 2 hours, is put into drying after the completion
Nitrogen, takes out battery, and upper formation cabinet connects charging；
5) the battery restocking after vacuumizing for the second time will be completed and carries out connecting charging, electric current 0.2C constant current constant voltage to formation cabinet
Charging, time restriction 300 minutes, voltage limited 3.65V, shelved 5 minutes, completed chemical conversion.
Embodiment 3 and the difference of comparative example 7 be, it is -80kpa that comparative example 7 takes out genuine vacuum degree twice, vacuum degree is big -
20Kpa, inside battery electrolyte are extracted with gas, and inside battery influences battery capacity because lacking electrolyte, equally
It takes 10Pcs battery capacity as a comparison: being 7 battery capacity comparison diagram of embodiment 3 and comparative example referring to Figure 11, Figure 11.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of chemical synthesis technology of long-life lithium-ion energy storage battery, which comprises the following steps:
A) by after fluid injection is shelved battery carry out initial charge, suspend after the completion, the battery after being suspended, it is described for the first time
The voltage of charging is the 10~20% of rated capacity；
B) battery after pause that step A) is obtained is placed in vacuum plant and vacuumize for the first time, carries out second after the completion
Secondary charging, suspends after charging complete, the battery after being suspended；
The time vacuumized for the first time is 1~2 hour, and vacuum values are -50~-60KPa；
The voltage of second of charging is the 65~85% of rated capacity；
C the battery after pause that step B) is obtained is vacuumized for the second time), third time charging is carried out after the completion, is changed
Battery after；
The time vacuumized for the second time is 1~2 hour, and vacuum values are -50~-60KPa.
2. chemical synthesis technology according to claim 1, which is characterized in that the initial charge electric current, second of charging current
And third time charging current is independent selected from 0.01C~0.3C.
3. chemical synthesis technology according to claim 1, which is characterized in that the battery is selected from ferric phosphate lithium cell or ternary lithium
Battery.
4. chemical synthesis technology according to claim 3, which is characterized in that the battery is ferric phosphate lithium cell, step A) in,
The method for carrying out initial charge are as follows:
0.01C~0.1C constant-current charge, time are 1~3 hour, and voltage is 3.2~3.3V, shelve 5~after ten minutes, then
0.05~0.15C constant-current charge, voltage limit 3.2~3.3V, suspend after the completion.
5. chemical synthesis technology according to claim 3, which is characterized in that the battery is ferric phosphate lithium cell, step B) in,
It vacuumizes for the first time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, and stopping when vacuum is evacuated to -30kpa is protected
It holds 5~10 minutes and is vacuumized again, until stopping when -50Kpa~-60Kpa, kept for 1~2 hour, be put into dry nitrogen after the completion
Gas takes out battery；
Second of charging are as follows: electric current 0.05~0.15C constant-current charge, time restriction 30~60 minutes, voltage limitation 3.4~
3.45V is shelved 5~10 minutes, turns 0.15~0.2C constant-current charge, and voltage is 3.4~3.5V, is suspended after the completion.
6. chemical synthesis technology according to claim 3, which is characterized in that the battery is ferric phosphate lithium cell, step C) in,
The method vacuumized for the second time are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is stopped when being evacuated to -30~40kpa
Only, it keeps being vacuumized again for 5~10 minutes, when -50~-60Kpa stops, and is kept for 1~2 hour, is put into dry nitrogen after the completion
Gas takes out battery；
Third time charges are as follows: will complete the battery after vacuumizing for the second time in electric current 0.2~0.3C constant-current constant-voltage charging, time
It 200~300 minutes, voltage 3.65V, shelves 5~10 minutes, completes chemical conversion.
7. chemical synthesis technology according to claim 3, which is characterized in that the battery is ternary lithium battery, step A) in, into
The method of row initial charge are as follows:
0.01C~0.1C constant-current charge, time restriction 1~3 hour, voltage be 3.6~3.8V, shelve 5 minutes, turn 0.05~
0.1C constant-current charge, voltage limit 3.6~38V, suspend after the completion.
8. chemical synthesis technology according to claim 3, which is characterized in that the battery is ternary lithium battery, step B) in, the
The method once vacuumized are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, and stopping when vacuum is evacuated to -30kpa is protected
It holds 5~10 minutes and is vacuumized again, when -50Kpa~-60Kpa, stops, and it is kept for 1~2 hour, is put into drying nitrogen after the completion,
Take out battery；
The method of second of charging are as follows:
Electric current 0.1C~0.15C constant-current charge, time are 30~60 minutes, and voltage is 3.8~4.0V, is shelved 5~10 minutes, are turned
0.15C~0.2C constant-current charge, voltage limit 3.8~4.0V, suspend after the completion.
9. chemical synthesis technology according to claim 3, which is characterized in that the battery is ternary lithium battery, step C) in, the
The method of secondary vacuum pumping are as follows:
Battery after pause is put into vacuum oven, closes vacuum chamber door and starts to vacuumize, vacuum is stopped when being evacuated to -30~35kpa
Only, it keeps being vacuumized again for 5~10 minutes, when -50~-60Kpa stops, and is kept for 1~2 hour, is put into dry nitrogen after the completion
Gas takes out battery；
The method of third time charging are as follows:
The battery after vacuumizing for the second time will be completed in 0.2~0.3C constant-current constant-voltage charging, the time is 200~300 minutes, voltage
For 4.2V, shelve 5~10 minutes.
10. chemical synthesis technology according to claim 1, which is characterized in that the charging voltage of the third time charging is 100%
Rated capacity.
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