CN115207500A - Negative pulse formation and capacity grading method for lithium iron phosphate cylindrical battery - Google Patents

Negative pulse formation and capacity grading method for lithium iron phosphate cylindrical battery Download PDF

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CN115207500A
CN115207500A CN202210937480.9A CN202210937480A CN115207500A CN 115207500 A CN115207500 A CN 115207500A CN 202210937480 A CN202210937480 A CN 202210937480A CN 115207500 A CN115207500 A CN 115207500A
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charging
discharging
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王乾
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Suzhou Times Huajing New Energy 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
    • 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
    • H01M10/4285—Testing apparatus
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a negative pulse formation and capacity grading method for a lithium iron phosphate cylindrical battery, which comprises the following steps of dividing a charging process into a plurality of charging cycles in the formation process or the capacity grading process, wherein the charging current value changes in a stepped manner in two adjacent charging cycles; each charging cycle comprises a charging stage, a discharging stage and a resting stage, wherein in the same charging cycle, the charging stage and the discharging stage are both constant-current charging or constant-current discharging, the current value of the discharging stage is greater than that of the charging stage, and the discharging time of the discharging stage is less than that of the charging stage. In the gap of the step charging, a negative pulse method is introduced to relieve concentration polarization and electrochemical polarization, and ohmic polarization is eliminated after the negative pulse.

Description

Negative pulse formation and capacity grading method for lithium iron phosphate cylindrical battery
Technical Field
The invention belongs to the field of battery manufacturing, and particularly relates to a negative pulse formation and capacity grading method for a lithium iron phosphate cylindrical battery.
Background
After the lithium ion battery is assembled, the lithium ion battery must be charged to activate positive and negative active materials, an SEI film is formed on the surface of a negative electrode, and the first lithium intercalation and lithium deintercalation of the negative electrode are completed at the same time. Formation is a very complex process and is also an important process that affects battery performance. After formation, the capacity is divided, the battery is charged and discharged by 100 percent DOD once, the capacity value of the battery is tested, whether the capacity is qualified is judged, and the battery with the same capacity grade is provided for subsequent battery pack assembly. Therefore, formation and capacity classification are important processes for activation and sorting of batteries, and the quality and efficiency of the processes have a great influence on lithium ion batteries.
The formation time of the power battery is different according to different material systems and different process flows. In the battery manufacturing procedure, the procedure time of formation and capacity grading is longer, and a large amount of equipment resources and procedure time are occupied.
The anode is mainly made of a ternary material and a lithium iron phosphate material, and the lithium iron phosphate has low diffusion coefficient in lithium and small charge-discharge current ratio to ternary; meanwhile, the charging curve of the half-cell can also be seen, the lithium iron phosphate half-cell has a longer charging platform, and the charging curve platform of the ternary material is relatively smaller; when the capacity of the full battery is divided to the final charging stage, in order to improve the voltage of the full battery, the reduction of the negative electrode potential of the lithium iron phosphate battery is quicker under the same current density, and the over potential is more easily generated to cause lithium precipitation. Therefore, the NP of the lithium iron phosphate battery needs to be given larger to ensure that the potential of the negative electrode of the capacity-separation charging does not precipitate lithium.
At present, the formation time of the lithium iron phosphate battery is generally 4-9h, the capacity grading time is generally 6-12h, and the capacity grading time of the ternary material battery under the same condition can be shortened by 10% -30%. Therefore, on the premise of ensuring the precision, the formation and grading efficiency of the lithium iron phosphate battery is improved, the working procedure time is shortened, and the method has greater economic benefit.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides a negative pulse formation and capacity grading method for a lithium iron phosphate cylindrical battery, which can greatly improve the formation and capacity grading efficiency of the lithium iron phosphate battery and shorten the working procedure time.
The technical scheme is as follows: in order to realize the purpose, the technical scheme of the invention is as follows:
a negative pulse formation and capacity grading method for a lithium iron phosphate cylindrical battery comprises a formation process and a capacity grading process, wherein in the formation process or the capacity grading process:
placing the battery cell in a corresponding formation temperature or capacity grading temperature environment, dividing a charging process into a plurality of charging periods, wherein in two adjacent charging periods, the charging current value changes in a stepped manner;
each charging cycle comprises a charging stage, a discharging stage and a resting stage, wherein the charging voltage limiting of the charging stage is the same in a plurality of charging cycles, the discharging voltage limiting of the discharging stage is the same, the charging stage enters the discharging stage after reaching the charging voltage limiting, and the resting stage enters after reaching the discharging voltage limiting;
in the same charging cycle, the charging stage and the discharging stage are both constant current charging or constant current discharging, the current value of the discharging stage is greater than that of the charging stage, and the discharging time of the discharging stage is less than that of the charging stage.
Furthermore, in the formation process or the capacity grading process, the charging current values of a plurality of charging stages are firstly from small to large and then from large to small.
Further, the discharge current range of the discharge stage in the formation process is 1C-3C; the discharge current range of the discharge stage in the capacity grading procedure is 2C-5C.
Further, the shelf time of the shelf stage in the formation process or the grading process ranges from 5s to 20s.
Further, the formation temperature range in the formation procedure is 40-50 ℃; the volume separation temperature range in the volume separation procedure is 20-30 ℃.
Further, the formation process comprises the following steps:
step 1: standing for 3min before charging;
step 2: charging at constant current of 0.05 ℃ for 120min, and limiting the voltage to 3.65V;
and 3, step 3: standing for 10min;
and 4, step 4: charging at 0.2C for 22min, and limiting voltage to 3.65V;
and 5, step 5: discharging at 1.5C constant current for 10s, and limiting voltage to 2.0V;
and 6, step 6: standing for 10s;
and 7, step 7: charging at 0.5C for 12min, and limiting voltage to 3.65V;
and 8, step 8: discharging at 2C constant current for 10s, and limiting voltage to 2.0V;
step 9: standing for 10s;
step 10: charging at 1.0C for 9min, and limiting voltage to 3.65V;
and 11, step 11: discharging at 2.5C constant current for 10s, and limiting voltage to 2.0V;
step 12: standing for 10s;
step 13: charging at 0.5C for 12min, and limiting voltage to 3.65V;
step 14: discharging at 2C constant current for 10s, and limiting voltage to 2.0V;
step 15: standing for 10min;
step 16: and finishing the formation.
Further, in the capacity grading process, the method comprises the following steps:
step 1: standing for 3min before charging;
step 2: charging at 1.5C for 6min, and limiting voltage to 3.65V;
and 3, step 3: discharging at 3C constant current for 10s, and limiting voltage to 2.0V;
and 4, step 4: standing for 10s;
and 5, step 5: charging at 1C for 9min with constant current, and limiting voltage to 3.65V;
and 6, step 6: discharging at 3C constant current for 10s, and limiting voltage to 2.0V;
and 7, step 7: standing for 10s;
and 8, step 8: charging at 0.5C for 6min with constant current, and limiting voltage to 3.65V;
step 9: discharging at 3C constant current for 10s, and limiting voltage to 2.0V;
step 10: standing for 10s;
and 11, step 11: charging with 0.33C constant current and constant voltage, stopping current at 0.05C, limiting time for 90min, and limiting voltage at 3.65V;
step 12: standing for 10min;
step 13: discharging at constant current of 0.33C, limiting time for 200min, and limiting voltage to 2.0V;
step 14: standing for 10min;
step 15: charging at constant current of 0.33C, cutting off current of 0.01C, limiting time for 30min, and limiting voltage for 3.3V;
step 16: standing for 3min;
step 17: and finishing the capacity grading.
Has the advantages that: in the invention, the concentration polarization and the electrochemical polarization are relieved by introducing a negative pulse method into the gap of step charging, and the ohmic polarization is eliminated after the negative pulse; by the method, the current of the step charging can be increased, and the charging efficiency in the formation or grading stage is improved.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
As shown in the attached figure 1, the negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery comprises a formation process and a capacity grading process, wherein in the formation process or the capacity grading process:
placing the battery cell in a corresponding formation temperature or capacity grading temperature environment, dividing a charging process into a plurality of charging periods, wherein in two adjacent charging periods, the charging current value changes in a stepped manner; namely, a stepped charging method is adopted to perform multi-periodic charging and discharging on the battery cell to form a negative pulse charging mode, and the current values of two adjacent charging periods are different, so that the phenomena of ohmic polarization, concentration polarization and electrochemical polarization are reduced.
Each charging cycle comprises a charging stage, a discharging stage and a resting stage, wherein the charging voltage limiting of the charging stage is the same in a plurality of charging cycles, the discharging voltage limiting of the discharging stage is the same, the charging stage enters the discharging stage after reaching the charging voltage limiting, and the resting stage enters after reaching the discharging voltage limiting;
in the same charging cycle, the charging stage and the discharging stage are both constant-current charging or constant-current discharging, the current value of the discharging stage is greater than that of the charging stage, the discharging time of the discharging stage is shorter than that of the charging stage, and the process increases the activity of active materials between the positive electrode and the negative electrode in a mode of forming negative pulse charging and discharging through short-time rapid discharging.
In the charging process of the lithium ion battery, the current acceptance of the battery can be improved by discharging the battery to a certain degree; and then, ohmic polarization elimination, negative pulse alleviation concentration polarization and electrochemical polarization are utilized, and a step charging method is combined on the basis, so that quick charging is realized, and lithium cannot be separated out from the negative electrode.
After the polarization is eliminated in a negative pulse mode, the current for step charging can be increased, the overall charging time is shortened, and the charging efficiency in the formation and grading stages is improved.
In the formation process or the capacity grading process, the charging current values of a plurality of charging stages are increased from small to large and then from large to small, and the process that the current is increased from small to large is to increase the charging grid current, shorten the whole charging time and improve the charging efficiency of the formation and the capacity grading stages. The current is stabilized to active material in the later stage of charge and discharge.
The discharge current range of the discharge stage in the formation process is 0.5-10C, preferably 1-3C, so that the variation amplitude is reduced, and the charging stability is ensured; the discharge current range of the discharge stage in the grading process is 0.5-10C, preferably 2-5C, so that charging stability is guaranteed, and meanwhile, quick discharge is realized.
The shelf time range of the shelf stage in the formation process or the capacity grading process is 1s-5min, preferably 5s-20s, and within the time range, a more obvious effect can be achieved, and the shelf time is too long, so that the effect is not obviously increased, and the integral formation or capacity grading time is obviously increased.
The formation temperature range in the formation process is 40-50 ℃, and the chemical activity of the materials in the battery is improved, the reaction and activation processes are accelerated, and the formation efficiency can be improved by 20-50% in a high-temperature environment.
The volume separation temperature range in the volume separation procedure is 20-30 ℃, and the temperature is normal temperature environment.
The following are the experimental data for example 1 and prior art comparative example 1 using this protocol:
example 1:
the battery cell is 32135-15Ah in model, and the lithium iron phosphate on the positive electrode, the graphite on the negative electrode and the cylindrical winding structure are adopted. After the battery is filled with liquid and placed aside, the formation and the capacity grading are carried out according to the following steps. Testing the capacity-grading discharge capacity, the first efficiency, self-discharging after standing for 30 days at normal temperature, disassembling to confirm whether lithium is separated out, and detecting the cycle performance at normal temperature, and further detecting whether the potential of the negative electrode to lithium is greater than 0V during charging.
The formation process comprises the following steps:
step (ii) of Temperature of Working steps
Step 1 45±3℃ Standing for 3min
Step 2 45±3℃ Charging at 0.05C under constant current, limiting time for 120min, and limiting voltage for 3.65V;
step 3 45±3℃ Standing for 10min
Step 4 45±3℃ 0.2C constant current charging for 22min, and 3.65V voltage limiting
Step 5 45±3℃ Constant current discharge at 1.5C for 10s, and voltage limitation of 2.0V
Step 6 45±3℃ Lay aside for 10s
Step 7 45±3℃ 0.5C constant current charging for 12min, and 3.65V voltage limiting
Step 8 45±3℃ 2C constant current discharge for 10s, and voltage limitation of 2.0V
Step 9 45±3℃ Lay aside for 10s
Step 10 45±3℃ 1.0C constant current charging for 9min, and voltage limiting for 3.65V
Step 11 45±3℃ 2.5C constant current discharge for 10s, and voltage limitation of 2.0V
Step 12 45±3℃ Lay aside for 10s
Step 13 45±3℃ 0.5C constant current charging for 12min, and 3.65V voltage limiting
Step 14 45±3℃ 2C constant current discharge for 10s, voltage limitation of 2.0V
Step 15 45±3℃ Standing for 10min
Step 16 25±3℃ End of formation
The total time of the assembly: 199min10s, formation capacity about 52% SOC;
the grading process comprises the following steps:
Figure BDA0003784181800000051
Figure BDA0003784181800000061
total volume grading time: 368min;
comparative example 1: the battery cell is 32135-15Ah in model, and the lithium iron phosphate on the positive electrode, the graphite on the negative electrode and the cylindrical winding structure are adopted. After the battery is filled with liquid and placed aside, the formation and the capacity grading are carried out according to the following steps. Testing the capacity-grading discharge capacity, the first efficiency, self-discharging after standing for 30 days at normal temperature, disassembling to confirm whether lithium is separated out, and detecting the cycle performance at normal temperature, and further detecting whether the potential of the negative electrode to lithium is greater than 0V during charging.
The formation process comprises the following steps:
step (ii) of Temperature of Working steps
Step 1 45±3℃ Standing for 3min
Step 2 45±3℃ Charging at 0.05 ℃ under constant current, limiting time for 120min and limiting voltage for 3.65V;
step 3 45±3℃ Standing for 10min
Step 4 45±3℃ Constant current charging at 0.10 deg.C, time limit 240min, and voltage limit 3.65V
Step 5 45±3℃ Standing for 10min
Step 6 25±3℃ End of formation
The total time of the assembly: 383min;
the capacity grading process comprises the following steps:
step (ii) of Temperature of Working steps
Step 1 25±3℃ Standing for 3min
Step 2 25±3℃ Charging at constant current and constant voltage of 0.33C, stopping current of 0.05C, limiting time for 240min, and limiting voltage to 3.65V;
step 3 25±3℃ Standing for 10min
Step 4 25±3℃ Constant current discharging at 0.33 deg.C, time limit of 200min, and voltage limit of 2.0V
Step 5 25±3℃ Standing for 10min
Step 6 25±3℃ Charging at constant current of 0.33C, stopping current of 0.01C, limiting time for 30min, and limiting voltage for 3.3V;
step 7 25±3℃ Standing for 3min
Step 8 25±3℃ End of capacity grading
Total volume grading time: 496min;
the data for example 1 and comparative example 1 are compared as follows:
Figure BDA0003784181800000071
as can be seen from the table, the formation and capacity separation time of example 1 is shorter and the charging efficiency is higher than that of comparative example 1. Without significant difference in electrical property data compared to the same. The pole piece after disassembly and capacity grading has no lithium separation, and the three-electrode test also shows that the potential of the negative electrode to lithium is more than 0V.
In conclusion, the formation and capacity grading method is used on the cylindrical lithium iron phosphate battery, the concentration polarization and the electrochemical polarization are relieved by introducing a negative pulse method, and the ohmic polarization is eliminated after the negative pulse; this method can improve the charging efficiency in the formation or capacity grading stage.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.

Claims (7)

1. A negative pulse formation capacity grading method for a lithium iron phosphate cylindrical battery is characterized by comprising the following steps: the method comprises a formation process and a capacity grading process, wherein in the formation process or the capacity grading process:
placing the battery cell in a corresponding formation temperature or capacity grading temperature environment, dividing a charging process into a plurality of charging periods, wherein in two adjacent charging periods, the charging current value changes in a stepped manner;
each charging cycle comprises a charging stage, a discharging stage and a resting stage, wherein the charging voltage limiting of the charging stage is the same in a plurality of charging cycles, the discharging voltage limiting of the discharging stage is the same, the charging stage enters the discharging stage after reaching the charging voltage limiting, and the resting stage enters after reaching the discharging voltage limiting;
in the same charging cycle, the charging stage and the discharging stage are both constant current charging or constant current discharging, the current value of the discharging stage is greater than that of the charging stage, and the discharging time of the discharging stage is less than that of the charging stage.
2. The negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery according to claim 1, characterized by comprising the following steps: in the formation process or the capacity grading process, the charging current values of a plurality of charging stages are firstly from small to large and then from large to small.
3. The negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery according to claim 1, characterized in that: the discharge current range of the discharge stage in the formation procedure is 1C-3C; the discharge current range of the discharge stage in the capacity grading procedure is 2C-5C.
4. The negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery according to claim 1, characterized in that: the shelf time range of the shelf stage in the formation process or the capacity grading process is 5s-20s.
5. The negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery according to claim 1, characterized in that: the formation temperature range in the formation procedure is 40-50 ℃; the volume separation temperature range in the volume separation procedure is 20-30 ℃.
6. The negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery according to claim 1, characterized in that: the chemical synthesis process comprises the following steps:
step 1: standing for 3min before charging;
step 2: charging at constant current of 0.05C, time limiting for 120min, and voltage limiting for 3.65V;
and 3, step 3: standing for 10min;
and 4, step 4: charging at 0.2C for 22min, and limiting voltage to 3.65V;
and 5, step 5: discharging at 1.5C constant current for 10s, and limiting voltage to 2.0V;
and 6, a step of: standing for 10s;
and 7, step 7: charging at 0.5C for 12min, and limiting voltage to 3.65V;
and 8, step 8: discharging at 2C constant current for 10s, and limiting voltage to 2.0V;
step 9: standing for 10s;
step 10: charging at 1.0C for 9min, and limiting voltage to 3.65V;
and 11, step 11: discharging at 2.5C constant current for 10s, and limiting voltage to 2.0V;
step 12: standing for 10s;
step 13: charging at 0.5C for 12min, and limiting voltage to 3.65V;
step 14: discharging at 2C constant current for 10s, and limiting voltage to 2.0V;
step 15: standing for 10min;
step 16: and finishing the formation.
7. The negative pulse formation and capacity grading method for the lithium iron phosphate cylindrical battery according to claim 1, characterized by comprising the following steps: in the capacity grading process, the method comprises the following steps:
step 1: standing for 3min before charging;
step 2: charging at 1.5C for 6min, and limiting voltage to 3.65V;
and 3, step 3: discharging at 3C constant current for 10s, and limiting voltage to 2.0V;
and 4, step 4: standing for 10s;
and 5, step 5: charging at 1C for 9min at constant current, and limiting voltage to 3.65V;
and 6, step 6: discharging at 3C constant current for 10s, and limiting voltage to 2.0V;
and 7, step 7: standing for 10s;
and 8, step 8: charging at 0.5C for 6min, and limiting voltage to 3.65V;
step 9: discharging for 10s at a constant current of 3C, and limiting the voltage to 2.0V;
step 10: standing for 10s;
and 11, step 11: charging with 0.33C constant current and constant voltage, stopping current at 0.05C, limiting time for 90min, and limiting voltage at 3.65V;
step 12: standing for 10min;
step 13: discharging at constant current of 0.33C, limiting time for 200min, and limiting voltage to 2.0V;
step 14: standing for 10min;
step 15: charging at constant current of 0.33C, cutting off current of 0.01C, limiting time for 30min, and limiting voltage for 3.3V;
step 16: standing for 3min;
step 17: and finishing the capacity grading.
CN202210937480.9A 2022-08-05 2022-08-05 Negative pulse formation and capacity grading method for lithium iron phosphate cylindrical battery Pending CN115207500A (en)

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