CN116718932A - Method for testing critical lithium-ion battery lithium-ion current - Google Patents
Method for testing critical lithium-ion battery lithium-ion current Download PDFInfo
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- CN116718932A CN116718932A CN202310600794.4A CN202310600794A CN116718932A CN 116718932 A CN116718932 A CN 116718932A CN 202310600794 A CN202310600794 A CN 202310600794A CN 116718932 A CN116718932 A CN 116718932A
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- 238000012360 testing method Methods 0.000 title claims abstract description 39
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 36
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000007599 discharging Methods 0.000 claims description 31
- 238000007600 charging Methods 0.000 claims description 21
- 230000003247 decreasing effect Effects 0.000 claims description 9
- 238000010277 constant-current charging Methods 0.000 claims description 7
- 230000001351 cycling effect Effects 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 abstract description 19
- 238000001514 detection method Methods 0.000 abstract description 5
- 238000009825 accumulation Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/385—Arrangements for measuring battery or accumulator variables
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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 invention relates to the technical field of lithium ion batteries, and discloses a method for testing critical lithium-ion battery current. The detection method provided by the invention can characterize the accumulation of trace lithium precipitation in time in the single charge and discharge process of the battery without disassembling the battery, analyze the lithium precipitation condition of the battery, has short experimental period, low requirements on equipment and operating environment, can utilize samples for multiple times, and has low experimental cost.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a method for testing critical lithium-ion battery lithium-ion current.
Background
When the lithium ion battery is subjected to working conditions such as overcharging, low-temperature charging, quick charging and the like, lithium ions can reach a lithium precipitation potential so as to generate lithium precipitation on the surface of the negative electrode, the cycle performance of the lithium ion battery is affected, and even serious potential safety hazards can be generated under serious conditions.
In order to avoid the occurrence of the phenomenon of negative electrode lithium precipitation, the detection of the negative electrode lithium precipitation becomes particularly important, but the sealing structure of the lithium ion battery makes the detection of the negative electrode lithium precipitation not easy.
At present, the most commonly used external characteristic method is to utilize data such as charge and discharge in the use process of a battery, and judge whether lithium precipitation occurs in the battery through data processing and analysis, including a cyclic voltammetry and a differential processing method of a charge and discharge curve. However, most of the existing external characteristic methods are based on single cycle under specific working conditions, the sensitivity of lithium precipitation detection is low, and a large amount of precipitated lithium metal can be detected under severe working conditions; under a certain milder working condition, when less lithium metal is precipitated on the surface of the single charge-discharge negative electrode, the existing external characteristic method is difficult to detect whether lithium precipitation occurs.
It is therefore necessary to propose a new external characteristic method for detecting lithium precipitation inside a battery.
Disclosure of Invention
The invention aims to provide a method for testing critical lithium-ion battery current, which is characterized in that continuous charge-discharge cyclic test is carried out with preset current in a preset SOC level and a fixed voltage window, trace lithium precipitation in a single charge-discharge process is accumulated in time, whether lithium precipitation occurs or not is determined through open-circuit voltage, internal resistance and capacity change, and then the critical lithium-ion battery current is determined.
The technical scheme adopted for solving the technical problems is as follows:
a method for testing critical lithium-ion battery current comprises the following steps:
s1, performing capacity calibration for 3-5 times according to standard multiplying power at test temperature, then discharging to 50% of SOC after full charge by adopting the standard multiplying power, pulse testing discharge DCR, and recording discharge capacity Q 0 Discharge DCR and open circuit voltage OCV；
S2, charging to the upper limit cutoff voltage V by using a preset current constant current max Record charge capacity Q 1 After standing, discharging again with a preset current constant current, the discharge capacity is deltaq= (Q) 0 +Q 1 ) Cut-off at/2, the discharge cut-off voltage is denoted as V min Then standing for a period of time;
s3, charging to the upper limit cutoff voltage V by using a preset current constant current max Then discharge with constant current of preset current, the discharge capacity is deltaq= (Q) 0 +Q 1 ) Stopping at/2, and stopping discharge at a voltage of V min Cycling for N times, wherein N is a natural number greater than or equal to 100;
s4, standing for at least 120min, and recording open circuit voltage OCV;
s5, fully charging the standard multiplying power, standing, discharging the standard multiplying power, and recording the discharge capacity Q x Then standing for a period of time, wherein x is a natural number;
s6, fully charging the battery with standard multiplying power, standing, and then discharging the battery with a discharge capacity Q x Calculating, discharging to 50% SOC, pulse testing the discharge DCR, recording the discharge DCR and the open circuit voltage OCV, and then standing for a period of time again;
s7, circulating the steps S3-S6 for a plurality of times;
s8, drawing a cycle number-OCV curve according to the data obtained in the steps, comparing the decreasing amplitude of OCV with the increasing amplitude of discharging DCR, if the decreasing amplitude is larger than a first preset threshold value, and meanwhile, the increasing amplitude of discharging DCR is larger than a second preset threshold value, then lithium can be separated from the corresponding lithium ion battery with the SOC level at the preset current constant current charge and discharge, otherwise, lithium can not be separated;
s9, if lithium is separated, reducing the preset current value, otherwise, increasing the preset current value, and repeating the steps until the corresponding preset current value X is found when the lithium is not separated max I.e. X max C is the critical lithium current of the lithium ion battery at this SOC level.
Preferably, the preset current is 3.5-4.5 ℃.
Preferably, the first preset threshold in the step S8 is 15% -30%.
Preferably, the second preset threshold in the step S8 is 50% -100%.
Preferably, the standing time in step S2 is at least 10min.
Preferably, in the step S1 and the step S6, the condition of the pulse test discharge DCR is to discharge for 10S with a 2C current.
Preferably, the rest time in each of the step S5 and the step S6 is at least 30min.
Preferably, the number of cycles in step S7 is at least 10.
Preferably, the experimental temperature in the step S1 is 25 ℃.
Compared with the prior art, the invention has the advantages that:
1. by the charge-discharge cycles in step S2 and step S3, the accumulation of micro-lithium precipitation in the battery during single charge-discharge process over time is rapidly characterized, and the discharge capacity is set as Δq= (Q) 0 +Q 1 ) And 2, taking an average value of the charge and discharge capacity, and comparing with the method which only adopts the charge or discharge capacity, the data is more accurate.
2. The rest time in step S4 is at least 120min because the OCV is not stable yet due to insufficient rest time and the data tested are not reliable. In the invention, pulse test discharge DCR is not directly performed after the steps S2 and S3 are circulated, because the state of the battery core is changed after the steps S2 and S3 are circulated, one capacity test is required to be performed to recover the state of the battery core, and then DCR test is performed, so that the tested DCR is more reliable.
3. The detection method provided by the invention can characterize the accumulation of trace lithium precipitation in time in the single charge and discharge process of the battery without disassembling the battery, analyze the lithium precipitation condition of the battery, has short experimental period, low requirements on equipment and operating environment, can utilize samples for multiple times, and has low experimental cost.
Drawings
FIG. 1 is a graph showing the OCV of a lithium ion battery according to the present invention as a function of cycle number;
fig. 2 is a graph showing the variation of the discharge DCR of the lithium ion battery according to the present invention with the number of cycles.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown.
All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Embodiment one:
a method for testing critical lithium-ion battery current comprises the following steps:
s1, performing capacity calibration for 3-5 times according to standard multiplying power at a test temperature of 25 ℃, then fully charging by adopting the standard multiplying power, discharging to 50% of SOC, pulse testing discharge DCR, and recording discharge capacity Q 0 Discharge DCR and open circuit voltage OCV;
s2, charging to the upper limit cutoff voltage V by using a preset current constant current max Record charge capacity Q 1 After standing, discharging again with a preset current constant current, the discharge capacity is deltaq= (Q) 0 +Q 1 ) Cut-off at/2, the discharge cut-off voltage is denoted as V min Then standing for a period of time;
s3, charging to the upper limit cutoff voltage V by using a preset current constant current max Then discharge with constant current of preset current, the discharge capacity is deltaq= (Q) 0 +Q 1 ) Stopping at/2, and stopping discharge at a voltage of V min Cycling for N times, wherein N is a natural number greater than or equal to 100;
s4, standing for at least 120min, and recording open circuit voltage OCV;
s5, fully charging the standard multiplying power, standing, discharging the standard multiplying power, and recording the discharge capacity Q x Then standing for a period of time;
s6, fully charging the standard multiplying power, standing, and then placingCapacitance Q x Calculating, discharging to 50% SOC, pulse testing the discharge DCR, recording the discharge DCR and the open circuit voltage OCV, and then standing for a period of time again;
s7, circulating the steps S3-S6 for a plurality of times;
s8, drawing a cycle number-OCV curve according to the data obtained in the steps, comparing the decreasing amplitude of OCV with the increasing amplitude of discharge DCR, if the decreasing amplitude is larger than a first preset threshold value or the increasing amplitude of discharge DCR is larger than a second preset threshold value, the lithium ion battery with the corresponding SOC level can be separated out in the preset current constant-current charging and discharging, otherwise, the lithium is not separated out;
s9, if lithium is separated, reducing the preset current value, otherwise, increasing the preset current value, and repeating the steps until the corresponding preset current value X is found when the lithium is not separated max I.e. X max C is the critical lithium current of the lithium ion battery at this SOC level.
The preset current is 3.5-4.5 ℃, the standing time in the step S2 is at least 10min, and the standing time in the step S5 and the step S6 is at least 30min. In step S1 and step S6, the condition of the pulse test discharge DCR is to discharge for 10S with a 2C current. The first preset threshold in step S8 is 15% to 30%, the percentage being 50% to 100% relative to the initial OCV tested in step S1, and the percentage being relative to the initial DCR tested in step S1.
Embodiment two:
a method for testing critical lithium-ion battery current comprises the following steps:
s1, performing standard multiplying power at a test temperature of 25 ℃ for 3 times of capacity calibration, then discharging to 50% of SOC after full charge by adopting the standard multiplying power, testing discharge DCR (internal resistance of a battery) by 2C discharge 10S pulse, and recording discharge capacity Q0, discharge DCR and open circuit voltage OCV (terminal voltage in an open circuit state of the battery);
s2, constant-current charging with 4C preset current to upper limit cutoff voltage V max Recording the charge capacity Q1, standing for 10min, discharging again with constant current of 4C preset current, and dischargingCapacitance Δq= (Q) 0 +Q 1 ) Cut-off at/2, discharge cut-off voltage is set to V min Then standing for 10min;
s3, constant-current charging is performed to the upper limit cutoff voltage Vmax by using 4C preset current, then constant-current discharging is performed by using 4C preset current, and the discharge capacity is delta Q= (Q) 0 +Q 1 ) Stopping at/2, and stopping discharge at a voltage of V min Cycling for 100 times;
s4, standing for at least 120min, and recording open circuit voltage OCV;
s5, fully charging the standard multiplying power, standing for 30min, discharging the standard multiplying power, and recording the discharge capacity Q x Standing for 30min;
s6, fully charging the battery with standard multiplying power, standing for 30min, and then taking the discharge capacity Q x Calculating, discharging to 50% SOC, pulse testing the discharge DCR, recording the discharge DCR and the open circuit voltage OCV, and standing for 30min again;
s7, circulating the steps S3-S6 for 10 times;
and S8, drawing a cycle number-OCV curve according to the data obtained in the steps, wherein the cycle number-discharge DCR curve has a decreasing amplitude of OCV smaller than 15% of a first preset threshold value, and an increasing amplitude of discharge DCR smaller than 50% of a second preset threshold value, namely, the 50% SOC level corresponds to the 4C current without lithium precipitation.
Embodiment III:
a method for testing critical lithium-ion battery current comprises the following steps:
s1, performing standard multiplying power at a test temperature of 25 ℃ for 3 times of capacity calibration, then discharging to 50% of SOC after full charge by adopting the standard multiplying power, testing discharge DCR (internal resistance of a battery) by 2C discharge 10S pulse, and recording discharge capacity Q0, discharge DCR and open circuit voltage OCV (terminal voltage in an open circuit state of the battery);
s2, constant-current charging with 4.5C preset current to upper limit cutoff voltage V max After the charge capacity Q1 is recorded and the mixture is kept stand for 10min, the mixture is discharged again at a constant current of 4.5C with a discharge capacity of DeltaQ= (Q) 0 +Q 1 ) Cut-off at/2, discharge cut-off voltage is set to V min Then standing for 10min;
s3, presetting with 4.5CThe current constant current is charged to the upper limit cutoff voltage Vmax, then the current constant current is discharged with 4.5C preset current, and the discharge capacity is Δq= (Q) 0 +Q 1 ) Stopping at/2, and stopping discharge at a voltage of V min Cycling for 100 times;
s4, standing for at least 120min, and recording open circuit voltage OCV;
s5, fully charging the standard multiplying power, standing for 30min, discharging the standard multiplying power, and recording the discharge capacity Q x Standing for 30min;
s6, fully charging the battery with standard multiplying power, standing for 30min, and then taking the discharge capacity Q x Calculating, discharging to 50% SOC, pulse testing the discharge DCR, recording the discharge DCR and the open circuit voltage OCV, and standing for 30min again;
s7, circulating the steps S3-S6 for 10 times;
and S8, drawing a cycle number-OCV curve according to the data obtained in the steps, wherein the cycle number-discharge DCR curve has a decreasing amplitude of OCV smaller than 15% of the first preset threshold value, and an increasing amplitude of discharge DCR smaller than 50% of the second preset threshold value, namely, the 50% SOC level corresponds to 4.5C current without lithium precipitation.
Embodiment four:
a method for testing critical lithium-ion battery current comprises the following steps:
s1, performing standard multiplying power at a test temperature of 25 ℃ for 3 times of capacity calibration, then discharging to 50% of SOC after full charge by adopting the standard multiplying power, testing discharge DCR (internal resistance of a battery) by 2C discharge 10S pulse, and recording discharge capacity Q0, discharge DCR and open circuit voltage OCV (terminal voltage in an open circuit state of the battery);
s2, constant-current charging with 5C preset current to upper limit cutoff voltage V max After the charge capacity Q1 is recorded and the mixture is kept stand for 10min, the mixture is discharged again at a constant current of 5C preset current, and the discharge capacity is DeltaQ= (Q) 0 +Q 1 ) Cut-off at/2, discharge cut-off voltage is set to V min Then standing for 10min;
s3, charging to the upper limit cutoff voltage Vmax by using 5C preset current constant current, and discharging by using 5C preset current constant current, wherein the discharge capacity is delta Q= (Q) 0 +Q 1 ) Stopping at/2, and stopping discharge at a voltage of V min Cycling for 100 times;
s4, standing for at least 120min, and recording open circuit voltage OCV;
s5, fully charging the standard multiplying power, standing for 30min, discharging the standard multiplying power, and recording the discharge capacity Q x Standing for 30min;
s6, fully charging the battery with standard multiplying power, standing for 30min, and then taking the discharge capacity Q x Calculating, discharging to 50% SOC, pulse testing the discharge DCR, recording the discharge DCR and the open circuit voltage OCV, and standing for 30min again;
s7, circulating the steps S3-S6 for 10 times;
and S8, drawing a cycle number-OCV curve according to the data obtained in the steps, wherein the cycle number-discharge DCR curve has a decreasing amplitude of OCV greater than 15% of a first preset threshold value, and an increasing amplitude of discharge DCR greater than 50% of a second preset threshold value, namely, a 50% SOC level corresponds to 5C current lithium precipitation.
As is evident from the curves of fig. 1 to 2, the lithium evolution can be clearly reflected when the cycle number is increased to 1000 times or more.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. The method for testing the critical lithium-ion battery lithium-ion current is characterized by comprising the following steps of:
s1, performing capacity calibration for 3-5 times according to standard multiplying power at test temperature, then discharging to 50% SOC after full charge by adopting the standard multiplying power, pulse testing discharge DCR, and recording discharge capacity Q 0 Discharge DCR and open circuit voltage OCV;
s2, constant current charging with preset currentUpper limit cut-off voltage V max Record charge capacity Q 1 After standing, discharging again with a preset current constant current, the discharge capacity is deltaq= (Q) 0 +Q 1 ) Cut-off at/2, the discharge cut-off voltage is denoted as V min Then standing for a period of time;
s3, charging to the upper limit cutoff voltage V by using a preset current constant current max Then discharge with constant current of preset current, the discharge capacity is deltaq= (Q) 0 +Q 1 ) Stopping at/2, and stopping discharge at a voltage of V min Cycling for N times, wherein N is a natural number greater than or equal to 100;
s4, standing for at least 120min, and recording open circuit voltage OCV;
s5, fully charging the standard multiplying power, standing, discharging the standard multiplying power, and recording the discharge capacity Q x Then standing for a period of time, wherein x is a natural number;
s6, fully charging the battery with standard multiplying power, standing, and then discharging the battery with a discharge capacity Q x Calculating, discharging to 50% SOC, pulse testing the discharge DCR, recording the discharge DCR and the open circuit voltage OCV, and then standing for a period of time again;
s7, circulating the steps S3-S6 for a plurality of times;
s8, drawing a cycle number-OCV curve according to the data obtained in the steps, comparing the decreasing amplitude of OCV with the increasing amplitude of discharging DCR, if the decreasing amplitude is larger than a first preset threshold value, and meanwhile, the increasing amplitude of discharging DCR is larger than a second preset threshold value, then lithium can be separated from the corresponding lithium ion battery with the SOC level at the preset current constant current charge and discharge, otherwise, lithium can not be separated;
s9, if lithium is separated, reducing the preset current value, otherwise, increasing the preset current value, and repeating the steps until the corresponding preset current value X is found when the lithium is not separated max I.e. X max C is the critical lithium current of the lithium ion battery at this SOC level.
2. The method for testing critical lithium-ion battery current according to claim 1, wherein the preset current is 3.5-4.5 ℃.
3. The method for testing critical lithium-ion battery current according to claim 2, wherein the first preset threshold in step S8 is 15% -30%.
4. The method for testing critical lithium-ion battery current according to claim 2, wherein the second preset threshold in step S8 is 50% -100%.
5. The method according to claim 2, wherein the rest time of each time in the step S2 is at least 10min.
6. The method according to claim 2, wherein in the step S1 and the step S6, the condition of pulse test discharge DCR is that 2C current is used for 10S.
7. The method according to claim 2, wherein the rest time of each of the steps S5 and S6 is at least 30min.
8. The method according to claim 1, wherein the number of cycles in step S7 is at least 10.
9. The method according to claim 1, wherein the experimental temperature in the step S1 is 25 ℃.
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| CN118625158A (en) * | 2024-08-09 | 2024-09-10 | 宁德时代新能源科技股份有限公司 | Lithium precipitation detection method, lithium precipitation detection device, electronic equipment, storage medium and product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118625158A (en) * | 2024-08-09 | 2024-09-10 | 宁德时代新能源科技股份有限公司 | Lithium precipitation detection method, lithium precipitation detection device, electronic equipment, storage medium and product |
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