CN115508721A - Lithium analysis detection method of lithium ion battery - Google Patents

Lithium analysis detection method of lithium ion battery Download PDF

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CN115508721A
CN115508721A CN202211100447.7A CN202211100447A CN115508721A CN 115508721 A CN115508721 A CN 115508721A CN 202211100447 A CN202211100447 A CN 202211100447A CN 115508721 A CN115508721 A CN 115508721A
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lithium
lithium ion
ion battery
battery
eis
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史金涛
周培俊
岳仍利
邓超
丁美超
刘立振
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Tianjin Juyuan New Energy Technology Co ltd
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Tianjin Lishen Battery JSCL
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    • G01—MEASURING; TESTING
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    • G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
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Abstract

The invention belongs to the field of lithium battery testing, and particularly relates to a lithium analysis detection method for a lithium ion battery. The method comprises the following steps: performing DRT analysis on EIS data; extracting relaxation time of different processes by a deconvolution technology; and analyzing or mapping and observing the obtained DRT data, comparing the peak intensity of the characteristic peak of the lithium ion in the frequency range of 30Hz-1000Hz or integrating the relaxation process to obtain the peak area, judging whether to analyze lithium and the amount of the lithium, and detecting the lithium analysis degree according to the characteristic peak of the lithium metal in the DRT result by adopting the method.

Description

Lithium analysis detection method of lithium ion battery
Technical Field
The invention belongs to the field of lithium battery testing, and particularly relates to a lithium analysis detection method of a lithium ion battery.
Background
In the long-term use process of the lithium ion battery, under the condition of extreme conditions such as high-current charging and low-temperature charging and aging, the lithium insertion dynamic conditions of the negative electrode are remarkably reduced, so that lithium metal is precipitated (lithium precipitation) on the surface of the negative electrode. The precipitated lithium metal has strong reactivity and reacts with the electrolyte, consuming the electrolyte and further deteriorating the kinetic conditions in the battery, resulting in more lithium precipitation. A part of lithium metal precipitated at the negative electrode is re-inserted into the positive electrode during discharge; another portion will be converted to "dead lithium" causing an irreversible loss of battery capacity. Meanwhile, the precipitated lithium metal may cause internal short circuit of the lithium ion battery, and cause catastrophic consequences such as combustion and explosion.
How to accurately detect when and how much lithium is extracted from a negative electrode has been a very challenging task in the industry. In order to research the lithium analysis behavior of the negative electrode, a plurality of methods are provided, which are mainly divided into two categories, one is a nondestructive testing method, including a coulombic efficiency method, a voltage relaxation method, a three-electrode method, a dQ/dV extreme value method and the like; one is a destructive detection method, i.e. the battery is disassembled and then subjected to pole piece analysis, including direct observation, isopropanol reaction, differential thermal analysis, titration gas chromatography, solid nuclear magnetic method (NMR), neutron diffraction and the like. Some of the current methods require the construction of a battery with a special structure, such as a three-electrode method; some tests need to be carried out for a long time, such as a coulombic efficiency method, a voltage relaxation method and a dQ/dV extreme value method; or require destructive disassembly of the cell such as destructive testing. The existing method is difficult to realize the quantitative detection of the lithium analysis amount, and when the lithium analysis detection is carried out by a loss detection method, the battery needs to be disassembled, and because lithium metal is very active and is easy to react with water in the air, the error in the detection is caused. The existing nondestructive detection has difficulty in quantitative detection of the lithium analysis amount, and is not high in sensitivity to a small amount of lithium analysis particularly. In summary, the existing lithium analysis detection technology has the following problems: the online real-time test cannot be carried out, the detection time is long, the lithium analysis amount is difficult to quantify, and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a lithium analysis detection method of a lithium ion battery.
In order to achieve the purpose, the invention adopts the technical scheme that:
a lithium analysis detection method of a lithium ion battery is characterized by comprising the following steps:
selecting a fresh lithium ion battery, and performing charge-discharge circulation on the fresh lithium ion battery, wherein the charge-discharge multiplying power is less than the maximum using multiplying power of the battery, and the circulation is performed for 3-5 times;
(ii) charging the selected fresh lithium ion battery to a state of charge SOC =100%; standing for more than 2 hours;
performing Electrochemical Impedance Spectroscopy (EIS) test, namely performing EIS test on the lithium ion battery in the step (II); and (3) testing conditions: the battery is placed in a constant temperature box for testing, the constant temperature is 20-45 ℃, the constant potential or constant current measuring method is adopted, the amplitude of the constant potential or constant current is adjusted, the current applied to the lithium ion battery is 5-20% of the common current, and the frequency range is as follows: 1mHz-10KHz, and performing EIS test;
(IV) performing Kramers-Kronig conversion on the EIS data tested in the step (III), checking the rationality of the EIS test result, and calculating the test error of the impedance; in the step (four), the test errors of the calculated impedance are all less than or equal to 10 percent; the test error comprises a real part error and an imaginary part error; if the error is more than 10 percent, adjusting the constant potential or constant current measuring method in the step (III) until the error is less than or equal to 10 percent; the specific detection principle is as follows:
Figure BDA0003840126610000021
Figure BDA0003840126610000022
Figure BDA0003840126610000023
Figure BDA0003840126610000024
wherein, Z j (x) Is a resistance of testReal part of the resistance, Z j (ω) is the imaginary impedance of the test,
Figure BDA0003840126610000025
is the real part of the impedance calculated,
Figure BDA0003840126610000026
is the imaginary part of the calculated impedance, Δ r (ω) is the real part error, Δ j (ω) is the imaginary error and x, ω is the frequency.
It should be noted that the formula given in the present application is a principle part, and those skilled in the art can realize the judgment of the test error through the self-contained software of the EIS test;
(V) performing DRT analysis on the EIS data obtained in the step (III); the DRT corresponds to characteristic time constants of different battery charging and discharging processes and is used for analyzing a polarization impedance rule of an electrochemical system; extracting relaxation time of different processes by a deconvolution technology;
to obtain the DRT of the battery, the total impedance Z (ω) is expressed as follows:
Figure BDA0003840126610000027
where Ro is the ohmic impedance and γ (ln τ) is the relaxation time distribution function; τ is the relaxation characteristic time, j is the complex unit, and ω is the frequency. Solving gamma (ln tau) corresponding to different relaxation time tau to obtain the relaxation time distribution of EIS data;
sixthly, analyzing or drawing and observing the DRT data obtained in the step five, comparing the peak intensity of the characteristic peak of the lithium ion within the frequency range of 30Hz-1000Hz or integrating the relaxation process to obtain the peak area to judge whether to analyze lithium and the amount of the analyzed lithium, and storing the data as a reference standard for judging the analyzed lithium so as to compare lithium ion batteries to be detected with the same model;
(VII) selecting a battery with the same type as that in the step (1), which is analyzed with lithium, a lithium ion battery to be detected or a fresh battery, and adopting a current which is 0.5-2 times of the allowable use rate of the battery to carry out charge-discharge circulation on the fresh battery for more than 5 times, then charging the lithium ion battery which is possibly analyzed with lithium to SOC =100%, carrying out the operation of the step (three) -the step (six), then comparing the gamma (ln tau) peak intensity or the integral peak area obtained by the fresh battery and the lithium ion battery which is possibly analyzed through the step (six), and comparing the peak intensity or the integral peak area of the lithium metal characteristic peak of the lithium ion battery which is possibly analyzed with the peak area of the lithium metal characteristic of the fresh lithium ion battery to identify whether to analyze with lithium;
respectively subtracting the SOC of the battery with the lithium analysis from the lithium analysis-free battery to represent the lithium analysis amount; and (3) mapping and analyzing by taking the peak intensity or the integral peak area of the characteristic peak as a vertical coordinate and the lithium analysis amount as a horizontal coordinate, wherein the lithium analysis amount can be obtained by testing the peak intensity or the integral peak area of the characteristic peak before the lithium analysis amount is lower than the inflection value. .
Preferably, in the step (one), the cycle number is 3, and the charge-discharge multiplying power is 0.5C.
Preferably, in the step (II), the charging rate is 0.5C, and the standing time is 2-72 hours.
Preferably, the lithium ion battery in the step (iii) is subjected to an off-line EIS test, where off-line refers to performing an EIS test on the lithium ion battery at an electrochemical workstation, and on-line refers to performing an EIS test on a lithium ion battery-using device.
Preferably, the frequency range of the off-line EIS test is: 10mHz-100KHz; the frequency range of the online EIS test is: 1Hz-10000Hz;
preferably, the constant temperature in the step (III) is 20-25 ℃.
Preferably, the frequency range of the characteristic peak of the lithium metal precipitated on the surface of the negative electrode in the step (six) is 30-500Hz; the peak intensity is used to detect the amount of lithium analyzed.
Compared with the prior art, the invention has the beneficial effects that:
in the process of charging and discharging a lithium ion battery, a plurality of physical processes are involved: electron conductance, ionic liquid phase transmission, interface reaction, ionic solid phase diffusion and other dynamic processes. The most common method for analyzing these processes at present is Electrochemical Impedance Spectroscopy (EIS), which has the advantages of simplicity, no damage, rapidness, and capability of characterizing the reaction kinetics and the transfer phenomenon of an electrochemical system, and analyzing the microstructure characteristics and the interface characteristics in the system. The traditional EIS analysis method, namely equivalent circuit modeling, cannot analyze or distinguish relaxation processes in an overlapped frequency range in an electrochemical impedance spectrum characteristic peak, and cannot effectively identify each dynamic process in the charging and discharging processes of a lithium ion battery.
Therefore, considering that a lithium ion battery system is analyzed by adopting a Relaxation time Distribution (DRT) technique, the DRT technique can analyze an overlapped Relaxation process into a series of local processes, so that changes in EIS data can be analyzed. In the charging process of the lithium ion battery, if lithium metal is precipitated on the surface of the negative electrode, the relaxation time distribution and the characteristic peak of the lithium metal precipitation and the corresponding frequency range of the lithium metal precipitation can be presented in an EIS test. In the DRT result, different characteristic peaks are used for distinguishing different dynamic processes in different lithium ion battery charging and discharging processes, the peak intensity of the characteristic peaks and the integral area of the characteristic peaks represent impedance characteristics of a certain dynamic process, and therefore the degree of lithium analysis can be detected according to the characteristic peaks of lithium metal in the DRT result.
Drawings
FIG. 1 is a flow chart of lithium ion battery lithium analysis detection;
FIG. 2 EIS results of lithium ion batteries charged to different voltages;
FIG. 3 shows DRT results when the lithium ion battery is charged to different voltages;
FIG. 4 shows the lithium precipitation of the negative electrode of the disassembled lithium ion battery with different voltages;
FIG. 5 characteristic peak intensities for different lithium deposition amounts.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
The embodiment provides a lithium analysis detection method of a lithium ion battery. In order to verify the effectiveness of the detection method, a battery with lithium precipitation needs to be detected, so a special lithium ion battery with N/P =0.7 (N/P is more than or equal to 1 in a normal battery) is designed, the positive electrode is made of a ternary material, the negative electrode is made of graphite, the battery is circular, and the capacity is 2.5Ah. The battery corresponds to a state of charge SOC =100% when the voltage is charged to 3.9V (state of charge SOC =100% at 4.2V for a normal battery), SOC =110% for a voltage of 4.0V, SOC =122% for a voltage of 4.1V, and SOC =137% for a voltage of 4.2V. Therefore, the lithium analysis amount can be quantitatively judged according to the battery voltage. After the special lithium ion battery is prepared, the detection of lithium analysis is carried out, and the specific steps are as follows:
selecting four fresh lithium ion batteries, performing charge-discharge circulation, wherein the charge-discharge multiplying power is 0.5C, the charge-discharge cutoff voltage is 3.9V and 2.5V respectively, and circulating for 3 times; then one of the lithium ion batteries is charged to 3.9V, the state of charge (SOC = 100%) is obtained, and the lithium ion batteries are kept still for 6 hours;
(II) Electrochemical Impedance Spectroscopy (EIS) testing, namely performing off-line EIS testing on the lithium ion battery in the step (I); and (3) testing conditions: the cell is placed in a constant temperature box for testing, the constant temperature is 20 ℃, a constant potential method is adopted, and the frequency range is as follows: carrying out EIS test at 10mHz-100KHz;
(III) performing Kramers-Kronig conversion on the EIS data tested in the step (II), checking the rationality of an EIS test result, and calculating the test error of the impedance; in the step (IV), the test errors of the calculated impedance are less than or equal to 10 percent; the test error comprises a real part error and an imaginary part error; if the error is more than 10 percent, adjusting the constant potential or constant current measuring method in the step (III) until the error is less than or equal to 10 percent; the specific detection principle is as follows:
Figure BDA0003840126610000051
Figure BDA0003840126610000052
Figure BDA0003840126610000053
Figure BDA0003840126610000054
wherein Z is j (x) Is the real part of the impedance of the test, Z j (ω) is the imaginary impedance of the test,
Figure BDA0003840126610000055
is the real part of the impedance calculated,
Figure BDA0003840126610000056
is the calculated imaginary impedance, Δ r (ω) is the real part error, Δ j (ω) is the imaginary error, and x, ω is the frequency.
It should be noted that the formula given in the present application is a principle part, and those skilled in the art can realize the judgment of the test error through the self-contained software of the EIS test;
fourthly, performing DRT analysis on the EIS data obtained in the second step; different relaxation time distributions in the DRT correspond to characteristic time constants of different dynamic processes in the battery charging process, and are used for analyzing the polarization impedance rule of an electrochemical system and characterizing the lithium metal precipitation characteristics.
The relaxation times of the different processes are extracted by deconvolution techniques. To obtain the DRT of the battery, the total impedance Z (ω) is expressed as follows:
Figure BDA0003840126610000057
where Ro is the ohmic impedance, γ (ln τ) is the relaxation time distribution function, τ is the relaxation characteristic time, j is the complex unit, and ω is the angular frequency. Solving gamma (ln tau) corresponding to different relaxation time tau to obtain the relaxation time distribution of EIS data;
and fifthly, analyzing or drawing and observing the DRT data obtained in the step four, comparing the characteristic peak intensity or the integral peak area of the lithium ions within the frequency range of 30Hz-500Hz to judge whether lithium is separated and the amount of the separated lithium, and storing the data serving as a reference standard for judging the separated lithium so as to compare the data with the lithium ion batteries of the same type.
Sixthly, selecting other three lithium ion batteries, then respectively charging the batteries to 4.0V, 4.1V and 4.2V, and then carrying out EIS test and DRT analysis, namely the steps (two) - (four);
the EIS results, i.e. DRT results, of the four cells are shown in FIGS. 2 and 3.
Seventhly, four lithium ion batteries are disassembled, and when the voltage is charged to 3.9V, the surface of the negative electrode is golden yellow, and no lithium precipitation occurs
FIG. 4 shows the lithium precipitation of the negative electrode of the disassembled lithium ion battery with different voltages; as can be seen from the figure, when the voltage was charged to 4.0V, silver-white lithium metal had been clearly seen to precipitate; when the voltage was charged to 4.1 and 4.2V, a large amount of lithium was precipitated. The disassembly result shows that the higher the charging voltage is, the more the amount of lithium metal precipitation is, and the more the degree of lithium precipitation is.
In connection with the DRT results in FIG. 3, the characteristic peak in the frequency range of 30-500Hz is the characteristic peak of lithium metal. The higher the conductivity of lithium metal, the more lithium metal is precipitated, the lower the impedance, and therefore the lower the peak intensity of the characteristic peak of lithium metal, which is consistent with the disassembly result.
The differences between the SOC of the three lithium analysis-occurring batteries and the SOC of the lithium analysis-not-occurring batteries are respectively made to represent the lithium analysis amount, the characteristic peak is taken as the ordinate, the lithium analysis amount is taken as the abscissa, and the analysis is carried out by plotting, as shown in FIG. 5. It can be seen from the graph that, when the amount of lithium deposition is less than 0.22, the intensity variation of the characteristic peak shows better linear variation, and the amount of lithium deposition can be obtained by testing the obtained intensity of the characteristic peak; when the amount of lithium deposition exceeds 0.22, the slope of change of the characteristic peak decreases, and at this time, lithium metal is completely covered on the surface of the negative electrode, indicating that the decrease in resistance due to lithium metal deposition is not significant. Due to the difference of the lithium ion electrochemical system, the numerical value of the lithium analysis amount shown in fig. 5 is only suitable for quantitative lithium analysis detection of the battery of the system, and the numerical value has no universality, but the method of the invention has universality for lithium analysis detection of the lithium ion battery.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.

Claims (7)

1. A lithium analysis detection method of a lithium ion battery is characterized by comprising the following steps:
selecting a fresh lithium ion battery, and performing charge-discharge circulation on the fresh lithium ion battery, wherein the charge-discharge multiplying power is less than the maximum using multiplying power of the battery, and the circulation is performed for 3-5 times;
(ii) charging the selected fresh lithium ion battery to a state of charge SOC =100%; standing for more than 2 hours;
(III) carrying out Electrochemical Impedance Spectroscopy (EIS) test, namely carrying out EIS test on the lithium ion battery in the step (II); and (3) testing conditions: the battery is placed in a constant temperature box for testing, the constant temperature is 20-45 ℃, the constant potential or constant current measuring method is adopted, the amplitude of the constant potential or constant current is adjusted, the current applied to the lithium ion battery is 5-20% of the common current, and the frequency range is as follows: 1mHz-10KHz, and performing EIS test;
(IV) performing Kramers-Kronig conversion on the EIS data tested in the step (III), checking the rationality of an EIS test result, and calculating the test error of the impedance; the test error of the calculated impedance in the step (four) is less than or equal to 10 percent; if the error is more than 10 percent, adjusting the constant potential or constant current measuring method in the step (III) until the error is less than or equal to 10 percent;
(V) performing DRT analysis on the EIS data obtained in the step (III); the DRT corresponds to characteristic time constants of different battery charging and discharging processes and is used for analyzing a polarization impedance rule of an electrochemical system; extracting relaxation times of different processes through a deconvolution technology;
sixthly, analyzing or drawing and observing the DRT data obtained in the step five, comparing the peak intensity of a characteristic peak of lithium ions in a frequency range of 30Hz-1000Hz or integrating a relaxation process to obtain a peak area to judge whether lithium is analyzed or not and the amount of the lithium is analyzed, and storing the data as a reference standard for judging the lithium analysis so as to compare lithium ion batteries to be detected in the same model;
(VII) selecting a battery with the same type as that in the step (1), which is analyzed with lithium, a lithium ion battery to be detected or a fresh battery, and adopting a current which is 0.5-2 times of the allowable use rate of the battery to carry out charge-discharge circulation on the fresh battery for more than 5 times, then charging the lithium ion battery which is possibly analyzed with lithium to SOC =100%, carrying out the operation of the step (three) -the step (six), then comparing the gamma (ln tau) peak intensity or the integral peak area obtained by the fresh battery and the lithium ion battery which is possibly analyzed through the step (six), and comparing the peak intensity or the integral peak area of the lithium metal characteristic peak of the lithium ion battery which is possibly analyzed with the peak area of the lithium metal characteristic of the fresh lithium ion battery to identify whether to analyze with lithium;
respectively subtracting the SOC of the battery with the lithium separation from the lithium separation-free battery to represent the lithium separation amount; and (3) mapping and analyzing by taking the peak intensity or the integral peak area of the characteristic peak as a vertical coordinate and the lithium analysis amount as a horizontal coordinate, and obtaining the lithium analysis amount by testing the peak intensity or the integral peak area of the characteristic peak before the lithium analysis amount is lower than the inflection value.
2. The method for detecting lithium ion battery lithium deposition according to claim 1, wherein in step (i), the cycle number is 3 times, and the charge/discharge rate is 0.5C.
3. The method for detecting lithium ion battery lithium deposition according to claim 1, wherein in step (ii), the charging rate is 0.5C, and the standing time is 2-72 hours.
4. The lithium ion battery lithium analysis detection method according to claim 1, wherein in the step (III), the lithium ion battery is subjected to off-line EIS test on an electrochemical workstation or on-line EIS test on equipment using the lithium ion battery.
5. The lithium ion battery lithium analysis detection method according to claim 4, wherein the frequency range of the offline EIS test is: 10mHz-100KHz; the frequency range of the online EIS test is: 1Hz-10000Hz;
6. the lithium ion battery lithium analysis detection method according to claim 1, wherein the constant temperature in step (III) is 20 to 25 ℃.
7. The lithium ion battery lithium deposition detection method according to claim 1, wherein the frequency range of the characteristic peak of the lithium metal deposited on the surface of the negative electrode in the step (six) is 30 to 1000Hz; the peak intensity was used to measure the amount of lithium analyzed.
CN202211100447.7A 2022-09-09 2022-09-09 Lithium analysis detection method of lithium ion battery Pending CN115508721A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117930064A (en) * 2024-03-21 2024-04-26 四川新能源汽车创新中心有限公司 Method, system, computing equipment and medium for nondestructive testing lithium precipitation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117930064A (en) * 2024-03-21 2024-04-26 四川新能源汽车创新中心有限公司 Method, system, computing equipment and medium for nondestructive testing lithium precipitation

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