CN113608135A - Method for prejudging circulating water jumping of lithium ion generation - Google Patents
Method for prejudging circulating water jumping of lithium ion generation Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 230000009191 jumping Effects 0.000 title claims abstract description 7
- 239000003792 electrolyte Substances 0.000 claims abstract description 108
- 238000012360 testing method Methods 0.000 claims abstract description 39
- 238000011065 in-situ storage Methods 0.000 claims abstract description 21
- 238000001514 detection method Methods 0.000 claims description 18
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 230000001351 cycling effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000010586 diagram Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000010812 external standard method Methods 0.000 claims description 3
- 230000010354 integration Effects 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 230000009189 diving Effects 0.000 claims 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 238000002347 injection Methods 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 238000011161 development Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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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]
- G01R31/392—Determining battery ageing or deterioration, e.g. state of health
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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]
- G01R31/3644—Constructional arrangements
- G01R31/3648—Constructional arrangements comprising digital calculation means, e.g. for performing an algorithm
-
- 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]
- G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
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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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- 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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- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention belongs to the field of lithium battery tests, and particularly relates to a method for prejudging circulating water jumping of lithium ions, which comprises the following steps: determining a lowest threshold value of the electrolyte content; the second step is that: measuring the electrolyte consumption rate after short-term circulation of the battery; the third step: testing and calculating the electrolyte content of the battery to be tested; the fourth step: predicting the occurrence of circulating water-jumping of the battery to be tested: namely, the cycle number of the battery to be tested when the water jumps. The method is an in-situ nondestructive test, the normal circulation of the battery is not influenced by the test, the volatilization of the electrolyte of the disassembled battery is not influenced, the accuracy of the test result is higher, and the service life test period of the battery is shortened.
Description
Technical Field
The invention belongs to the field of lithium battery tests, and particularly relates to a method for prejudging circulating water jumping of lithium ions.
Background
Lithium ion batteries are widely used in life and production as a new generation of green high-energy environment-friendly batteries, and have become important development objects of secondary batteries. Along with the continuous upgrading of the market, the cycle life of the lithium ion battery is correspondingly prolonged, and in the process of developing the battery, the evaluation test period of the service life of the lithium ion battery is prolonged, so that the development progress is seriously influenced. With the wide application of the lithium ion battery, the safety performance of the battery is concerned, the battery cycle water-jumping can be judged in advance, the safe service cycle of the battery is greatly helped, and the occurrence of battery safety accidents can be effectively reduced.
Therefore, the development of the method for prejudging the occurrence of the circulating water-jumping of the lithium ion battery plays a positive role in the evaluation test of the service life of the battery in the research and development process of the battery and the evaluation of the safety performance of the battery, the research and development period can be shortened, and more profits are created for the research and development enterprises of the battery.
The lithium ion battery has a small injection amount which affects the cycle performance of the battery, so that a minimum injection amount exists to ensure the normal cycle of the battery. In the battery circulation process, the consumption of the electrolyte is divided into two stages, namely a battery formation stage and an initial circulation stage, the electrolyte consumption rate is high, and after the battery is stable in circulation, the electrolyte consumption rate is stable and is a constant.
Disclosure of Invention
The invention aims to overcome the defect of providing a method for prejudging the circulating water-jumping of lithium ions.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for prejudging circulating water jumping of lithium ions comprises the following steps:
the first step is as follows: determining a lowest threshold value of the electrolyte content: carrying out charge-discharge circulation on batteries with different electrolyte contents at the same multiplying power as that of the battery to be tested, periodically updating circulation data, stopping circulation when an inflection point appears on a battery circulation curve and the battery has a water-jumping trend, and discharging the battery to a safe voltage; testing the electrolyte content of a standard battery with the water jump trend by using an in-situ detection device for the electrolyte content of the lithium ion battery, wherein the obtained electrolyte content is the lowest threshold value of the electrolyte content of the battery of the system and is recorded as m2；
The second step is that: measuring the electrolyte consumption rate after short-term circulation of the battery, wherein the short-term circulation number is nl；
Step 1: testing short-term circulation n of battery to be tested by using in-situ detection device for electrolyte content of lithium ion batterylAfter that time, the electrolyte content, denoted mp0。；
Step 2: after the battery to be tested is circulated for np times in the circulating mode in the first step, the battery to be tested is tested by the established in-situ detection device for the electrolyte content of the lithium ion battery, and after the battery to be tested is circulated for np times, the electrolyte content is recorded as mp2；
And 3, step 3: determination of the electrolyte consumption rate after short cycling of the battery: using the formula Vp ═ (mp)0-mp2) (iv) np; calculating the electrolyte consumption rate; wherein Vp is the electrolyte consumption rate in a certain cycle phase, mp0Is the initial electrolyte content, mp, in a certain cycle phase2The electrolyte content at the end of a certain cycle phase, np is the cycle number in the certain cycle phase;
the third step: and (3) testing and calculating the electrolyte content of the battery to be tested: testing the electrolyte content of the battery to be tested by using the established in-situ detection device for the electrolyte content of the lithium ion battery, and recording the electrolyte content as m1；
The fourth step: predicting the occurrence of circulating water-jumping of the battery to be tested: namely predicting the cycle times of the battery to be tested when the battery jumps; by the formula n ═ m1-m2) And calculating the times of the battery which can still circulate before the battery generates the circulating water-jumping by using the/Vp, wherein n is the times of the battery which can still circulate before the battery generates the circulating water-jumping.
The method for testing the content of the battery electrolyte by the in-situ detection device comprises the following steps:
step 1: making a reference Cell Ref Cell according to the model of the battery to be detected; the difference between the reference battery and the normal battery is that absolute ethyl alcohol or other organic solvents with the solidification temperature lower than the solidification temperature range of the electrolyte are injected into the reference battery, and the electrolyte is injected into the normal battery and then packaged;
step 2: manufacturing series batteries with different electrolyte contents; in order to quantitatively calculate the content of the electrolyte in the battery, a series of batteries with different electrolyte contents, namely Std Cell 1, Std Cell 2 and Std Cell 3 … …, are manufactured according to the test principle of an external standard method;
and 3, step 3: respectively testing and analyzing a reference battery and batteries with different electrolyte contents by using an established in-situ detection device for the electrolyte contents of the lithium ion battery to obtain differential peak areas of the batteries with different electrolyte contents;
and 4, step 4: taking the temperature of each battery as an abscissa and the temperature difference of each battery relative to a reference battery as an ordinate, drawing a temperature difference versus temperature curve of each battery, and performing peak area integration on the temperature difference versus temperature curves of the batteries with different electrolyte contents; and drawing a scatter diagram by taking the peak area as an abscissa and the electrolyte content in the battery as an ordinate, and performing linear fitting to obtain a relational expression between the peak area x and the electrolyte content y, wherein y is kx + b, x is the peak area, and y is the electrolyte content and the unit g.
Preferably, n islIs more than or equal to 100. Vp is the rate of consumption when the cell has reached a cycling steady state; the battery is in a stable circulating state, namely the consumption rate of the electrolyte is basically unchanged, and the amount of the electrolyte is linearly reduced.
Compared with the prior art, the invention has the beneficial effects that:
the method is an in-situ nondestructive test, the normal circulation of the battery is not influenced by the test, the volatilization of the electrolyte of the disassembled battery is not influenced, the accuracy of the test result is higher, and the service life test period of the battery is shortened.
Drawings
FIG. 1 is a graph showing the relationship between the peak area and the amount of injected liquid in example 1 of the present invention;
FIG. 2 is a graph showing the cycle curves of batteries with different injection amounts in example 1 of the present invention.
Fig. 3 is a graph showing a cycle chart of a battery to be tested in embodiment 1 of the present invention.
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.
Example 1 prediction of occurrence of cycle water-jumping of a battery to be tested by using the method of the invention in the example.
1. The establishment of the method for testing the content of the battery electrolyte by the in-situ detection device comprises the following steps:
step 1: and (4) making a reference Cell Ref Cell according to the model of the battery to be tested. The difference between the reference battery and the normal battery is that absolute ethyl alcohol or other organic solvents with the solidification temperature lower than the solidification temperature range of the electrolyte are injected into the reference battery, and the electrolyte is injected into the normal battery and then packaged according to the normal process.
Step 2: and (5) manufacturing series batteries with different electrolyte contents. In order to quantitatively calculate the electrolyte content in the battery, a series of batteries with different electrolyte contents were prepared according to the test principle of the external standard method, and the injection amounts of Std Cell 1, Std Cell 2, Std Cell 3 and Std Cell 4 were 7.1g, 6.4g, 5.8g and 4.9g, respectively.
And 3, step 3: and respectively carrying out test analysis on a reference battery and batteries with different electrolyte contents by using an established in-situ detection device for the electrolyte contents of the lithium ion battery to obtain differential peak areas of the batteries with different electrolyte contents. 1.87, 1.79, 1.70 and 1.64 respectively. The detailed data of the batteries with different injection amounts are shown in table 1.
TABLE 1
| Battery numbering | Injection amount/g | Peak |
| Std Cell | ||
| 1 | 7.1 | 1.87 |
| |
6.4 | 1.79 |
| Std Cell 3 | 5.8 | 1.70 |
| Std Cell 4 | 4.9 | 1.64 |
And 4, step 4: and drawing a temperature difference versus temperature curve of each battery by taking the battery temperature as an abscissa and the temperature difference of each battery relative to a reference battery as an ordinate, and performing peak area integration on the temperature difference versus temperature curves of the batteries with different electrolyte contents. And drawing a scatter diagram by taking the peak area as an abscissa and the electrolyte content in the battery as an ordinate, and performing linear fitting to obtain a relational expression between the peak area x and the electrolyte content y, wherein y is 9.0735x-9.8321, x is the peak area, and y is the electrolyte content and has a unit g. As shown in fig. 1.
2. The method for predicting the occurrence of the circulating water-jumping of the battery to be tested comprises the following steps:
the first step is as follows: determining a lowest threshold value of the electrolyte content: and (3) charging the standard battery at 0.5C, performing charge-discharge cycle at 1C, periodically updating cycle data, wherein the injection amount is 4.9g, the cycle attenuation of the battery is relatively quick, and when an inflection point appears on a battery cycle curve, stopping the cycle and discharging the battery to the safe voltage of 3.5V. Testing the residual quality of the electrolyte by using an established in-situ detection device for the content of the electrolyte of the lithium ion battery to obtain a peak area of 1.57, substituting the peak area into a relation y of 9.0735x-9.8321, calculating the lowest threshold value m of the content of the electrolyte at the moment24.5 g. The cycle data are shown in FIG. 2.
The second step is that: step 1: testing short-term circulation n of battery to be tested by using established in-situ detection device for electrolyte content of lithium ion batteryl120 times ═Thereafter, the electrolyte content was 5.6 g.
Step 2: and (3) circulating the battery to be tested for 100 times in the circulating mode in the first step, and testing the battery to be tested for 100 times by using the established in-situ detection device for the electrolyte content of the lithium ion battery, wherein the electrolyte content is 5.5 g.
And 3, step 3: determining the electrolyte consumption rate of the battery to be tested after short-term circulation: using the formula Vp ═ (mp)0-mp2) (iv) np; the electrolyte consumption rate was calculated. Vp (5.6-5.5)/100 0.001 g/cycle. Wherein Vp is the electrolyte consumption rate in a certain cycle phase, mp0 is the initial electrolyte content in a certain cycle phase, mp2 is the final electrolyte content in a certain cycle phase, and np is the cycle number in a certain cycle phase.
The third step: and (3) testing and calculating the electrolyte content of the battery to be tested: testing the battery to be tested by using the established in-situ detection device for the content of the electrolyte of the lithium ion battery to obtain a peak area of 1.65, substituting the peak area into a relation y of 9.0735x-9.8321, calculating the content mass m of the electrolyte of the battery to be tested1＝5.1g。
The fourth step: predicting the cycle life of the battery to be tested: by the formula n ═ m1-m2) And calculating by/Vp to obtain the number of times of the circulation of the battery before the circulation of the water-skipping, wherein n is (5.1-4.5)/0.001 is 600 cycles. And n is the number of times that the battery can be circulated before the battery generates circulating water jumping, namely the cycle life of the battery. The detailed data of the batteries to be tested are shown in Table 2, and the cycle data are shown in FIG. 3.
TABLE 2
The method is an in-situ nondestructive test, the normal circulation of the battery is not influenced by the test, the volatilization of the electrolyte of the disassembled battery is not influenced, the accuracy of the test result is higher, and the service life test period of the battery is shortened.
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 decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A method for prejudging circulating water jumping of lithium ions is characterized by comprising the following steps:
the first step is as follows: determining a lowest threshold value of the electrolyte content: carrying out charge-discharge circulation on batteries with different electrolyte contents at the same multiplying power as the batteries to be tested, periodically updating circulation data, stopping circulation when the battery circulation curve has an inflection point and has a diving trend, discharging the batteries to a safe voltage, testing the electrolyte content of a standard battery with the diving trend by using an in-situ detection device for the electrolyte content of the lithium ion battery, wherein the obtained electrolyte content is the lowest threshold value of the electrolyte content of the battery of the system and is recorded as m2；
The second step is that: measuring the electrolyte consumption rate after short-term circulation of the battery, wherein the short-term circulation number is nl；
Step 1: testing short-term circulation n of battery to be tested by using in-situ detection device for electrolyte content of lithium ion batterylAfter that time, the electrolyte content, denoted mp0。；
Step 2: after the battery to be tested is circulated for np times in the circulating mode in the first step, the battery to be tested is tested by the established in-situ detection device for the electrolyte content of the lithium ion battery, and after the battery to be tested is circulated for np times, the electrolyte content is recorded as mp2；
And 3, step 3: determination of the electrolyte consumption rate after short cycling of the battery: using the formula Vp ═ (mp)0-mp2) (iv) np; calculating the electrolyte consumption rate; wherein Vp is the electrolyte consumption rate in a certain cycle phase, mp0Is the initial electrolyte content, mp, in a certain cycle phase2The electrolyte content at the end of a certain cycle phase, np is the cycle number in the certain cycle phase;
the third step: and (3) testing and calculating the electrolyte content of the battery to be tested: testing the electrolyte content of the battery to be tested by using the established in-situ detection device for the electrolyte content of the lithium ion battery, and recording the electrolyte content as m1；
The fourth step: circulating water-jumping of battery to be testedAnd (3) prediction: namely predicting the cycle times of the battery to be tested when the battery jumps; by the formula n ═ m1-m2) And calculating the times of the battery which can still circulate before the battery generates the circulating water-jumping by using the/Vp, wherein n is the times of the battery which can still circulate before the battery generates the circulating water-jumping.
2. The method for prejudging lithium ion generation cycle water-skipping according to claim 1, wherein the method for testing the content of the battery electrolyte by the in-situ detection device comprises the following steps:
step 1: making a reference Cell Ref Cell according to the model of the battery to be detected; the difference between the reference battery and the normal battery is that absolute ethyl alcohol or other organic solvents with the solidification temperature lower than the solidification temperature range of the electrolyte are injected into the reference battery, and the electrolyte is injected into the normal battery and then packaged;
step 2: manufacturing series batteries with different electrolyte contents; in order to quantitatively calculate the content of the electrolyte in the battery, a series of batteries with different electrolyte contents, namely Std Cell 1, Std Cell 2 and Std Cell 3 … …, are manufactured according to the test principle of an external standard method;
and 3, step 3: respectively testing and analyzing a reference battery and batteries with different electrolyte contents by using an established in-situ detection device for the electrolyte contents of the lithium ion battery to obtain differential peak areas of the batteries with different electrolyte contents;
and 4, step 4: taking the temperature of each battery as an abscissa and the temperature difference of each battery relative to a reference battery as an ordinate, drawing a temperature difference versus temperature curve of each battery, and performing peak area integration on the temperature difference versus temperature curves of the batteries with different electrolyte contents; and drawing a scatter diagram by taking the peak area as an abscissa and the electrolyte content in the battery as an ordinate, and performing linear fitting to obtain a relational expression between the peak area x and the electrolyte content y, wherein y is kx + b, x is the peak area, and y is the electrolyte content and the unit g.
3. The method according to claim 1, wherein n is nl≥100。
4. The method of claim 1, wherein Vp is the consumption rate of the battery when the battery has reached a steady state of cycling; the battery is in a stable circulating state, namely the consumption rate of the electrolyte is basically unchanged, and the amount of the electrolyte is linearly reduced.
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