CN115754727A - Control method for quantitative lithium analysis of lithium ion battery - Google Patents
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Abstract
The invention relates to the technical field of lithium ion batteries, and discloses a control method for quantitative lithium analysis of a lithium ion battery, which comprises the following steps: calibrating initial capacity C for battery 0 Then discharging the battery to a battery capacity C corresponding to the lithium analysis amount to be researched 1 (ii) a Disassembling the discharged battery, and taking out a negative pole piece in the battery; removing impurities from the disassembled negative pole piece; assembling and combining the cathode pole piece after removing impurities with a newly-made anode pole piece to obtain a reassembled lithium ion battery, and calculating the capacity C of the reassembled lithium ion battery according to the anode pole piece 2 (ii) a According to battery capacity C 0 、C 1 、C 2 And calculating the lithium analysis amount m of the negative pole piece. The lithium ion battery cathode surface reassembled by the method of the invention is uniform in lithium precipitation, the phenomenon of lithium precipitation agglomeration is avoided, the lithium precipitation can be effectively qualitatively and quantitatively analyzed, and the safety problem of the battery caused by the lithium precipitation of the cathode is effectively avoided.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a control method for quantitative lithium analysis of a lithium ion battery.
Background
As an energy storage material, a lithium ion battery has the advantages of high energy density, long cycle life, recoverability and the like, and has been increasingly integrated into the lives of people, such as new energy vehicles, smart phones, energy storage power stations, unmanned aerial vehicles and other lithium ion battery energy storage devices which are visible everywhere in life, and these represent the convenience and social popularity of the lithium ion battery. Data show that the goods output of the lithium ion battery in China reaches 334GWH in 2021, the capacity of the lithium ion battery planned in China reaches 1TWh even in 2025, the market space is estimated to reach trillion scale, and the development prospect is extremely wide. However, because the lithium ion battery has the characteristic of high energy density, the temperature rise is very fast in the thermal runaway process, the heat release is huge, the influence on the life and property safety of people is very easy, and because the lithium ion battery is widely popularized in the society, the thermal runaway phenomenon of the battery becomes a problem which cannot be ignored, so a series of research and improvement measures are carried out in the current industry aiming at the thermal runaway safety of the battery, and the research specifically comprises the intrinsic safety improvement of the battery, the thermal runaway safety mechanism research of the battery, the failure trigger mechanism research of the battery and the like.
In the process of safety research on thermal runaway of lithium batteries, thermal runaway of internal short circuit caused by lithium separation on the interface of a negative electrode of a battery is always a research hotspot, and due to the charging and discharging characteristics of the lithium ion battery, the lithium ion is subjected to deintercalation and intercalation of lithium ions in the positive electrode and the negative electrode, and the inactivation, disorder of N/P ratio, electrolyte loss, polarization of the positive electrode and the negative electrode and the like of positive and negative electrode materials in the circulation process, the phenomenon that lithium metal is separated out on the surface of the negative electrode is usually accompanied in the middle and later life periods of the lithium ion battery, and the serious lithium separation phenomenon has the potential risk of short circuit in the battery caused by conduction of the positive electrode and the negative electrode, so that the research on the safety performance of the lithium separation of the battery has important significance. Currently, the following methods are commonly used in the industry for lithium battery lithium precipitation safety research: (1) battery lithium precipitation reproduction: the method is characterized in that the lithium ion intercalation process in the negative electrode is regulated and controlled by methods such as high-rate charge and discharge, long-term cycle, low-temperature cycle and the like so as to realize the condition of lithium analysis on the surface of the negative electrode, the capacity loss of the lithium battery caused by the method is generally caused by lithium analysis, but the capacity loss of the lithium battery is generally caused by the conditions of inactivation of an electrode material, decomposition of an electrolyte, formation of an SEI film and the like in the normal cycle process of the lithium battery, and the capacity of the battery is also reduced, but the influence of the factors is not considered in the method, so the lithium analysis amount calculated by the lithium analysis of the battery is generally smaller than the actual lithium analysis amount, side reaction also often causes the conditions of deformation, gas production and the like of the lithium battery in the cycle process, and the reliability of safety research on the lithium analysis of the battery is also influenced; secondly, since lithium deposition on the surface of the battery cathode is an accumulative process, the method of repeating lithium deposition by battery cycling requires that the battery be cycled for hundreds of weeks, which is a huge time cost. (2) artificially implanting metal lithium powder to reproduce lithium analysis: the method comprises the steps of weighing the weight of metal lithium powder corresponding to a certain lithium analysis amount of the battery in advance, implanting the weighed metal lithium powder into the battery in the lithium battery assembling process, and performing a series of tests on the battery with the implanted metal lithium powder to represent the safety performance of the battery with the corresponding lithium analysis amount. However, this method also has some disadvantages: firstly, the lithium metal powder has light molar mass (6.94 g/mol), so the requirements on electronic weighing and operation are extremely high when the lithium metal powder is weighed; secondly, the whole process of implanting the lithium metal powder is carried out in a dry environment, the requirement on the environment is strict, the process is complicated, and the operation difficulty is high; finally, because the particle size of the metal lithium powder is small, the agglomeration phenomenon usually occurs in the implantation process, so the uniformity of the distribution of the metal lithium powder on the surface of the pole piece is poor in the implantation process, the phenomenon that the content of the metal lithium powder in a part of regions is high but the metal lithium powder is hardly distributed in the part of regions is easy to occur, and the research significance of the safety research on the lithium separation of the battery under the condition is not great.
Disclosure of Invention
In view of the above, the invention provides a control method for quantitative lithium analysis of a lithium ion battery, so as to solve the problems that the accuracy of lithium analysis amount is poor and the time consumption is long due to more influence factors of lithium analysis safety research of the conventional lithium battery, or the result accuracy is poor due to higher operation requirements and poor distribution uniformity of metal lithium powder.
In order to solve the technical problems, the invention adopts the following technical scheme:
a control method for quantitatively analyzing lithium of a lithium ion battery comprises the following steps:
(1) Calibrating initial capacity C for battery 0 Then discharging the battery to a battery capacity C corresponding to the lithium analysis amount to be researched 1 ；
(2) Disassembling the discharged battery, and taking out a negative pole piece in the battery;
(3) Removing impurities from the disassembled negative pole piece;
(4) Assembling and combining the cathode pole piece after removing impurities with a newly-made anode pole piece to obtain a reassembled lithium ion battery, and calculating the capacity C of the reassembled lithium ion battery according to the anode pole piece 2 ；
(5) According to battery capacity C 0 、C 1 、C 2 And calculating the lithium analysis amount m of the negative pole piece.
Preferably, the lithium ion battery is quantitatively analyzedIn the control method, the battery is subjected to charge-discharge circulation at least once in the step (1), and the discharge capacity of the last circulation period is marked as the initial capacity C of the battery 0 。
Preferably, in the control method for quantitatively analyzing lithium of the lithium ion battery, the lithium analyzing amount in the step (1) is 0-80%, and the corresponding electric quantity condition of the negative pole piece is 0-80%;
further preferably, the lithium precipitation amount is 0-50%, and the corresponding electric quantity condition of the negative pole piece is 0-50%.
In the test operation process, the lithium precipitation amount is not suitable to be too large in consideration of the condition that the safety risk is easily generated due to the combustion caused by oxidation.
Preferably, in the above control method for quantitatively analyzing lithium in a lithium ion battery, before the disassembling in step (2), the method further includes: placing the battery in an environment with the temperature of 15-35 ℃ and fully standing for more than 2 h;
further preferably, the battery is placed in an environment with the temperature of 20-28 ℃ and fully stands for more than 5 h.
Preferably, in the above method for controlling quantitative lithium deposition of a lithium ion battery, the impurity removal operation in step (3) is: and soaking the disassembled negative pole piece in an organic solvent for cleaning and vacuum drying.
Preferably, in the control method for quantitatively analyzing lithium of the lithium ion battery, the soaking time of the negative electrode plate in the organic solvent is at least 2 hours, the vacuum drying temperature is at least 40 ℃, and the drying time is at least 1 hour;
further preferably, the organic solvent is a DMC solvent.
Through experimental research, if the soaking time is too short, the drying temperature is too low, and the drying time is too short, impurities are not thoroughly removed, the water content is too large, the accuracy of a result is seriously affected, and lithium precipitation of a negative electrode plate is not uniform.
Preferably, in the method for controlling the quantitative lithium analysis of the lithium ion battery, in the step (4), the capacity C of the reassembled lithium ion battery is calculated according to the area, the active material component and the content of the positive electrode plate 2 。
Preferably, in the control method for quantitatively analyzing lithium of a lithium ion battery, the newly prepared positive electrode piece in the step (4) is an uncharged positive electrode piece.
Preferably, in the method for controlling quantitative lithium deposition of a lithium ion battery, in the step (5), the amount of lithium deposition m = C in the negative electrode tab 1 *C 2 /(C 0 * m), wherein m is gram capacity, m is more than or equal to 100mAh/g, and more preferably, m is 3860mAh/g.
Preferably, in the method for controlling the quantitative lithium deposition of the lithium ion battery, C is 2 The electrode sheet area per gram volume of positive electrode active material per coated surface density.
Preferably, the method for controlling the quantitative lithium deposition of the lithium ion battery further includes the steps of:
(6) Charging the reassembled lithium ion battery with a charging capacity of C 2 And then disassembling the charged battery, and observing the lithium precipitation condition on the surface of the negative pole piece.
Preferably, the method for controlling the quantitative lithium deposition of the lithium ion battery further includes the steps of:
(7) And (4) carrying out mechanical abuse test, electrical abuse test and thermal abuse test on the reassembled lithium ion battery, namely obtaining the safety performance of the lithium ion battery under the corresponding lithium precipitation condition.
Preferably, in the control method for quantitatively analyzing lithium of the lithium ion battery, the manufacturing of the negative electrode plate and the preparation process of the battery both require to maintain a dry environment.
In addition, the invention also provides a control device, and the control device adopts the control method for quantitatively analyzing lithium of the lithium ion battery.
The invention provides a control method for quantitatively analyzing lithium of a lithium ion battery, which has the following beneficial effects compared with the prior art:
the lithium ion battery cathode surface reassembled by the method is uniform in lithium ion battery cathode surface lithium precipitation, the phenomenon of lithium precipitation agglomeration is avoided, the lithium precipitation can be effectively qualitatively and quantitatively analyzed, the precision of lithium precipitation in the battery is ensured, and the safety problem of the battery caused by lithium precipitation of the cathode is effectively avoided;
the method is suitable for the lithium analysis safety research of various types of lithium ion batteries, in particular to the lithium analysis safety research of soft package lithium ion batteries, square lithium ion batteries and cylindrical lithium ion batteries; the lithium ion analysis safety device is suitable for researching lithium ion analysis safety of a single battery cell, a Pack battery and a battery module; the method is suitable for lithium ion battery lithium separation safety research on the lamination process, the winding process and the cylindrical process; the method is suitable for lithium precipitation safety research of lithium iron phosphate system batteries, ternary system batteries, lithium cobaltate system batteries, lithium manganate system batteries, silicon cathode systems and the like; the method is suitable for lithium analysis safety research of solid lithium ion batteries, semi-solid lithium ion batteries and liquid lithium ion batteries;
according to the invention, the negative pole piece is soaked in the organic solvent before the lithium ion battery is reassembled so as to fully remove impurities, so that the test result is prevented from being influenced due to incomplete removal of the impurities; and the negative pole piece is completely dried and then reassembled into a new lithium ion battery, so that the influence of quality change on a test result is avoided.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of the surface lithium deposition of the negative electrode tab in example 1 of the present invention;
FIG. 2 is a schematic view of the surface lithium deposition of the negative electrode plate in example 2 of the present invention;
fig. 3 is a schematic diagram of the lithium deposition on the surface of the negative electrode tab in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a method for quantitatively controlling lithium separation in a lithium ion battery, and relates to preparation of an experimental battery corresponding to safety test of the lithium ion battery. The invention provides a method for controlling the quantitative lithium analysis in a lithium ion battery by assembling and combining a charged negative electrode plate and a newly-made positive electrode plate.
Example 1
In the process of manufacturing a single battery and conducting 10% safety research on lithium separation of the lithium ion battery, the single battery adopts a 'two-positive three-negative' structure, the initial capacity of the battery is calibrated to be 320mAh, the battery is subjected to constant current discharge for 18min at the current of 0.33C, the discharge capacity is 288mAh, the discharged battery is disassembled and an internal negative pole piece is taken out, the negative pole piece is placed in a DMC solution in a dry environment and is soaked for 48h and then taken out, and then the negative pole piece is baked in an oven at the temperature of 80 ℃ for 24h and is dried. The dried negative pole piece and a newly-made positive pole piece of the same system are laminated and assembled to prepare a single-chip battery with the same area and the structure of 'two positive poles and three negative poles', and the capacity C of the single-chip battery is calculated 2 Is 320mAh, wherein C 2 The calculation formula is as follows: c 2 ＝40cm 2 (electrode piece area) 230mAh/g (gram volume of positive electrode active material) 96.5% (positive electrode active material ratio) 0.036g/cm 2 (coating surface density), charging the prepared single battery, disassembling the fully charged battery and observing the lithium precipitation condition on the surface of the negative pole piece, wherein uniform lithium precipitation and no lithium precipitation occur on the surface of the negative pole as shown in figure 1And (4) lithium agglomeration.
Example 2
In the process of manufacturing a single battery and carrying out 30% safety research on lithium ion battery lithium precipitation, the single battery adopts a 'two-positive-three-negative' structure, the calibration initial capacity of the battery is 600mAh, the battery is subjected to constant current discharge for 54min at the current of 0.33C, the discharge capacity is 420mAh, the discharged battery is disassembled and an internal negative pole piece is taken out, the negative pole piece is placed in a DMC solution in a dry environment and is soaked for 12h and then taken out, and then the negative pole piece is baked in an oven at the temperature of 80 ℃ for 24h and is dried. The dried negative pole piece and a newly-made positive pole piece of the same system are laminated and assembled to prepare a single-chip battery with the same area and the structure of 'two positive poles and three negative poles', and the capacity C of the single-chip battery is calculated 2 Is 600mAh, wherein C 2 The calculation formula is as follows: c 2 ＝90cm 2 (electrode piece area) 250mAh/g (gram volume of positive electrode active material) 95.2% (positive electrode active material ratio) 0.028g/cm 2 (coating surface density), charging the prepared single battery, disassembling the fully charged battery and observing the lithium precipitation condition on the surface of a negative pole piece, wherein as shown in figure 2, the lithium precipitation occurs uniformly on the surface of the negative pole, and the phenomenon of precipitated lithium agglomeration does not occur.
Example 3
In the process of manufacturing a single battery and carrying out 15% safety research on lithium ion battery lithium precipitation, the single battery adopts a 'two-positive-three-negative' structure, the calibration initial capacity of the battery is 450mAh, the battery is subjected to constant current discharge for 27min at a current of 0.33C, the discharge capacity is 67.5mAh, the discharged battery is disassembled to take out an internal negative pole piece, the negative pole piece is placed in a DMC solution in a dry environment and is soaked for 18h and then taken out, and then the negative pole piece is baked in a 90 ℃ oven for 24h to be dried. The dried negative pole piece and a newly-manufactured positive pole piece of the same system are laminated and assembled to prepare a single-chip battery with the same area and the structure of 'two positive poles and three negative poles', the prepared single-chip battery is charged, and the capacity C of the single-chip battery is calculated 2 Is 450mAh, wherein C 2 The calculation formula is as follows: c 2 ＝50cm 2 (electrode piece area) 240mAh/g (gram volume of positive electrode active material) 98.7% (positive electrode active material ratio) 0.038g/cm 2 (coating)Cloth cover density), charging the prepared single battery, disassembling the charged battery and observing the lithium precipitation condition on the surface of the negative pole piece, wherein uniform lithium precipitation occurs on the surface of the negative pole and the phenomenon of lithium precipitation agglomeration does not occur as shown in figure 3.
Example 4
In the process of manufacturing a single battery and conducting 20% safety research on lithium separation of the lithium ion battery, the single battery adopts a 'two-positive three-negative' structure, the initial capacity of the battery is calibrated to be 320mAh, the battery is discharged at the current of 0.33C, the discharge capacity is 256mAh, the discharged battery is disassembled and an internal negative pole piece is taken out, the negative pole piece is placed in a DMC solution in a dry environment and soaked for 48h, and then taken out and baked in an oven at 80 ℃ for 24h for drying treatment. The dried negative pole piece and a newly-made positive pole piece of the same system are laminated and assembled to prepare a single-chip battery with the same area and the structure of 'two positive poles and three negative poles', and the capacity C of the single-chip battery is calculated 2 Is 320mAh, wherein C 2 The calculation formula is as follows: c 2 ＝40cm 2 (electrode piece area) 230mAh/g (gram volume of positive electrode active material) 96.5% (positive electrode active material ratio) 0.036g/cm 2 (coating surface density), charging the prepared single battery, the charging capacity is 320mAh, disassembling the charged battery, and observing the lithium precipitation condition on the surface of a negative pole piece: the surface of the negative electrode has uniform lithium precipitation, and the phenomenon of lithium precipitation agglomeration does not occur.
In summary, the present invention provides a control method capable of implementing quantitative lithium analysis of a lithium ion battery, in the process of assembling the lithium ion battery, a negative electrode plate with a certain amount of electricity is combined with a newly-made positive electrode plate to form the lithium ion battery, the battery capacity can be calculated through the compacted density, thickness, type and content of active materials coated on the positive electrode plate and the negative electrode plate of the lithium ion battery, and then the assembled lithium ion battery is charged (the charging amount is the calculated battery capacity), so that the lithium ion battery with uniform lithium analysis on the surface of the negative electrode can be obtained, and meanwhile, the quantitative regulation and control of the lithium analysis amount in the battery can be implemented by adjusting the charge amount of the negative electrode plate.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the scheme disclosed in the embodiment, the method corresponds to the method disclosed in the embodiment, so the description is simple, and the relevant points can be referred to the description of the method part.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A control method for quantitatively analyzing lithium of a lithium ion battery is characterized by comprising the following steps:
(1) Calibrating initial capacity C for battery 0 Then discharging the battery to a battery capacity C corresponding to the lithium analysis amount to be researched 1 ；
(2) Disassembling the discharged battery, and taking out a negative pole piece in the battery;
(3) Removing impurities from the disassembled negative pole piece;
(4) Assembling and combining the cathode pole piece after removing impurities with a newly-made anode pole piece to obtain a reassembled lithium ion battery, and calculating the capacity C of the reassembled lithium ion battery according to the anode pole piece 2 ；
(5) According to battery capacity C 0 、C 1 、C 2 And calculating the lithium analysis amount m of the negative pole piece.
2. The method as claimed in claim 1, wherein the step (1) comprises cycling the battery at least once and calibrating the discharge capacity of the last cycle as the initial discharge capacity of the batteryCapacity C 0 ；
And/or the lithium precipitation amount in the step (1) is 0-80%;
and/or step (2) further comprises before disassembly: and (3) fully standing the battery for more than 2 hours in an environment of 15-35 ℃.
3. The control method for quantitatively analyzing lithium for a lithium ion battery according to claim 1, wherein the impurity removing operation in step (3) is: and soaking the disassembled negative pole piece in an organic solvent for cleaning and vacuum drying.
4. The control method for the quantitative lithium separation of the lithium ion battery according to claim 3, wherein the soaking time of the negative electrode plate in the organic solvent is at least 2h, the vacuum drying temperature is at least 40 ℃, and the drying time is at least 1h.
5. The method for controlling quantitative lithium analysis of a lithium ion battery according to claim 1, wherein in the step (4), the capacity C of the reassembled lithium ion battery is calculated according to the area, the active material component and the content of the positive pole piece 2 。
6. The method for controlling quantitative lithium analysis of the lithium ion battery according to claim 1, wherein the lithium analysis amount m = C of the negative electrode sheet in the step (5) 1 *C 2 /(C 0 * m), wherein m is gram capacity and is more than or equal to 100mAh/g.
7. The control method for quantitatively analyzing lithium of the lithium ion battery according to claim 6, wherein the value of m is 3860mAh/g.
8. The method for controlling the quantitative lithium separation of a lithium ion battery according to any one of claims 1 to 7, wherein C is 2 And = pole piece area positive electrode active material gram volume positive electrode active material accounts for specific coating surface density.
9. The control method for the quantitative lithium analysis of the lithium ion battery according to any one of claims 1 to 7, characterized by further comprising the following steps:
(6) Charging the reassembled lithium ion battery with a charge capacity of C 2 Then disassembling the charged battery, and observing the lithium precipitation condition on the surface of the negative pole piece;
and/or (7) carrying out mechanical abuse test, electrical abuse test and thermal abuse test on the reassembled lithium ion battery, namely obtaining the safety performance of the lithium ion battery under the corresponding lithium separation condition.
10. A control apparatus, characterized in that the control apparatus employs the control method for quantitatively analyzing lithium of a lithium ion battery according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115995276A (en) * | 2023-03-22 | 2023-04-21 | 四川新能源汽车创新中心有限公司 | Method and device for determining surface density of lithium battery plate and computer terminal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115995276A (en) * | 2023-03-22 | 2023-04-21 | 四川新能源汽车创新中心有限公司 | Method and device for determining surface density of lithium battery plate and computer terminal |
| CN115995276B (en) * | 2023-03-22 | 2023-05-23 | 四川新能源汽车创新中心有限公司 | Method and device for determining surface density of lithium battery plate and computer terminal |
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