CN108508067A - A method of evaluating the battery material of lithium ion battery using Symmetrical cells - Google Patents
A method of evaluating the battery material of lithium ion battery using Symmetrical cells Download PDFInfo
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Abstract
The present invention relates to a kind of methods of battery material that evaluating lithium ion battery using Symmetrical cells, belong to technical field of lithium ion.The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, is included the following steps:1) lithium ion battery is disassembled to obtain pole piece, same sex pole piece is taken to assemble Symmetrical cells;2) Symmetrical cells for obtaining step 1) carry out electro-chemical test;3) battery material is evaluated according to the Electrochemical results of step 2).The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, the performance of electrode material that can be to lithium ion battery full battery in different conditions is accurately tested, and is avoided the electrode material in different conditions affected by the ambient and can not directly be tested its performance.
Description
Technical field
The present invention relates to a kind of methods of battery material that evaluating lithium ion battery using Symmetrical cells, belong to lithium-ion electric
Pool technology field.
Background technology
Lithium ion battery from realize Commercialization application since, achieve in 3C class field of portable electronic apparatus and widely answer
With.In recent years, it is also developed rapidly in fields such as electric vehicles.
When lithium ion battery charges, lithium ion is deviate from from anode, and embedded cathode forms lithium in cathode;When electric discharge, lithium is from negative
Pole is deviate from, again embedded anode.Therefore the cyclical stability of the positive and negative anodes electrode material charge/discharge capacity of lithium ion battery, material
It is related with the insertion of lithium ion and abjection with the high rate performance of material.By to lithium ion battery electrode material lithium ion
Electrochemistry resistance is studied the diffusion impedance of ohmage, charge transfer and lithium ion in solids in abjection and embedded research
The research of anti-spectrum, the research of the cyclic voltammetric performance of Symmetrical cells can have the performance for studying lithium ion battery entirety very big
Meaning.
Currently, for lithium ion battery prepare before positive and negative pole material research comparison it is abundant, but for be prepared into lithium from
Shortcoming is just compared in the research of sub- battery rear electrode material.It is primarily due to after being prepared into battery, after charge and discharge occur, electrode material
Initial state can not be returned to, such as negative material cannot take off lithium completely, in this case to lithium ion cell electrode
The evaluation of material can not accurately reflect the virtual condition of material.
Invention content
The purpose of the present invention is to provide a kind of accurate evaluation can be carried out to the state of the battery material of lithium ion battery
Using Symmetrical cells evaluate lithium ion battery battery material method.
To achieve the above object, the skill of the method for the battery material of the invention that lithium ion battery is evaluated using Symmetrical cells
Art scheme is:
A method of battery material that being evaluated lithium ion battery using Symmetrical cells is included the following steps:
1) lithium ion battery is disassembled to obtain pole piece, same sex pole piece is taken to assemble Symmetrical cells;
2) Symmetrical cells for obtaining step 1) carry out electro-chemical test;
3) battery material is evaluated according to the Electrochemical results of step 2).
The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, can be complete to lithium ion battery
The performance of battery material of the battery in different conditions is accurately tested, avoid the battery material in different conditions by
The influence of ambient enviroment and can not directly test its performance.
The state-of-charge of lithium ion battery in step 1) is 10-90%SOC.
Symmetrical cells in step 1) are button cell or soft-package battery.When button cell or soft-package battery is made, need
Punching press is carried out to the pole piece that dismantling obtains in step 1), suitable shape and the small pole piece of size is made.When button cell is such as made,
Disk is made in punching press.
The preparation method of Symmetrical cells in step 1) includes the following steps:Pole piece is stacked alternately successively with diaphragm, is entered
Shell adds electrolyte, seal, compacting, stand to get.
The pressure of the compacting is 0.09-0.1MPa.
The time of the standing is 20-24h.
The electro-chemical test is ac impedance measurement.
The frequency of disturbance alternating current when the ac impedance measurement is 100kHz-0.01Hz, amplitude 5mV.
The lithium ion battery that there are different electrochemical states from the lithium ion battery in step 1) is taken, step 1) -2 is repeated)
Operation, obtain comparison Electrochemical results, the Electrochemical results in Electrochemical results and step 2) will be compared
It is compared, evaluates the chemical property of battery material;
It is following any one that the lithium ion battery from step 1), which has the lithium ion battery of different electrochemical states,
Kind:A) identical but different recurrent state lithium ion battery is formed from the material of the lithium ion battery material in step 1);B) with
Lithium ion battery material composition difference in step 1) but the identical lithium ion battery of recurrent state;C) with step 1) in lithium from
Sub- battery material forms lithium ion battery that is identical but passing through high-temperature process or low-temperature treatment.
The chemical property of the evaluation battery material refers to the cycle performance or the different electricity of evaluation for evaluating battery material
Influence or evaluation temperature influence to the chemical property of battery material of the pond material to cycle performance of battery.Temperature is to battery
The influence of the chemical property of material refers to the influence of internal resistance of the temperature to the battery prepared using the battery material.
It is described identical as the material composition of the lithium ion battery material in step 1) to refer to and the lithium-ion electric in step 1)
The lithium ion battery for the same size that pond is prepared using identical battery material, identical manufacturing process.Same size refers to electricity
Rated capacity, rated voltage, the specified internal resistance all same in pond.
The material composition difference with the lithium ion battery material in step 1) refers to the lithium ion battery in step 1)
Using the lithium ion battery of same size prepared by different battery materials but identical manufacturing process.Different battery materials
Refer to that any one in positive electrode, negative material, diaphragm, electrolyte differs.
The high-temperature process refers to isothermal holding at temperatures greater than room temperature.The low-temperature treatment refers to less than room temperature
At a temperature of isothermal holding.The time of the isothermal holding is 2-10d.When isothermal holding an AC impedance is carried out every 2-3d
Test.
The present invention effectively, can be commented accurately using the method for the battery material of Symmetrical cells evaluation lithium ion battery
The chemical property of valence battery battery material after different cycle periods, to the cycle life of expected battery, to lithium ion battery
The research etc. of failure mechanism all makes great sense.
Description of the drawings
Fig. 1 is the ac impedance spectroscopy test comparison figure in embodiment 1;
Fig. 2 is the ac impedance spectroscopy test comparison figure in embodiment 2.
Specific implementation mode
Technical scheme of the present invention is described further with reference to specific embodiment.
Embodiment 1
The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, is included the following steps:
1) the qualified lithium ion battery A just produced is taken, after being recycled 50 weeks with the rate charge-discharge of 1C, then with the multiplying power of 0.1C
Charge to the carrying capacity of 50%SOC.
2) lithium ion battery for charging to 50%SOC in step 1) is disassembled in glove box, takes out positive plate, it will
The disk of a diameter of 12.5mm is made in positive plate punching press.Two panels positive plate disk is taken to assemble button cell, the specific steps are:According to
4 drop lithium-ion electrics are added dropwise in the sequence assembling of anode cover, positive plate, the diaphragm of a diameter of 16mm, positive plate, spring leaf, negative electrode casing
Pond electrolyte, sealing.Then the pressure for applying 0.09MPa in two sides of button cell suppresses 1s, and then normal temperature and pressure is quiet again
It sets for 24 hours.
3) battery stood in step 2) is taken, ac impedance spectroscopy test is carried out.The disturbance exchange of ac impedance spectroscopy test
The frequency of electricity is 100kHz-0.01Hz, amplitude 5mV.
The ac impedance spectroscopy measured is as shown in Figure 1.As can be seen from Figure, the impedance value of above-mentioned button cell is
11.01Ω。
4) it is using the same of identical manufacturing process preparation to take the qualified lithium ion battery B, battery B and battery A that have just produced
The battery of batch, the positive electrode used are the ternary material of same specification, other battery materials also all same that the two uses,
After being recycled 100 weeks with the rate charge-discharge of 1C, then charge to the multiplying power of 0.1C the carrying capacity of 50%SOC.It repeats the above steps
1) operation in-step 3).The impedance spectrum measured is as shown in Figure 1, the impedance value for measuring the corresponding button cells of battery B is
12.46Ω。
The test result of the corresponding Symmetrical cells of battery B Symmetrical cells corresponding with battery A is compared, obtains two
The impedance differences of Symmetrical cells are 1.45 Ω.As can be seen that compared with the battery after recycling 50 times, the battery after recycling 100 times
The impedance variations caused by positive electrode are larger.And the ratio of the impedance value according to impedance differences Symmetrical cells corresponding with battery A
Value, can also judge that the variation degree that above-mentioned lithium ion battery occurs in cyclic process material structure is larger.
Impedance results are fitted using ZSimpwin softwares, by fitting result it can be found that both ohmages phase
Poor less SEI membrane impedances A is more than B, and charge transfer impedance A is less than B, but impedance of the impedance of entirety A less than B, the charge of material
Influence of the transfer impedance to material is obvious here.So should focus on to reduce positive electrode to improve the performance of battery
Charge transfer impedance.
Embodiment 2
The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, is included the following steps:
1) the qualified lithium ion battery C just produced is taken, after being recycled 50 weeks with the rate charge-discharge of 1C, then with the multiplying power of 0.1C
Charge to the carrying capacity of 50%SOC.
2) lithium ion battery for charging to 50%SOC in step 1) is disassembled in glove box, takes out negative plate, it will
The disk of a diameter of 12.5mm is made in negative plate punching press.Two panels negative plate disk is taken to assemble button cell, the specific steps are:According to
2 drop lithium-ion electrics are added dropwise in the sequence assembling of anode cover, negative plate, the diaphragm of a diameter of 16mm, negative plate, spring leaf, negative electrode casing
Pond electrolyte, sealing.Then the pressure for applying 0.1MPa in two sides of button cell suppresses 1s, and then normal temperature and pressure is stood
20h。
3) battery stood in step 2) is taken, ac impedance spectroscopy test is carried out.The disturbance exchange of ac impedance spectroscopy test
The frequency of electricity is 100kHz-0.01Hz, amplitude 5mV.
The ac impedance spectroscopy measured is as shown in Figure 2.As shown in Figure 2, the impedance value of the corresponding Symmetrical cells of battery C is
85.8Ω。
4) the qualified lithium ion battery D, battery D and battery C that have just produced is taken to use the different size of different manufacturers
Graphite cathode material, but the same a batch of battery for using identical manufacturing process to prepare, other battery materials that the two uses
All same after being recycled 50 weeks with the rate charge-discharge of 1C, then charges to the multiplying power of 0.1C the carrying capacity of 50%SOC.In repetition
State the operation in step 1)-step 3).The impedance spectrum measured is as shown in Fig. 2, measure the impedance of the corresponding button cells of battery D
Value is 122.42 Ω.
According to ac impedance spectroscopy test data, judge the different materials of battery under same loop state to the influence of battery
Size, battery C and battery D use different negative materials, the two others battery material consistent.Take battery C and battery D difference
It is 3.16m Ω and 3.11m Ω to test its initial impedance value, then tests its impedance value after being recycled 50 weeks with the rate charge-discharge of 1C and be
3.56m Ω and 3.48m Ω.It can not judge that material is more preferable from the internal resistance of full battery, technique is more suitable in other words.
Test result according to Fig.2, is it is found that under identical recurrent state, negative material phase corresponding with battery D
Than caused total resistance is big after cycling for the corresponding negative materials of battery C, it can be determined that the cycle performance of final battery C
Poor circulation of the meeting than battery D.Moreover, using Symmetrical cells come when judging, the impedance differences of the corresponding Symmetrical cells of battery C
Change more obvious.As can be seen from the figure negative material C is bigger than the SEI membrane impedances of negative material D, can be with according to fitting result
Obtain big 20 Ω of SEI impedances of C ratios D.
Embodiment 3
The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, is included the following steps:
1) the qualified lithium ion battery E just produced is taken, after being recycled 50 weeks with the rate charge-discharge of 1C, then with the multiplying power of 0.1C
Charge to the carrying capacity of 50%SOC.
2) lithium ion battery for charging to 50%SOC in step 1) is disassembled in glove box, takes out positive plate, it will
The disk of a diameter of 12.5mm is made in positive plate punching press.Two panels positive plate disk is taken to assemble button cell, the specific steps are:According to
3 drop lithium-ion electrics are added dropwise in the sequence assembling of anode cover, positive plate, the diaphragm of a diameter of 16mm, positive plate, spring leaf, negative electrode casing
Pond electrolyte, sealing.Then the pressure for applying 0.1MPa in two sides of button cell suppresses 1s, is then stood in normal temperature and pressure
22h。
3) battery stood in step 2) is taken, ac impedance spectroscopy test is carried out.The disturbance exchange of ac impedance spectroscopy test
The frequency of electricity is 100kHz-0.01Hz, amplitude 5mV.It specifically tests and is:
The battery stood in step 2) is taken, is placed in 55 DEG C of baking oven, every 3 days, carries out an ac impedance measurement,
It tests 3 times in total;The frequency of the disturbance alternating current of ac impedance spectroscopy test is 100kHz-0.01Hz, amplitude 5mV.It surveys three times
The impedance value obtained is respectively 11.83 Ω, 20.56 Ω, 28.15 Ω.
4) electrode material of used in battery is evaluated according to test acquired results in step 3).Specially according to exchange
Impedance spectrum test data is it is found that positive Symmetrical cells are with the growth of the time preserved at 55 DEG C, and impedance value gradually increases, i.e.,
Lead to the degradation of positive electrode under high temperature.
The qualified lithium ion battery E just produced is taken, after being recycled 50 weeks with the rate charge-discharge of 1C, then is filled with the multiplying power of 0.1C
Electricity to 50%SOC carrying capacity.According to step 1) -2), dismantling battery prepares cathode using negative plate and symmetrically buckles electricity, is placed in 55 DEG C
Baking oven in, every 3 days, carry out an ac impedance measurement, in total test 3 times;The disturbance alternating current of ac impedance spectroscopy test
Frequency be 100kHz-0.01Hz, amplitude 5mV.The impedance value measured three times is respectively 27.94 Ω, 29.9 Ω, 32.88 Ω.
As can be seen that growth of the cathode Symmetrical cells with the time preserved at 55 DEG C, impedance value gradually increase, but the increasing of resistance value
Width is big without positive electrode, i.e., the degradation of positive electrode leads to full battery core poor performance at high temperature under high temperature, i.e., in high temperature
Under, for negative material, positive electrode plays the role of more crucial.
Embodiment 4
The method of the battery material that lithium ion battery is evaluated using Symmetrical cells of the present invention, is included the following steps:
1) the qualified lithium ion battery E just produced is taken, after being recycled 50 weeks with the rate charge-discharge of 1C, then with the multiplying power of 0.1C
Charge to the carrying capacity of 50%SOC.
2) lithium ion battery for charging to 50%SOC in step 1) is disassembled in glove box, takes out positive plate, it will
The disk of a diameter of 12.5mm is made in positive plate punching press.Two panels positive plate disk is taken to assemble button cell, the specific steps are:According to
3 drop lithium-ion electrics are added dropwise in the sequence assembling of anode cover, positive plate, the diaphragm of a diameter of 16mm, positive plate, spring leaf, negative electrode casing
Pond electrolyte, sealing.Then the pressure for applying 0.1MPa in two sides of button cell suppresses 1s, is then stood in normal temperature and pressure
22h。
3) battery stood in step 2) is taken, ac impedance spectroscopy test is carried out.Specially:
The battery stood in step 2) is taken, is placed in subzero 10 DEG C of cryogenic box, every 3 days, carries out primary exchange resistance
Anti- spectrum test, is tested 3 times in total.The frequency of the wherein disturbance alternating current of ac impedance spectroscopy test is 100kHz-0.01Hz, amplitude
For 5mV.
4) electrode material of used in battery is evaluated according to test acquired results in step 3).Specially:According to friendship
Flow impedance spectrum test data 346.04 Ω, 356.52 Ω, 378.23 Ω it is found that Symmetrical cells with preserved at -10 DEG C when
Between growth, impedance value gradually increases, i.e., low temperature can cause the cycle performance of battery material to decline, but anode symmetrical button electricity
Change in resistance is not too much big.
The qualified lithium ion battery E just produced is taken, after being recycled 50 weeks with the rate charge-discharge of 1C, then is filled with the multiplying power of 0.1C
Electricity to 50%SOC carrying capacity.Cathode is prepared using dismantling negative plate according to step 1) to step 2) and symmetrically detain electricity, be placed in 55 DEG C
Baking oven in, every 3 days, carry out an ac impedance measurement, in total test 3 times;The disturbance alternating current of ac impedance spectroscopy test
Frequency be 100kHz-0.01Hz, amplitude 5mV.The impedance value measured three times be respectively 221.85 Ω, 351.34 Ω,
436.59Ω.As can be seen that the impedance value measured using Symmetrical cells is changed greatly, it can more reflect battery material in low temperature
Influence to battery impedance.
Can be seen that anode button electricity by results of AC impedance data comparison, impedance variations are little at low temperature, and cathode
It is relatively more to detain impedance value increase, so negative material is the key that influence battery performance electrode material under cryogenic.
Claims (9)
1. a kind of method of battery material that evaluating lithium ion battery using Symmetrical cells, which is characterized in that include the following steps:
1) lithium ion battery is disassembled to obtain pole piece, same sex pole piece is taken to assemble Symmetrical cells;
2) Symmetrical cells for obtaining step 1) carry out electro-chemical test;
3) battery material is evaluated according to the Electrochemical results of step 2).
2. the method for the battery material according to claim 1 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:The state-of-charge of lithium ion battery in step 1) is 10-90%SOC.
3. the method for the battery material according to claim 1 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:Symmetrical cells in step 1) are button cell or soft-package battery.
4. the method for the battery material according to claim 3 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:The method of assembling Symmetrical cells includes the following steps in step 1):Pole piece is stacked alternately successively with diaphragm, enters shell, is powered up
Solve liquid, seal, compacting, stand to get.
5. the method for the battery material according to claim 4 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:The pressure of the compacting is 0.09-0.1MPa.
6. the method for the battery material according to claim 4 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:The time of the standing is 20-24h.
7. the method for the battery material according to claim 1 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:The electro-chemical test is ac impedance measurement.
8. the method for the battery material according to claim 7 for being evaluated lithium ion battery using Symmetrical cells, feature are existed
In:The frequency of disturbance alternating current when the ac impedance measurement is 100kHz-0.01Hz, amplitude 5mV.
9. the side of the battery material according to any one of claims 1 to 8 for evaluating lithium ion battery using Symmetrical cells
Method, it is characterised in that:The lithium ion battery that there are different electrochemical states from the lithium ion battery in step 1) is taken, step is repeated
1) operation -2) obtains comparison Electrochemical results, will compare Electrochemical results and the electro-chemical test in step 2)
As a result it is compared, evaluates the chemical property of battery material;
The lithium ion battery from step 1) have different electrochemical states lithium ion battery be it is following any one:a)
Identical but different recurrent state lithium ion battery is formed from the material of the lithium ion battery material in step 1);B) with step 1)
In lithium ion battery material composition is different but the identical lithium ion battery of recurrent state;C) with step 1) in lithium ion battery
Material forms lithium ion battery that is identical but passing through high-temperature process or low-temperature treatment.
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CN113138345A (en) * | 2021-03-22 | 2021-07-20 | 万向一二三股份公司 | Method for evaluating performance of lithium ion battery by using symmetric battery |
CN113138345B (en) * | 2021-03-22 | 2023-08-15 | 万向一二三股份公司 | Method for evaluating performance of lithium ion battery by using symmetrical battery |
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