CN108896618A - A kind of method and application of the variation of detection anode slice of lithium ion battery residual alkali - Google Patents
A kind of method and application of the variation of detection anode slice of lithium ion battery residual alkali Download PDFInfo
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- CN108896618A CN108896618A CN201810683173.6A CN201810683173A CN108896618A CN 108896618 A CN108896618 A CN 108896618A CN 201810683173 A CN201810683173 A CN 201810683173A CN 108896618 A CN108896618 A CN 108896618A
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Abstract
The method and application that the present invention discloses a kind of detection anode slice of lithium ion battery residual alkali variation reflect the situation of change for shelving aerial anode pole piece residual alkali particular by the method for test anode pole piece internal resistance.The variation of anode slice of lithium ion battery residual alkali mainly due in positive electrode and air water and carbon dioxide react and generate lithium hydroxide and lithium carbonate, the lithium hydroxide and lithium carbonate of generation will increase the internal resistance of anode pole piece, influence battery safety and chemical property.This method is under constant impressed pressure, test the pole piece internal resistance of anode pole piece, by test result and standard specimen comparative analysis, to which the situation of change of aerial anode pole piece residual alkali is shelved in reaction, it can be used for assessing the environment that anode pole piece is shelved, meanwhile, when the internal resistance of pole piece is more than the upper limit, pole piece is scrapped, and prevents battery core inferior from generating.This method is easy to operate, and feasibility is strong, can effectively screen bad anode pole piece.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of detection anode slice of lithium ion battery residual alkali change
The method and application of change.
Technical background
As countries in the world government is to the heightened awareness of global warming and the brought harm of environmental pollution, change the energy
Structure, development new energy industry are to solve one of the important means of global climate and environmental problem.Lithium ion battery has high energy
The advantages that metric density, high voltage, low self-discharge, memory-less effect, long circulation life, environmental protection is the key that develop new energy skill
Art.Currently, being mainly used in the fields such as communications and transportation, E-consumer, energy storage, have to promotion mankind's daily life level great
Meaning.Automobile slowly becomes the indispensable walking-replacing tool of mankind's daily life, so as a kind of common transport facility
And popularizing with automobile, atmosphere pollution caused by motor vehicle exhaust emission has seriously affected mankind's daily life, so greatly
It is one of the effective measures for reducing carbon emission amount and improving environment for human survival that power, which develops new-energy automobile,.Carried out at present in China
" double integrator " policy, it can be seen that comprehensively enter the new-energy automobile epoch be a matter of time.
Lithium ion battery is made of anode, cathode, diaphragm, electrolyte and shell, and wherein the performance of positive electrode is greatly
Determine the performance of battery.Currently, the method that the synthesis of positive electrode is all made of high-temperature calcination, in the condition of sintering high temperature
Under, lithium salts has certain volatilization to a certain extent, so can slightly improve the ratio of lithium to make up sintering process when mixing
In lithium loss, therefore more or less have a small amount of lithium residual, react with air and generate residual alkali, residual alkali is higher to be led
Flatulence in the cyclic process of pond is sent a telegraph, the security performance and cycle performance of battery are greatly reduced.Particular for nickelic positive electrode,
The content of nickel is higher, and the formation of material surface residual alkali is easier.With the continuous improvement required battery core energy density, it is nickelic just
Pole material is the main route for realizing energy density 300Wh/Kg.Although can be carried out to positive electrode after materials synthesis
Residual alkali analysis, whether judgement material is qualified, but in battery core manufacturing process, and anode pole piece can contact more or less production with air
Raw residual alkali.However, there is no more easy methods at present since the temperature that residual alkali (lithium carbonate, lithium hydroxide etc.) decomposes is higher
Pole piece residual alkali content is analyzed, so proposing the method for an analysis anode pole piece residual alkali variation for preventing from producing battery tool inferior
It is of great importance.
CN106248670A discloses a kind of method for measuring residual alkali in a variety of positive electrodes based on automatic titering process, step packet
It includes：Tap water is reburned through water purification machine filtering and boils the obtained pure water of removal CO2；Positive electrode sample is dissolved with pure water and is precipitated, is obtained
Obtain filtrate 1 and residue；Residue is cleaned with pure water again, obtains flushing liquor 2；Filtrate 1 and flushing liquor 2 are merged into solution 3；Using certainly
Dynamic titration outfit, titrates solution 3 with HCl, and titration point is pH=8.5 point and pH=4.0 point respectively；Do not made simultaneously
It is tested with the pure water blank titration of sample, titration point is pH=4.0 point；Positive electrode sample is finally calculated according to measurement data
Residual alkali total amount in product.This method can accurately calculate the residual alkali content in positive electrode sample, but operating process
It is complex, it is not very practical, cannot quickly learn whether residual alkali is exceeded in anode pole piece, to realize to anode pole piece quality
Control.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of methods of detection anode slice of lithium ion battery residual alkali variation
And application.
In order to solve the above technical problem, the present invention provides technical solution it is as follows：
A kind of method of detection anode slice of lithium ion battery residual alkali variation is provided, the particular content is as follows：
The method detects to shelve aerial anode pole piece residual alkali particular by test anode pole piece internal resistance
Situation of change.
Further,
Above-mentioned test anode pole piece internal resistance is to test anode pole piece in constant impressed pressure and under specific pressing time
The pole piece internal resistance value of multiple and different positions.
Further,
During anode pole piece inner walkway, additional constant pressure is 1 × 106~1 × 107Pa。
Further,
During anode pole piece inner walkway, pressing time is 5~30S.
In testing, when testing same (same batch) pole piece, in order to guarantee the accuracy of test, it is necessary to use
Same parameter.
Further,
During anode pole piece inner walkway, the number of positions for testing anode pole piece is 20~40.
Further,
The anode pole piece internal resistance value of test needs the internal resistance value comparative analysis with standard sample, and the standard sample is same
Batch shelves the anode pole piece sample that the time is 0h.
The method of above-mentioned detection anode slice of lithium ion battery residual alkali variation is in the environment that assessment anode pole piece is shelved
Application.
Application of the method for above-mentioned detection anode slice of lithium ion battery residual alkali variation in screening anode pole piece.
Further, for screening anode pole piece, when the anode pole piece internal resistance value of test is above standard the internal resistance value of sample
When the upper limit, the anode pole piece is scrapped.
Working principle：
Anode pole piece is that have already passed through ingredient, coating, roll-in, die cutting procedure latter made.It is fabricated to by anode pole piece
Before battery core, anode pole piece can expose to be contacted with air in air, the high-nickel material in anode pole piece easily with the water in air
Point, carbon dioxide reaction can generate lithium carbonate, lithium hydroxide insulating materials, to reduce pole piece electric conductivity.However, detection pole piece
Lithium carbonate produced, lithium hydroxide are highly difficult, meanwhile, if lithium carbonate, lithium hydroxide remain in battery core, meeting and hydrofluoric acid
Carbon dioxide is produced, flatulence is caused, the water of generation can generate hydrofluoric acid with solute lithium hexafluoro phosphate, form a vicious circle,
Eventually lead to the properties rapid decrease of battery core.
The case where this patent is the internal resistance by detecting pole piece from side, reflects the residual alkali of battery core pole piece.Moreover, production
The internal resistance of anode pole piece changes, be due in positive electrode and air water and carbon dioxide react generate lithium hydroxide and
Caused by lithium carbonate, and the lithium hydroxide and lithium carbonate generated will increase the internal resistance of anode pole piece (without others factor shadow
Ring the variation of pole piece internal resistance), influence battery core chemical property and security performance.
The present invention reflects the situation of change for shelving aerial anode pole piece residual alkali by test anode pole piece internal resistance.
Since the variation of anode slice of lithium ion battery residual alkali is mainly since method provided by the invention is in constant impressed pressure
Under, the pole piece internal resistance of anode pole piece is tested, test result and standard specimen (are shelved the sample that the time is 0h, become at this time without residual alkali
Change) so that the situation of change of aerial anode pole piece residual alkali is shelved in reaction following effect may be implemented in comparative analysis：
(1) invention contacts the residual alkali generated according to anode pole piece with air influences the principle of pole piece internal resistance, from side point
The situation of change of anode pole piece residual alkali is precipitated, can be used for assessing the environment that anode pole piece is shelved.
(2) invention can be used for screening pole piece, when anode pole piece internal resistance is more than the test standard specimen internal resistance upper limit, can scrap
Pole piece prevents the generation of battery core inferior.
(3) the invention this method is easy to operate, feasibility and practical, can be applied to production technology, can effectively sieve
Select bad anode pole piece.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the change curve that anode pole piece internal resistance value in different time periods is shelved in embodiment 1.
Specific embodiment
In order to preferably illustrate the present invention, below by specific example to further description of the present invention.It is special to illustrate herein,
Example is only that more directly description is of the invention, they are a part of the invention, cannot constitute any restrictions to the present invention.
By taking the soft bag lithium ionic cell of model 465473 as an example, wherein workshop condition：Humidity is 20 ± 5%, and temperature is
25 ± 2 DEG C, specific manufacturing process is as follows：
Anode pole piece production：Firstly, positive electrode binder Kynoar (PVDF) is dispersed in Solvents N-methyl pyrrole
In pyrrolidone (NMP), the glue that solid content is 6.5% is made；Then, by positive conductive agent SP (carbon black conductive agent) and CNT (carbon
Nanotube) conductive slurries are separately added into glue, and under conditions of revolving speed is 3000rpm, stirring at normal temperature 240min will then be mixed
It closes anode material nickel cobalt aluminium (NCA) to be added thereto by weight, wherein each material mass percentage ratio is NCA：SP：CNT：PVDF
=97.5%：0.5%：1%：1.0%, under conditions of revolving speed is 2600rpm, stirring at normal temperature 200min, vacuum degassing bubble
20min is 6000-12000mPa.s by the way that NMP is added to adjust slurry viscosity, and solid content is 63%-70%；Finally, will match
The anode sizing agent made is uniformly coated on utter misery aluminium foil front and back sides, and aluminium foil both sides reserve sky foil as pole-piece pole-ear position, is used for
Tab welding, by the way that positive plate is made after roll-in, cross cutting, for use.
Negative electrode tab production：Firstly, sodium carboxymethylcellulose (CMC) is evenly dispersed in deionized water, solid content is made
For 1.2% glue, conductive agent SP is added in glue, under conditions of revolving speed is 2100rpm, stirring at normal temperature 180min, with
Cathode graphite is added afterwards, under conditions of revolving speed is 2400rpm, stirring at normal temperature 200min, finally, SBR suspension is added
Slurry mixes slowly, and vacuumizes bubble removing 20min, wherein each material mass percentage ratio is C：SP：CMC：SBR=95%：
1.5%：1.0%：2.5%, it is 2000-5000mPa.s by the way that deionized water is added to adjust viscosity, solid content is 42%-
50%；Finally, configured negative electrode slurry is uniformly coated on copper foil front and back sides, copper foil both sides reserve sky foil as pole piece pole
Ear is to be used for tab welding, by the way that negative electrode tab is made after roll-in, cross cutting, for use.
Embodiment 1
Test anode pole piece internal resistance, by taking the soft bag lithium ionic cell anode pole piece of model 465473 as an example, concrete operations
Steps are as follows：
1) take 4 cross cutting after anode pole piece (same batch), be washed into 30 sequins, test can be determined by being washed into sequin
The position of internal resistance, because pole piece inner walkway will be ensured of in the same position measurement, this just may insure the accuracy of result.
Sequin diameter is 1cm, and carries out mark and number S1-S30；
2) clamp sequin with tweezers, be placed between probe, open breather valve, the center of probe alignment disk into
Pole pressure piece under row test (test position being scheduled on to the center of sequin, to ensure the accuracy of test result) then is until pressure
Reach 1 × 106Pa keeps 30S, records the internal resistance value of the wafer test point；
3) such as above-mentioned steps 2), successively test the internal resistance value of other sequin centers；
4) the internal resistance Value Data that number S1-S30 sequin measures is collected, mean value is acquired, is denoted as pole piece internal resistance R1；
5) by 30 sequins of above-mentioned number S1-S30, shelve respectively 6h, 12h, 18h, for 24 hours, 30h, 36h, 42h, so
Successively test afterwards and record above-mentioned 30 disks shelve 6h, 12h, 18h, for 24 hours, 30h, 36h, 42h when pole piece internal resistance value, survey
Method for testing is same as above step 2) with test condition, shelve 6h, 12h, 18h, for 24 hours, 30h, 36h, 42h when measure 30 pole piece internal resistances
Value is averaged respectively, is denoted as R2, R3, R4, R5, R6, R7, R8 respectively.
1 embodiment of table, 1 sample shelves time and internal resistance value situation of change table
Internal resistance value situation of change and the change curve for shelving the time are as shown in Fig. 1, can be seen that from upper table 1 with attached drawing 1：
Internal resistance value is incremental with the increase for shelving the time.
Embodiment 2
The present embodiment the difference from embodiment 1 is that, test internal resistance value when, probe apply pressure be 1 × 107Pa is protected
Holding the time is 5S.For test method with embodiment 1, the sample measured shelves time and internal resistance value situation of change table such as the following table 2：
2 embodiment of table, 2 sample shelves time and internal resistance value situation of change table
| Serial number | Sample shelves the time | Serial number | Sample average internal resistance value (Ω) |
| 1 | (h0) | R1 | 0.320 |
| 2 | 6 | R2 | 0.336 |
| 3 | 12 | R3 | 0.350 |
| 4 | 18 | R4 | 0.358 |
| 5 | 24 | R5 | 0.398 |
| 6 | 30 | R6 | 0.417 |
| 7 | 36 | R7 | 0.449 |
| 8 | 42 | R8 | 0.461 |
Embodiment 3
The present embodiment the difference from embodiment 1 is that, test internal resistance value when, probe apply pressure be 4 × 106Pa is protected
Holding the time is 20S.For test method with embodiment 1, the sample measured shelves time and internal resistance value situation of change table such as the following table 3：
3 embodiment of table, 3 sample shelves time and internal resistance value situation of change table
It can be seen that from the test result of above-described embodiment 1-3：
Applying under different pressures and pressure time, the resistance value measured has difference, therefore in order to ensure the test results
Accuracy should be tested in same pressure and under the same pressure time.
The test result of above-described embodiment 1-3 is shown：The internal resistance value of anode pole piece is passed with the increase for shelving the time
Increase.
Comparative example 1：
The anode pole piece, cathode pole piece, diaphragm that shelve 0h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 2：
The anode pole piece, cathode pole piece, diaphragm that shelve 6h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 3：
The anode pole piece, cathode pole piece, diaphragm that shelve 12h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 4：
The anode pole piece, cathode pole piece, diaphragm that shelve 18h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 5：
Anode pole piece, cathode pole piece, the diaphragm of shelving for 24 hours are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 6：
The anode pole piece, cathode pole piece, diaphragm that shelve 30h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 7：
The anode pole piece, cathode pole piece, diaphragm that shelve 36h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
Comparative example 8：
The anode pole piece, cathode pole piece, diaphragm that shelve 42h are fabricated to naked battery core, short-circuit test by the way of lamination
Afterwards, after tab welding, top side seal, baking, fluid injection, chemical conversion, the forming of two envelopes, partial volume, being fabricated to capacity is 2Ah, model
465473 soft bag lithium ionic cell.
The anode pole piece of above-mentioned comparative example 1-8 is same batch, and the battery core that comparative example 1~8 makes is done room temperature respectively and is followed
Ring test, test result are as shown in table 1：
The test of 4 normal temperature circulation of table
| Comparative example serial number | Cycle-index | Conservation rate | Flatulence situation |
| 1 | 506 | 90.6% | Non- flatulence |
| 2 | 498 | 90.8% | Non- flatulence |
| 3 | 510 | 89.3% | Non- flatulence |
| 4 | 503 | 88.9% | Non- flatulence |
| 5 | 512 | 88.1% | Non- flatulence |
| 6 | 508 | 85.6% | Slight flatulence |
| 7 | 511 | 84.3% | Slight flatulence |
| 8 | 518 | 82.4% | Flatulence |
Comparative example 1-8 be respectively shelve 0h, 6h, 12h, 18h, for 24 hours, after 30h, 36h, 42h positive plate production battery core
Corresponding cycle performance and flatulence situation, shown in specific test result table 4 as above, as can be seen from Table 4：Positive plate and air
Time of contact is longer (it is longer to shelve the time), and cycle performance is poorer, flatulence situation is also more serious.
The time is shelved in air when above-mentioned pole piece reaches 30h, when, battery will start slight flatulence occur, and electric discharge is held
Amount conservation rate also drops to 85.6%, and when shelving the time up to 42, battery will appear more serious flatulence.
Therefore the method for above-mentioned detection anode slice of lithium ion battery residual alkali variation provided by the invention can pass through internal resistance
The variation of value relatively accurately reflects the variation of anode pole piece residual alkali, whether can be used for assessing environment that anode pole piece is shelved
Suitable for storing pole piece；It can be used for screening anode pole piece simultaneously, when the anode pole piece internal resistance value of test is above standard sample
When the internal resistance value upper limit, the anode pole piece is scrapped, prevents the generation of battery core inferior.
The above is a specific embodiment of the invention, but any restrictions cannot be constituted to the present invention, therefore need special
It points out, it is all based on the present invention, it is made any modification and is all fallen within the scope of the present invention with improvement.
Claims (10)
1. a kind of method of detection anode slice of lithium ion battery residual alkali variation, which is characterized in that the method is to pass through test
The method of anode pole piece internal resistance shelves the situation of change of aerial anode pole piece residual alkali to detect.
2. a kind of method of detection anode slice of lithium ion battery residual alkali variation according to claim 1, which is characterized in that
Test anode pole piece internal resistance is to test the multiple and different positions of anode pole piece in constant impressed pressure and under specific pressing time
Pole piece internal resistance value.
3. a kind of method of detection anode slice of lithium ion battery residual alkali variation according to claim 2, which is characterized in that
During anode pole piece inner walkway, additional constant pressure is 1 × 106~1 × 107Pa。
4. a kind of method of detection anode slice of lithium ion battery residual alkali variation according to claim 2, which is characterized in that
During anode pole piece inner walkway, pressing time is 5~30S.
5. a kind of method of detection anode slice of lithium ion battery residual alkali variation according to claim 2, which is characterized in that
During anode pole piece inner walkway, the number of positions for testing anode pole piece is 20~40.
6. a kind of method of detection anode slice of lithium ion battery residual alkali variation according to claim 1, which is characterized in that
The anode pole piece internal resistance value of test needs the internal resistance value comparative analysis with standard sample, and the standard sample is that same batch is shelved
Time is the anode pole piece sample of 0h.
7. a kind of method of detection anode slice of lithium ion battery residual alkali variation according to claim 1, which is characterized in that
Above-mentioned anode pole piece includes：Positive electrode NCA, conductive agent SP, CNT conduction slurries and binder Kynoar,
In：NCA：SP：CNT：The mass percent of PVDF is 97.5%：0.5%：1%：1.0%.
8. the method that a kind of detection anode slice of lithium ion battery residual alkali as described in claim 1-7 any one changes is being commented
Estimate the application in the environment that anode pole piece is shelved.
9. the method that a kind of detection anode slice of lithium ion battery residual alkali as described in claim 1-7 any one changes is being sieved
Select the application in anode pole piece.
10. application according to claim 9, which is characterized in that for screening anode pole piece, when in the anode pole piece of test
Resistance value be above standard sample the internal resistance value upper limit when, scrap the anode pole piece.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109738309A (en) * | 2019-01-31 | 2019-05-10 | 河北超威电源有限公司 | Lead charcoal power battery electrode board detecting method based on numerical analysis |
| CN109888295A (en) * | 2019-02-28 | 2019-06-14 | 合肥国轩高科动力能源有限公司 | A kind of affluxion body in lithium ion batteries coating paste, collector and preparation method thereof |
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| CN109738309A (en) * | 2019-01-31 | 2019-05-10 | 河北超威电源有限公司 | Lead charcoal power battery electrode board detecting method based on numerical analysis |
| CN109738309B (en) * | 2019-01-31 | 2021-07-20 | 河北超威电源有限公司 | Lead-carbon power battery pole plate detection method based on numerical analysis |
| CN109888295A (en) * | 2019-02-28 | 2019-06-14 | 合肥国轩高科动力能源有限公司 | A kind of affluxion body in lithium ion batteries coating paste, collector and preparation method thereof |
| CN109888295B (en) * | 2019-02-28 | 2021-09-03 | 合肥国轩高科动力能源有限公司 | Coating slurry for lithium ion battery current collector, current collector and preparation method of current collector |
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| CN108896618B (en) | 2023-06-09 |
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