CN110095380A - A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability - Google Patents
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability Download PDFInfo
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- CN110095380A CN110095380A CN201910242683.4A CN201910242683A CN110095380A CN 110095380 A CN110095380 A CN 110095380A CN 201910242683 A CN201910242683 A CN 201910242683A CN 110095380 A CN110095380 A CN 110095380A
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Abstract
The invention discloses a kind of methods of Fast Evaluation lithium ion battery electrode sizing agent stability, the following steps are included: S1, uniform electrode slurry is taken to be placed in rheometer test slot, the rheological behaviour of electrode slurry, obtains rheological curve A when test shear rate is changed from small to big；S2, test shear rate from large to small when test trough in electrode slurry after S1 is tested rheological behaviour, obtain rheological curve B；S3, the repeatability for analyzing rheological curve A and rheological curve B, judge the stability of electrode slurry.The method of Fast Evaluation lithium ion battery electrode sizing agent stability proposed by the present invention, it is simple and quick, the testing time is short, test result is accurate, practical.
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of Fast Evaluation lithium ion battery electrode sizing agent are steady
Qualitative method.
Background technique
With the exhaustion of traditional energy and becoming increasingly conspicuous for environmental problem, lithium ion battery has specific capacity height, puts certainly
Electricity is small, operating temperature range is wide, voltage platform is high, have extended cycle life, memory-less effect, it is environmentally friendly the features such as, as new
Attention of the developing direction of type clean energy resource increasingly by national governments and scientist, is constantly dedicated to developmental research more
Practical and efficient lithium ion battery.In recent years, it attracts attention by the new-energy automobile of core of new energy power, new-energy automobile
It can obtain society to be widely recognized as and receive, be largely determined by the performance of vehicle-mounted lithium ion battery.
New-energy automobile power battery requires lithium-ion battery monomer battery core to have extraordinary consistency of performance, and in electricity
During pond is made, the uniform and stable property of electrode slurry is to influence one of the key factor of battery performance consistency.Lithium-ion electric
The first step that pond is manufactured is exactly that positive and negative anodes electrode closes slurry, is then applied on collector and carries out subsequent battery core production.Electricity
Pond electrode slurry is the suspension system formed after being mixed evenly by active material, conductive agent, binder and solvent, slurry
There are greatest differences for middle different material grains partial size, and surface group is also to be not quite similar to the compatibility of solvent, different
Substance has the different rates of settling, in addition causes different material particle to disperse in the slurry not it also occur that reuniting between particle
Uniformly, the bad stability of slurry.The slurry of stability difference can settle in coating procedure, serious to will lead to slurry point
Layer, causes the coated weight of active material on collector uneven, to influence insertion of the lithium ion in active material and de-
Out, this will lead to production battery core consistency it is very poor, and battery performance is severely impacted, as the internal resistance of cell is high, capacity is relatively low,
Cycle performance is poor etc., and in addition active material unevenly may result in local super-charge super-discharge and form security risk in pole piece.Cause
This, in process of production the stability of Fast Evaluation electrode slurry to ensure lithium ion battery consistency of performance and safety extremely
It closes important.
It generally requires the electrode slurry stirred evenly not settle interior for 24 hours, generallys use settled process characterization electricity at present
The stability of pole slurry stands the slurry stirred evenly for 24 hours, the variation of testing size the upper and lower solid content characterizes
The stability of electrode slurry, this method are takeed a long time, low efficiency using the method stood, existing test method and
Lack the method for rapidly judging to its stability in standard.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of Fast Evaluation lithium ion battery electrode sizing agents
The method of stability, it is simple and quick, the testing time is short, test result is accurate, practical.
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability proposed by the present invention, comprising the following steps:
S1, uniform electrode slurry is taken to be placed in rheometer test slot, electrode slurry when test shear rate is changed from small to big
Rheological behaviour, obtain rheological curve A；
S2, test shear rate from large to small when test trough in electrode slurry after S1 is tested rheological behaviour, obtain
Rheological curve B；
S3, the repeatability for analyzing rheological curve A and rheological curve B, judge the stability of electrode slurry.
Preferably, in S1, the electrode slurry is anode sizing agent or negative electrode slurry.
Preferably, in S1, the electrode slurry is oil system slurry or aqueous slurry.
Preferably, in S1, the solid content of the electrode slurry is 30-70wt%.
Preferably, in S1, shear rate is tested by 1s-1Become larger as 300s-1When electrode slurry rheological behaviour.
Preferably, in S2, shear rate is tested by 300s-1Become smaller as 1s-1When test trough in electrode after S1 is tested
The rheological behaviour of slurry.
Preferably, in the test process of S1 and S2, shear rate change rate is 1s-1/min。
It preferably, is 10s by comparing rheological curve A and rheological curve B medium shear rate in S3-1When viscosity number
To analyze the repeatability of rheological curve A Yu rheological curve B.
Preferably, in S3, if rheological curve B medium shear rate is 10s-1When viscosity number relative in rheological curve A
Shear rate is 10s-1When viscosity number change rate≤10%, then the repeatability of rheological curve A and rheological curve B is good, is surveyed
Slurry is stablized；If rheological curve B medium shear rate is 10s-1When viscosity number relative to rheological curve A medium shear rate be 10s-1When viscosity number change rate > 10%, then rheological curve A and the repeatability of rheological curve B are poor, and surveyed slurry is unstable；Become
Rate calculates as follows: ηAIt is 10s for rheological curve A medium shear rate-1When
Viscosity number, ηBIt is 10s for rheological curve B medium shear rate-1When viscosity number.
In the manufacturing process of lithium ion battery, closing slurry is the first step, generally requires the electrode slurry stirred evenly for 24 hours
It does not settle inside, to ensure the consistency of battery performance.If it is solid to test standing front and back slurry in such a way that tradition is stood
Changing to characterize the stability of slurry for content, then need time of repose for 24 hours, time-consuming, low efficiency；Rheometer is research slurry
One of the instrument for expecting rheological property, can test the viscosity of slurry under different shear rate, if slurry is not sufficiently stable, in high shear
It can be layered under rate, viscosity is caused to become larger.The side of Fast Evaluation lithium ion battery electrode sizing agent stability of the present invention
Method, for existing evaluation method, time-consuming, the defect of low efficiency, electric when changing from small to big first with rheometer test shear rate
The rheological behaviour of pole slurry accelerates the layering of slurry using rheometer high-rate of shear, is then followed by test after above-mentioned test
Electrode slurry shear rate from large to small when rheological behaviour, the rheological behaviour of different test mode slurries is compared, to sentence
Whether disconnected slurry is stable, and this method has many advantages, such as that simple and quick, the testing time is short, test result is accurate, practical；
Compared with prior art, the beneficial effects of the present invention are:
The first, the present invention accelerates the sedimentation of electrode slurry to be layered by rheometer high-rate of shear, surveys to reach shortening
Try the purpose of time, can will the characterization time by being reduced for 24 hours to 10min or so；
The second, the present invention changed from small to big by comparison shear rate and from large to small when slurry rheological behaviour, and then sentence
The stability of broken Electrode slurry can quantify and very accurate；
Third, judgment method of the invention are with simple and quick, the testing time is short, test result is accurate, practicability
The advantages that strong.
Detailed description of the invention
Fig. 1 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 1；
Fig. 2 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 2；
Fig. 3 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 3；
Fig. 4 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 4.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability, comprising the following steps:
S1, it takes the water system negative electrode slurry stirred evenly to be placed in rheometer test slot, tests shear rate from 1s-1Become larger for
300s-1When negative electrode slurry rheological behaviour, obtain rheological curve A, wherein shear rate change rate be 1s-1/min；
S2, still the negative electrode slurry in test trough is used to be tested, tests shear rate from 300s-1Become smaller as 1s-1When
The rheological behaviour of negative electrode slurry obtains rheological curve B, wherein shear rate change rate is 1s-1/min；
S3, compare rheological curve A and rheological curve B medium shear rate for 10s-1When viscosity number, analysis rheological curve A with
The repeatability of rheological curve B judges the stability of slurry.
Fig. 1 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 1, from Fig. 1
It is found that the rheological curve A that two kinds of different test modes measure in S1 and S2 is close with rheological curve B, it is 10s in shear rate-1
When viscosity number be respectively 5469mPa.s and 5431mPa.s, the two is close, therefore thinks that the electrode slurry is stable.Using biography
The method test of the standing of system for 24 hours, the original solid content of the slurry is 53.71%, and slurry upper layer solid content is after standing for 24 hours
51.86%, amplitude of variation 3.44%, less than 5%, therefore the slurry is stable.Method and traditional settled process of the invention
As a result consistent, illustrate that test result of the present invention is accurate, efficient.
Embodiment 2
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability, comprising the following steps:
S1, it takes the oil system anode sizing agent stirred evenly to be placed in rheometer test slot, tests shear rate from 1s-1Become larger for
300s-1When anode sizing agent rheological behaviour, obtain rheological curve A；
It is still tested using the anode sizing agent in test trough after the completion of S2, test, tests shear rate from 300s-1Become
Small is 1s-1When anode sizing agent rheological behaviour, obtain rheological curve B；
S3, compare rheological curve A and rheological curve B medium shear rate for 10s-1When viscosity number analysis rheological curve A with
The repeatability of rheological curve B judges the stability of slurry.
Fig. 2 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 2, from Fig. 2
In it is found that the rheological curve A that two kinds of different test modes measure in S1 and S2 is close with rheological curve B, rheological curve A and rheology
Curve B medium shear rate is 10s-1When viscosity number be respectively 6565mPa.s and 7183mPa.s, amplitude of variation 9.41% is small
In 10%, therefore think that the electrode slurry is stable.Using traditional method test stood for 24 hours, the original solid content of the slurry
It is 60.16%, slurry upper layer solid content is 60.07% after standing for 24 hours, amplitude of variation 0.15%, much smaller than 5%, therefore the slurry
Material is highly stable.Method of the invention is consistent with traditional result of settled process, illustrates that test result of the present invention is accurate, high
Effect.
Embodiment 3
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability, comprising the following steps:
S1, it takes the water system negative electrode slurry stirred evenly to be placed in rheometer test slot, tests shear rate from 1s-1Become larger for
300s-1When negative electrode slurry rheological behaviour, obtain rheological curve A；
It is still tested using the negative electrode slurry in test trough after the completion of S2, S1 test, tests shear rate from 300s-1
Become smaller as 1s-1When negative electrode slurry rheological behaviour, obtain rheological curve B；
S3, compare rheological curve A and rheological curve B medium shear rate for 10s-1When viscosity number analysis rheological curve A with
The repeatability of rheological curve B judges the stability of slurry.
Fig. 3 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 3, from Fig. 3
In it is found that the rheological curve A and rheological curve B that S1 and S2 difference test mode obtains differs greatly, rheological curve A and rheology are bent
Line B medium shear rate is 10s-1When viscosity number be respectively 4522mPa.s and 7077mPa.s, amplitude of variation 56.50%, far
Greater than 10%, therefore think that the electrode slurry is unstable.Using traditional method test stood for 24 hours, the slurry is original solid
Content is 54.31%, and slurry upper layer solid content is 50.09% after standing for 24 hours, amplitude of variation 7.77%, is greater than 5%, therefore should
Slurry is unstable.Method of the invention is consistent with traditional result of settled process, illustrates that test result of the present invention is accurate, high
Effect.
Embodiment 4
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability, comprising the following steps:
S1, it takes the oil system anode sizing agent stirred evenly to be placed in rheometer test slot, tests shear rate from 1s-1Become larger for
300s-1When anode sizing agent rheological behaviour, obtain rheological curve A；
S2, still the anode sizing agent in test trough is used to be tested, tests shear rate from 300s-1Become smaller as 1s-1When
The rheological behaviour of anode sizing agent obtains rheological curve B；
S3, compare rheological curve A and rheological curve B medium shear rate for 10s-1When viscosity number analysis rheological curve A with
The repeatability of rheological curve B judges the stability of slurry.
Fig. 4 is the rheological curve for the electrode slurry that S1 with S2 difference test mode obtains in the embodiment of the present invention 4, from Fig. 4
In it is found that the rheological curve A and rheological curve B that S1 with S2 difference test mode obtains differ greatly, rheological curve A and rheology are bent
Line B medium shear rate is 10s-1When viscosity number be respectively 3497mPa.s and 6358mPa.s, amplitude of variation 81.81%, far
Greater than 10%, therefore think that the electrode slurry is unstable.Using traditional method test stood for 24 hours, the slurry is original solid
Content is 59.37%, and slurry upper layer solid content is 53.77% after standing for 24 hours, amplitude of variation 9.43%, is greater than 5%, therefore should
Slurry is unstable.Method of the invention is consistent with traditional result of settled process, illustrates that test result of the present invention is accurate, high
Effect.
Embodiment 5
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability proposed by the present invention, comprising the following steps:
S1, it takes uniform electrode slurry to be placed in rheometer test slot, tests shear rate by 1s-1Become larger as 300s-1When
The rheological behaviour of electrode slurry obtains rheological curve A；Wherein, the electrode slurry is water system negative electrode slurry；The water system cathode
The solid content of slurry is 70wt%；
S2, test shear rate are by 300s-1Become smaller as 1s-1When test trough in electrode slurry after S1 is tested rheology
Behavior obtains rheological curve B；
S3, by comparing rheological curve A and rheological curve B medium shear rate are 10s-1When viscosity number come analyze rheology song
The repeatability of line A and rheological curve B judge the stability of electrode slurry；
Wherein, in the test process of S1 and S2, shear rate change rate is 1s-1/min。
Embodiment 6
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability proposed by the present invention, comprising the following steps:
S1, it takes uniform electrode slurry to be placed in rheometer test slot, tests shear rate by 1s-1Become larger as 300s-1When
The rheological behaviour of electrode slurry obtains rheological curve A；Wherein, the solid content of the electrode slurry is 30wt%；The electrode slurry
Material is oil system anode sizing agent；In test process, shear rate change rate is 1s-1/min；
S2, test shear rate are by 300s-1Become smaller as 1s-1When test trough in electrode slurry after S1 is tested rheology
Behavior obtains rheological curve B；Wherein, in test process, shear rate change rate is 1s-1/min；
S3, by comparing rheological curve A and rheological curve B medium shear rate are 10s-1When viscosity number come analyze rheology song
The repeatability of line A and rheological curve B judge the stability of electrode slurry.
Embodiment 7
A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability proposed by the present invention, comprising the following steps:
S1, uniform electrode slurry is taken to be placed in rheometer test slot, electrode slurry when test shear rate is changed from small to big
Rheological behaviour, obtain rheological curve A；
S2, test shear rate from large to small when test trough in electrode slurry after S1 is tested rheological behaviour, obtain
Rheological curve B；
S3, the repeatability for analyzing rheological curve A and rheological curve B, judge the stability of electrode slurry；
Wherein, in S1, the solid content of the electrode slurry is 55wt%；The electrode slurry is oil system anode sizing agent；
In test process, shear rate is tested by 1s-1Become larger as 300s-1When electrode slurry rheological behaviour；
In S2, shear rate is tested by 300s-1Become smaller as 1s-1When test trough in electrode slurry after S1 is tested
Rheological behaviour；
In the test process of S1 and S2, shear rate change rate is 1s-1/min；
It is 10s by comparing rheological curve A and rheological curve B medium shear rate in S3-1When viscosity number come analyze stream
The repeatability of varied curve A and rheological curve B.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability, which comprises the following steps:
S1, uniform electrode slurry is taken to be placed in rheometer test slot, the stream of electrode slurry when test shear rate is changed from small to big
Change behavior obtains rheological curve A；
S2, test shear rate from large to small when test trough in electrode slurry after S1 is tested rheological behaviour, obtain rheology
Curve B；
S3, the repeatability for analyzing rheological curve A and rheological curve B, judge the stability of electrode slurry.
2. the method for Fast Evaluation lithium ion battery electrode sizing agent stability according to claim 1, which is characterized in that in S1
In, the electrode slurry is anode sizing agent or negative electrode slurry.
3. the method for Fast Evaluation lithium ion battery electrode sizing agent stability according to claim 1 or claim 2, which is characterized in that
In S1, the electrode slurry is oil system slurry or aqueous slurry.
4. the method for Fast Evaluation lithium ion battery electrode sizing agent stability described in any one of -3 according to claim 1, special
Sign is, in S1, the solid content of the electrode slurry is 30-70wt%.
5. the method for Fast Evaluation lithium ion battery electrode sizing agent stability described in any one of -4 according to claim 1, special
Sign is, in S1, tests shear rate by 1s-1Become larger as 300s-1When electrode slurry rheological behaviour.
6. the method for Fast Evaluation lithium ion battery electrode sizing agent stability described in any one of -5 according to claim 1, special
Sign is, in S2, tests shear rate by 300s-1Become smaller as 1s-1When test trough in electrode slurry after S1 is tested stream
Change behavior.
7. the method for Fast Evaluation lithium ion battery electrode sizing agent stability described in any one of -6 according to claim 1, special
Sign is, in the test process of S1 and S2, shear rate change rate is 1s-1/min。
8. the method for Fast Evaluation lithium ion battery electrode sizing agent stability described in any one of -7 according to claim 1, special
Sign is, is 10s by comparing rheological curve A and rheological curve B medium shear rate in S3-1When viscosity number come analyze stream
The repeatability of varied curve A and rheological curve B.
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| CN112198092A (en) * | 2020-08-24 | 2021-01-08 | 浙江南都电源动力股份有限公司 | Method for testing stability of battery slurry |
| CN114235902A (en) * | 2021-11-15 | 2022-03-25 | 湖北亿纬动力有限公司 | Method for testing dispersion stability of carbon black |
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