CN109211714A - A kind of evaluation method of pulp of lithium ion battery stability - Google Patents
A kind of evaluation method of pulp of lithium ion battery stability Download PDFInfo
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- CN109211714A CN109211714A CN201811287212.7A CN201811287212A CN109211714A CN 109211714 A CN109211714 A CN 109211714A CN 201811287212 A CN201811287212 A CN 201811287212A CN 109211714 A CN109211714 A CN 109211714A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
Abstract
The present invention is the suspension system being made of using pulp of lithium ion battery different material, there is no chemical reactions between each ingredient in slurry, there is no stable chemical bonds, it can be settled as time went under static condition, the homogeneity of slurry is broken, the slurry weight of same volume is changed, the smallest very poor value for obtaining slurry variation of slurry weight is subtracted with slurry weight is maximum, then with this value divided by the smallest slurry weight value multiplied by 100%, what the change rate obtained reacted is the difference of whole slurry, operation of the present invention is simple, testing time is short, it can quickly obtain test result and the accurate stability and consistency for objectively reacting pulp of lithium ion battery.
Description
Technical field
The present invention relates to commenting for lithium ion power battery technology field more particularly to a kind of pulp of lithium ion battery stability
Valence method.
Background technique
As the continuous increase of population in the world radix and (natural gas, petroleum, coal etc.) of non-renewable resources constantly consume,
It is extremely urgent to the exploitation regenerated environment protecting energy.Lithium ion battery has numerous excellent characteristics such as operating voltage height, high-energy-density, work
Make temperature range is wide, specific power is big, the service life is long, it is pollution-free and itself memory effect it is small etc., become the regenerated environment protecting energy
Only choosing.Prepare have excellent performance, the lithium ion battery that security performance is high be industry survival and development inevitable requirement, this
It requires to set about controlling battery production quality from source, and during lithium ion battery is manufactured, the quality of slurry preparation
The performance of battery is influenced huge.Very complicated in view of the system and ingredient of slurry, the stability and consistency of testing size are obvious
It is extremely important, so a kind of method for finding efficient and convenient, simple and practical testing size stability is particularly important.
Cell size is made of solid matter and the liquid substance mixing of different component, is made active material by stirring, is led
Electric agent, binder, solvent etc., which are uniformly dispersed, reaches technique requirement, and final slurry forms a kind of uniformly mixed suspension system.One
As in the case of, the slurry prepared can be coated operation being transferred to next process at the first time, when slurry goes to transfer
Tank and for a long time stand after, the slurry of suspension system will appear layering.Many micron orders, nanoscale pulp particle are easy to send out
Raw to reunite, system uniformity is broken, settles.If Stability of Slurry is poor, active material, conductive agent occur cohesion, divide
Layer just will appear active material, conductive agent is unevenly coated in subsequent coating operations, thus influence battery electric conductivity and
Consistency.After such electrode assembling is at battery, there can be local super-charge super-discharge, negative terminal surface analysis lithium is serious, and capacity is jumped
Water and decaying, cycle life are shunk.If there are such single batteries in a battery pack, can be because of the difference of single battery core
The different pressure difference for causing entire battery pack is big, and battery pack can terminate in advance electric discharge, and actual capacity does not play, and has dragged down battery
Energy density, therefore the stability of slurry has vital influence to battery.The stability of slurry is carried out in production process
Assessment plays guarantee lithium ion battery consistency and energy most important.
The research of evaluation Stability of Slurry is more at present, and it is stable that a kind of cell size is mentioned in patent CN 106124363A
Property measurement method: take prepared positive or negative pole slurry, test revolving speed respectively when changing from small to large and viscosity change and turn
Viscosity change when speed changes from big to small, and two slurry viscosities are drawn respectively with rotation speed change curve；It is viscous to analyze two slurries
Degree illustrates that the positive or negative pole slurry is stablized when two curve co-insides are good with the repeatability of rotation speed change curve
Property is good, when two curve co-insides differences, illustrates that the positive or negative pole Stability of Slurry is poor.This method is although convenient
But also there is its limitation, there is no selection criteria on revolving speed first, need to do a large amount of experiment to verify；Secondly operation is more multiple
Miscellaneous, needing to have higher professional knowledge and technical ability could operate, and operation difficulty is big for battery production personnel.Patent CN
104880384A discloses a kind of evaluation method of lithium ion battery anode glue size stability: anode sizing agent is seated in acid drop
Determine in pipe, vertical standing measured slurry from the top and bottom position of buret respectively after 1-5 hours, used rheometry
Shear rate-viscograph of slurry, when the shear rate of top and bottom position slurry-viscograph repeatability is preferable
It waits, shows that the stability of slurry is good, conversely, showing that the stability of slurry is poor.This method is although simple and fast, but he cannot
Reflect the globality of slurry, and slurry can be stirred during measuring from acid dropper slurry, test result it is accurate
Property needs to be considered.
A kind of evaluation method of pulp of lithium ion battery stability: step S1 is disclosed in patent CN201711330594,
The weight of several samplers is weighed, respectively number record；A certain amount of configured cell size is contained in container by step S2
In, n sampler was placed respectively in the top of container, middle part, the height and position of bottom three, by container sealing and standing A minutes；Step
Rapid S3 slowly respectively takes a sampler from the top of container, middle part, bottom, claims after wiped clean sampler outer wall and bead
Weight, and record the weighing data W of each height and position1；Step S4 repeats step S3 after container sealing, standing B hours, and
Record the weighing data W of each height and position2；Step S5 repeats step S3, and record after container sealing, standing C hours
The weighing data W of each height and position3, until sampler all takes out；Step S6 constantly repeats step S5, and records each
The weighing data W each time of a height and position4、W5…Wn, until sampler all takes out；Step S7, according to weighing data,
The weight rate of upper, middle and lower is calculated, if change rate is not more than 1%, shows that Stability of Slurry is good, conversely,
Show that Stability of Slurry is poor.The patent needs to place n sampler in the slurry, since slurry is suspension system, in slurry
Micron order, nanoscale pulp particle can be easy to sampling wall reunite, accelerate the coagulation of slurry, sampler takes
Slurry can be stirred when out, breaks the state of slurry, and test result objective cannot reflect the stability of slurry；This is special simultaneously
Change rate in benefit is the variation of the same position slurry weight based on different time points, not can determine that the slurry under the time point
Whether stability can continue to coating operations, and timeliness is bad, be unfavorable for operation instruction, influence production efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide it is a kind of it is easy to operate, the testing time is short, can quickly obtain test
As a result the evaluation of the stability of pulp of lithium ion battery and the lithium-ion electric Stability of Slurry of consistency and is accurately objectively reacted
Method.
In order to solve the above-mentioned technical problem, the invention adopts the following technical scheme: a kind of lithium-ion electric Stability of Slurry
Evaluation method, comprising steps of
S1 takes a certain amount of slurry being just stirred with large beaker；
S2 prepares the small beaker of several same sizes, and in the same time, with pipette, the different location from large beaker is distinguished
The slurry of 10ml is pipetted in small beaker, record sample position and calculates separately out the weight of sampling slurry, obtains the same time
Different location samples the maximum value and minimum value of slurry weight, while large beaker being sealed, and stands storage；
S3 calculates the weight rate of sampling slurry, the calculation formula of the weight rate are as follows:
Wherein, MmaxFor the maximum value for sampling slurry weight, MminFor the minimum value for sampling slurry weight；
S4 after large beaker seals the standing A time up for safekeeping, repeats step S2 and S3；
S5 after large beaker seals the standing B time up for safekeeping, repeats step S2 and S3；
S6, if the weight rate of sampling slurry shows that the stability of slurry is good less than 1%, if the weight of sampling slurry
Change rate shows having good stability for slurry between 1%-1.5%, if the weight rate of sampling slurry is greater than 1.5%,
The stability of slurry is not up to standard.
Further, in step s 2, the sample position is apart from slurry upper surface 1cm, 3cm, 5cm, 7cm, 9cm
Place.
Further, in step s 2, the preservation sealed environment temperature is 23~27 DEG C.
Further, in step s 2, the preservation sealed environment humidity is 55~65RH%.
Further, in step s 2, described to be sealed into preservative film sealing.
Further, in step s 4, the A time is 1~10 hour, preferably 10 hours.
Further, in step s 5, the B time is 10~20 hours, preferably 20 hours.
Beneficial effects of the present invention: influence of the present invention by pipette acquisition sampling slurry to slurry form is small, test
As a result the stability of slurry objective can be reflected, weight rate is the slurry weight variation based on same time different location,
It can directly determine whether the Stability of Slurry under the time point can continue to coating operations, timeliness is more preferable, refers to conducive to production
It leads.
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 flow diagram of Example 1 and Example 2 of the present invention.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art without creative labor it is obtained it is all its
His embodiment, shall fall within the protection scope of the present invention.
It should be noted that the directional instruction (up, down, left, right, before and after etc.) of institute is only in the embodiment of the present invention
For explaining in the relative positional relationship under a certain particular pose (as shown in the picture) between each component, motion conditions etc., if
The particular pose changes, then directionality instruction also correspondingly changes correspondingly.
In addition, such as design " first ", " second " description are used for description purposes only in the present invention, and should not be understood as indicating
Or it implies its relative importance or implicitly includes at least one this feature.In description of the invention, the meaning of " plurality " is
At least two, such as two, three etc., unless otherwise specifically defined.
It in addition, the technical solution between each embodiment of the present invention can be combined with each other, but must be general with this field
Based on logical technical staff can be realized, this will be understood that when the combination of technical solution appearance is conflicting or cannot achieve
The combination of kind of technical solution is not present, also not the present invention claims protection scope within.
As shown in Figure 1, the present invention provides a kind of evaluation methods of lithium-ion electric Stability of Slurry, comprising steps of
S1 takes a certain amount of slurry being just stirred with large beaker；
S2 prepares the small beaker of several same sizes, and in the same time, with pipette, the different location from large beaker is distinguished
The slurry of 10ml is pipetted in small beaker, record sample position and calculates separately out the weight of sampling slurry, obtains the same time
Different location samples the maximum value and minimum value of slurry weight, while large beaker being sealed, and stands storage；
S3 calculates the weight rate of sampling slurry, the calculation formula of the weight rate are as follows:
Wherein, MmaxFor the maximum value for sampling slurry weight, MminFor the minimum value for sampling slurry weight；
S4 after large beaker seals the standing A time up for safekeeping, repeats step S2 and S3；
S5 after large beaker seals the standing B time up for safekeeping, repeats step S2 and S3；
S6, if the weight rate of sampling slurry shows that the stability of slurry is good less than 1%, if the weight of sampling slurry
Change rate shows having good stability for slurry between 1%-1.5%, if the weight rate of sampling slurry is greater than 1.5%,
The stability of slurry is not up to standard.
The sample position is the preservation sealed environment temperature at slurry upper surface 1cm, 3cm, 5cm, 7cm, 9cm
Degree is 23~27 DEG C, and the preservation sealed environment humidity is 55~65RH%, described to be sealed into preservative film sealing, the A time
It is 1~10 hour, preferably 10 hours, the B time is 10~20 hours, preferably 20 hours.
Embodiment 1
LiNiCoMn, SP, KS-6 and PVDF are weighed, mass percent presses 95.5,2.0,0.5,2.0, solvent NMP.?
Above-mentioned material is stirred 12 hours in double planetary de-airing mixer, uniform and stable anode sizing agent is made.
What a 500mL glass large beaker prepared first, the small beaker of several 50mL is taken about with 500mL beaker dress
450mL slurry, with RAININ pipette apart from slurry upper surface 1cm, 3cm, 5cm, 7cm, 9cm (from the upper surface of slurry to
The bottom of slurry) at pipette 10ml slurry respectively in 5 beakers, weigh the weight of slurry, be recorded as m respectively1、m2、 m3、m4
And m5.23~27 DEG C of temperature, 55~65RH% of humidity environment in, slurry is sealed with preservative film.After standing 10 hours,
The step of repeating front, pipettes 10ml slurry in 5 beakers in 1cm, 3cm, 5cm, 7cm, 9cm respectively, weighs the weight of slurry
Amount, records respectively；After standing 20 hours, repeatedly the step of front, pipettes 10ml slurry in 1cm, 3cm, 5cm, 7cm, 9cm respectively
In 5 beakers, the weight of slurry is weighed, is recorded respectively, data record is shown in Table 1.
Table 1
By record sheet data and according to weight rate formulaIt can divide
The weight rate that 0h (slurry just prepared) Suan Chu not stood, stand 10h and 20h, as shown in table 2:
Table 2
| Time/h | 0 | 10 | 20 |
| Weight rate/% | 0.22 | 0.57 | 0.75 |
The slurry is up to 0.75% to the weight rate for standing 20h from configuration is good as can be seen from the table, is less than
1%, show that Stability of Slurry is good.
Embodiment 2
Graphite (A8-5), SP, CMC, SBR and EC (dry powder accounting) are weighed, mass percent presses 94.0,2.0,1.5,2.5
With 2.0%, solvent is deionized water.Above-mentioned material is stirred 12 hours in double planetary de-airing mixer, is made uniformly steady
Fixed negative electrode slurry.
What a 500mL glass large beaker similarly prepared, the small beaker of several 50mL is taken about with 500mL beaker dress
450mL slurry, with RAININ pipette apart from slurry upper surface 1cm, 3cm, 5cm, 7cm, 9cm (from the upper surface of slurry to
The bottom of slurry) at pipette 10ml slurry respectively in 5 beakers, weigh the weight of slurry, record respectively.In temperature 23~27
DEG C, in the environment of 55~65RH% of humidity, slurry is sealed with preservative film.After standing 10 hours, repeatedly the step of front, distinguishes
10ml slurry is pipetted in 5 beakers in 1cm, 3cm, 5cm, 7cm, 9cm, is weighed the weight of slurry, is recorded respectively；It is small to stand 20
The step of Shi Hou, repetition front, 10ml slurry is pipetted in 5 beakers in 1cm, 3cm, 5cm, 7cm, 9cm respectively, weigh slurry
Weight, record respectively, data record is shown in Table 3.
Table 3
The weight change that can be calculated respectively by record sheet data and stand 0h (slurry just prepared), stand 10h and 20h
Rate, as shown in table 4:
Table 4
| Time/h | 0 | 10 | 20 |
| Weight rate/% | 0.43 | 1.5 | 1.9 |
After slurry stands 10h known to calculating,It is 1.5%, slurry weight interconversion rate has reached technical papers
The upper limit shows the time of slurry standing no more than 10h, and coating operations must be completed within honest material 10 hours matching.Work as slurry
Material time of repose is 20h,It is 1.9%, the stability of slurry is not up to standard, and the slurry of production is no longer satisfied production work
The requirement of skill.
Working principle of the present invention: the present invention is the suspension system being made of using pulp of lithium ion battery different material,
There is no chemical reactions between each ingredient in slurry, and there is no stable chemical bonds, can prolong with the time under static condition
It grows and settles, the homogeneity of slurry is broken, and the slurry weight of same volume is changed, maximum with slurry weight
Subtract slurry weight it is the smallest obtain slurry variation very poor value, then with this value divided by the smallest slurry weight value multiplied by
100%, what the change rate obtained reacted is the difference of whole slurry, can intuitively determine whether the slurry currently meets technique
It is required that the timeliness to operation instruction is good, while also to reflect slurry face in subsequent coating operations close for the size of very poor value
Spend the size of difference.The stability of slurry can be judged according to this change rate size, the smaller Stability of Slurry of change rate is got over
It is good.
The present invention is complicated in view of existing evaluation and test pulp of lithium ion battery stability and coherence method, and as a result preciseness is inadequate
Height causes the quality of production and production efficiency low, and the test method about Stability of Slurry is proposed in the present invention, is had many excellent
Point, instrumentation is simple first, and operating staff can easily gain the essentials, and secondly instrument and equipment is cheap, not will increase
In addition production cost is that the testing time is short there are one prior feature, can quickly show that test result is simultaneously accurate objective
Ground reacts the stability and consistency of pulp of lithium ion battery, substantially increases the production efficiency of enterprise.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent defines.
Claims (9)
1. a kind of evaluation method of lithium-ion electric Stability of Slurry, which comprises the following steps:
S1 takes a certain amount of slurry being just stirred with large beaker；
S2 prepares the small beaker of several same sizes, and in the same time, with pipette, the different sample position from large beaker are distinguished
The slurry of 10ml is pipetted in small beaker, record sample position and calculates separately out the weight of sampling slurry, obtains the same time
Different location samples the maximum value and minimum value of slurry weight, while large beaker being sealed, and stands storage；
S3 calculates the weight rate of sampling slurry, the calculation formula of the weight rate are as follows:
Wherein, MmaxFor the maximum value for sampling slurry weight, MminFor the minimum value for sampling slurry weight；
S4 after large beaker seals the standing A time up for safekeeping, repeats step S2 and S3；
S5 after large beaker seals the standing B time up for safekeeping, repeats step S2 and S3；
S6, if the weight rate of sampling slurry shows that the stability of slurry is good less than 1%, if the weight change of sampling slurry
Rate shows having good stability for slurry between 1%-1.5%, if the weight rate of sampling slurry is greater than 1.5%, shows to starch
The stability of material is not up to standard.
2. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 1, which is characterized in that in step S2
In, the sample position is at slurry upper surface 1cm, 3cm, 5cm, 7cm, 9cm.
3. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 1, which is characterized in that in step S2
In, the large beaker sealed environment temperature is 23~27 DEG C.
4. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 1, which is characterized in that in step S2
In, the large beaker sealed environment humidity is 55~65RH%.
5. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 1, which is characterized in that in step S2
In, it is described to be sealed into preservative film sealing.
6. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 1, which is characterized in that in step S4
In, the A time is 1~10 hour.
7. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 6, which is characterized in that when the A
Between be 10 hours.
8. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 1, which is characterized in that in step S5
In, the B time is 10~20 hours.
9. a kind of evaluation method of lithium-ion electric Stability of Slurry according to claim 8, which is characterized in that when the B
Between be 20 hours.
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| CN111398140A (en) * | 2019-08-19 | 2020-07-10 | 杭州正银电子材料有限公司 | Stability detection method for silver paste carrier on front side of PREC solar cell |
| CN111624136A (en) * | 2020-06-18 | 2020-09-04 | 合肥国轩高科动力能源有限公司 | Method for detecting stability and viscosity of battery slurry |
| CN112414883A (en) * | 2020-11-22 | 2021-02-26 | 同济大学 | Method for testing stability of catalyst slurry of proton exchange membrane fuel cell |
| CN113075087A (en) * | 2021-04-09 | 2021-07-06 | 芜湖天弋能源科技有限公司 | Electrode paste performance testing device and testing method thereof |
| CN113406274A (en) * | 2021-05-28 | 2021-09-17 | 中国人民解放军空军研究院航空兵研究所 | Mixing uniformity analysis method based on viscosity on-line detection and mixing device |
| CN113702235A (en) * | 2021-07-29 | 2021-11-26 | 浙江野马电池股份有限公司 | Quantitative test method and device for stability of zinc paste for alkaline manganese battery |
| CN117250321A (en) * | 2023-11-17 | 2023-12-19 | 广东众志检测仪器有限公司 | Detection device and detection method for lithium battery |
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| CN111398140A (en) * | 2019-08-19 | 2020-07-10 | 杭州正银电子材料有限公司 | Stability detection method for silver paste carrier on front side of PREC solar cell |
| CN111624136A (en) * | 2020-06-18 | 2020-09-04 | 合肥国轩高科动力能源有限公司 | Method for detecting stability and viscosity of battery slurry |
| CN112414883A (en) * | 2020-11-22 | 2021-02-26 | 同济大学 | Method for testing stability of catalyst slurry of proton exchange membrane fuel cell |
| CN112414883B (en) * | 2020-11-22 | 2022-04-05 | 同济大学 | Method for testing stability of catalyst slurry of proton exchange membrane fuel cell |
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