CN110411913A - A kind of lithium ion battery separator coating size performance evaluation method - Google Patents
A kind of lithium ion battery separator coating size performance evaluation method Download PDFInfo
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- CN110411913A CN110411913A CN201910625513.4A CN201910625513A CN110411913A CN 110411913 A CN110411913 A CN 110411913A CN 201910625513 A CN201910625513 A CN 201910625513A CN 110411913 A CN110411913 A CN 110411913A
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- coating
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- ion battery
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
- G01N2013/0208—Investigating surface tension of liquids by measuring contact angle
Abstract
The invention discloses a kind of lithium ion battery separator coating size performance evaluation methods, the following steps are included: carrying out testing graininess, contact angle test, potential value test, rheometer test with slurry to coating, it is set according to coating slurry items test result standards of grading or grade, it is summed up in conjunction with the default weight of items test, obtains the comprehensive performance of coating slurry.Test method in the present invention is easy to operate, and testing result is reliable, and practicability is stronger, can be that application of the diaphragm coating slurry under different technology conditions improves accurately reference.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of lithium ion battery separator coating is evaluated with size performance
Method.
Background technique
Diaphragm is one of four big main materials very crucial in battery, and electrical property and security performance to battery have directly
It influences, with the gradually promotion of battery energy density, lightening, diaphragm the functionalization of basement membrane is had become for application trend, band
There is the coated separator of resistance to heat function, infiltration function, temperature-sensitive function, adhesion strength to apply also more and more extensive, painting in battery system
Cover the lithium ion transport rate that diaphragm will directly affect battery, dispersibility, stability and the stream of floating coat slurry
Levelling directly affects the consistency and stability of coating, so the performance of diaphragm coating slurry is also more and more important.
But size performance difference is very big under different technology conditions, evaluates and tests diaphragm coating slurry properties in industry not yet at present
The method of energy, but the test and evaluation of lithium ion battery coating diaphragm production floating coat size performance are an important rings
Section needs that coating is combined to require the assessment for carrying out slurry comprehensive performance, can play certain guidance for coated separator performance
Effect.
Summary of the invention
In view of this, it is necessary to provide a kind of lithium ion battery separator coating size performance evaluation methods by the present invention, originally
Test method in invention is easy to operate, and testing result is reliable, and practicability is stronger, can be diaphragm coating slurry in difference
Application under process conditions improves accurately reference.
A kind of lithium ion battery separator coating size performance evaluation method, comprising the following steps:
Testing graininess is carried out with slurry to coating, the coating slurry is judged according to testing graininess result and dispersion degree
Dispersibility；
Contact angle test is carried out with slurry to coating, the coating slurry and coating are judged according to contact angle test result
Levelability and wellability between substrate；
Potential test is carried out with slurry to coating, the stabilization of the coating slurry is judged according to potential value test result
Property；
Viscosity test is carried out with slurry to coating, is starched according to the coating slurry viscosity and shear rate, the coating
Expect that viscosity and time changing curve judge the viscosity and rheological characteristic of slurry；
It is set according to coating slurry items test result standards of grading or grade, in conjunction with the default weight of items test
It sums up, obtains the comprehensive performance of coating slurry.
Further, the testing graininess use laser particle analyzer, test respectively the coating slurry D10,
D50 and D90 calculates the span R of slurry by (D90-D10)/D50, under the conditions of can assessing different slurry-stirring process by span R
The degree of scatter of slurry, different slurry-stirring process can be one or both of high speed dispersion, sand milling dispersion here.It is specific next
It says, D10 and D90 respectively indicate the size indicator of sample taper end and butt end to be tested, and D50 is meso-position radius or median particle diameter, commonly use
Indicate average particle size, creative definition span R is (D90-D10)/D50 in the present invention, can be used to assess coating and starch
The dispersion degree of material, when span R is smaller, show greater particle size with it is suitable compared with small particle difference and D50, the stability of slurry entirety is more
Height illustrates the dispersibility of slurry under this state very well.That is, partial size is smaller, span is smaller, show slurry dispersibility compared with
It is good；Partial size and span are bigger, show that slurry dispersibility is poor, may will affect the homogeneity of coating.It is surveyed in granularity of the invention
Conventional particle size analyzer is used, as long as the purpose for being able to achieve testing graininess may be used to technical side of the invention
Case, and laser particle analyzer due to its be advanced laser diffraction technology and height it is practical conventional granulates characterization perfect combination,
Its particle size distribution measurement result is relatively reliable, therefore, preferably uses laser particle analyzer in some embodiments of the invention.
Further, contact angle refers to that the tangent line of the liquid-vapor interface made by gas, liquid, solid three-phase point of intersection, this tangent line exist
The angle α between solid-liquid boundary line of one side of liquid is the measurement of wetness degree.If α < 90 °, the surface of solids is hydrophilic
Property, i.e. liquid is easier to wetting solid, and angle is smaller, indicates that wetability is better；If α > 90 °, the surface of solids be it is hydrophobic,
I.e. liquid is not easily wetted by solid, and it is related with the interfacial tension of system to be easy shifting wet processes on the surface.One drop of liquid is fallen in
On the horizontal surface of solids, when equilibrium is reached, following young's formula is met between the contact angle of formation and each interfacial tension
(Young Equation): γ SV=γ SL+ γ LV × cos θ e
Following several Wet Outs can be predicted by it:
1) when θ=0, complete wetting；
2) when 90 ° of θ ﹤, partially wetted or wetting；
It 3) is line of demarcation whether wetting when θ=90 °；
4) nonwetting when 90 ° of θ ﹥；
5) completely nonwetting when θ=180 °.
Therefore, its levelability and wellability can be commented by measuring the contact angle of coating slurry, specifically, when contact
Angle α is smaller, and levelability and wellability are better；Contact angle α is bigger, and levelability and wellability are poor, may will affect the one of coating
Cause property and coating processes.The contact angle test is measured by contact angle tester using amount supreme people's court, and fluid injection is adopted in measurement process
With impregnator drop capillary, testing substrates select diaphragm face to be tested, diaphragm face to be tested here can selected from PP basement membrane,
PE basement membrane, aluminium oxide ceramics diaphragm, boehmite ceramic diaphragm, gluing diaphragm.
Further, the potential test use Zeta potential analysis instrument, wherein Zeta potential range be -150mV~
150mV, particle size range are 10nm~30 μm, and conductivity range is 0~200mS/cm, and measurement angle is 90 °, temperature range 2
~90 DEG C.Zeta potential is the important indicator for characterizing colloidal dispersion stability, is continuous phase and to be attached on dispersed particle
Potential difference between fluid stable layer, its numerical value is related to the stability of colloidal dispersion, be to mutually exclusive between particle or
The measurement of the intensity of attraction.Molecule or dispersed particle are smaller, and the absolute value (positive or negative) of Zeta potential is higher, and system is more steady
It is fixed, that is, it dissolves or disperses that aggregation can be resisted.Conversely, Zeta potential (positive or negative) is lower, more tends to condense or agglomerate, that is, inhale
Gravitation has been more than repulsive force, and dispersion is destroyed and coagulates or agglomerate, and Zeta potential absolute value represents its stability size, just
Negative which kind of charge of particle band represented, the general relationship between Zeta potential and system stability is as follows:
Zeta potential [mV] colloidal stability
0 to ± 5, rapid condensation or cohesion
± 10 to ± 30, start to become unstable
± 30 to ± 40, stability is general
± 40 to ± 60, preferable stability
More than ± 61, excellent stability.
Therefore, the potential test instrument of this field routine can be used in the potential test in the present invention using testing size, as long as
It is able to achieve the purpose of potential test, uses Zeta potential analyzer in some embodiments of the present invention.Pass through potential value
Size can judge the stability of slurry, specifically, current potential β test result is bigger, the stability of slurry is better；Current potential β test
As a result smaller, Stability of Slurry it is bad it is easier settle, be unfavorable for production technology processing coating.
Further, by rheometer test it is recognized that viscosity under some test condition, also is understood that fluid
Characteristic, for example be Newtonian fluid, pseudoplastic fluid or Bingham plastic fluid etc., subsequent test is more advantageous to after understanding fluid type
Demonstrate,prove work.The rheometer test instrument of this field routine can be used in rheometer test in the present invention, as long as being able to achieve the mesh of rheometer test
.The condition for crossing setting test, directly can obtain test curve from instrument test result.Further, the stream
Become test and use rotational rheometer, the rheometer selects the torque of disk plate, and the disk plate diameter is 35mm, relatively more suitable
For diaphragm coating paste.Alternation formula shear rate is 1~300s-1, shearing force be 1~300Pa, shear time 100s~
200s.The preferred rotational rheometer of the present invention is can to measure torque in stabilization or speed change since rotational rheometer is measured,
It converts physical quantity to the fixture factor parameter of rheology, carries out speed of steady state scanning, apply different shear rates, it can be with
The shear rate and viscosity under stable state are recorded, the viscosity and rheological data of slurry are obtained.And in the relatively small slurry of viscosity
More evenly, pulp surface may be implemented uniformly to break portion's stress, and the interface planarization of breaking part is fine；Viscosity is relatively small
Slurry has better mobility and tensile property, and whole levelability is slightly good when coating, and the homogeneity of coating also can be more preferable.Cause
This, according to the slurry viscosity η and shear rate, slurry viscosity η and time changing curve of test result judge slurry viscosity and
Rheological characteristic, alternation formula rheometer test viscosity is smaller, is relatively suitble to coating, viscosity is larger, is unfavorable for the adjustment of coating processes.
Further, every test result standards of grading are to be followed successively by 3 points, 2 points, 1 point, the items from high in the end
The default weight of test is granularity 30%, contact angle 30%, current potential 20%, viscosity 20%.
Evaluation method of the invention can quickly test the comprehensive performance for evaluating diaphragm slurry, easy to operate, test knot
Fruit high reliablity, practicability is stronger, and the application that can be diaphragm coating slurry under different technology conditions provides accurate ginseng
It examines.
Detailed description of the invention
Fig. 1 is the flow diagram of the coating slurry evaluation method of a preferred embodiment in the present invention.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with specific embodiments to invention is more fully described.But
It is that the invention can be realized in many different forms, however it is not limited to embodiments described herein.On the contrary, providing
The purpose of these embodiments is to make to make the present disclosure more fully understandable.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
The evaluation of coating slurry in the embodiment of the present invention uses method as shown in Figure 1, specific as follows:
Testing graininess: opening particle size analyzer attachment, opens optical element, and switch starting computer opens software and instrument
Parameter, pump speed 2000, ultrasonic intensity 13, interior ultrasonic time 30s is arranged after preheating 30min in link.Pump speed is opened, in beaker
In be put into pure water cleaning pipeline and sample cell, in beaker plus the pure water of 800ml, fill in sample in software test menu
Name is clicked green color key and is started, its optical property parameter is arranged, refractive index is respectively 1.78/1.80/ in Examples 1 to 3
2.55, dispersing agent 1.33, obscurity 13~16%, system focuses rear testing background automatically, after system prompt sample is added
Beaker is added in sample by product, is opened ultrasonic wave, is started to test within 10-12 seconds or so after ultrasound, and system will test 3 times automatically,
An average value and size indicator D10, D50, D90 are created, test data is recorded, is obtained according to formula R=(D90-D10)/D50
Span R judges the dispersibility of slurry according to the numerical value of span R.
Contact angle test: basement membrane to be measured selects PE basement membrane, and drop is suspended in capillary needle by impregnator drop capillary
At head, workbench is adjusted, stops and save image after observing drop and PE basement membrane face contact, the measurement of utilization supreme people's court obtains
Contact angular data records data.The levelability and wellability of slurry are judged according to the contact angle size measured.
Potential test: testing coating with slurry using Zeta potential analyzer, parameter is arranged are as follows: current potential range-
150mV~150mV, particle size range 10nm~30 μm, 0~200mS/cm of conductivity range, 90 ° of measurement angle, temperature range 2~
90 DEG C, scanning times 3, residence time 5S selects solvent for water, starts to test, and records Zeta potential value, is surveyed according to potential value
The size of test result judges the stability of slurry.
Rheometer test: testing slurry using rheometer, according to the slurry viscosity η of test result and shear rate with
And slurry viscosity and time changing curve judge the viscosity and rheological characteristic of slurry, rheometer selects the torque of disk plate, and diameter is
35mm, alternation formula shear rate are 1-300S-1, shearing force 1-300Pa, shear time 100S-200S, it is bent that record saves test
Line number evidence, alternation formula rheometer test viscosity is smaller, is relatively suitble to coating, viscosity is larger, is unfavorable for the adjustment of coating processes.
Embodiment 1
The preparation of slurry: according to parts by weight, by 30 parts of aluminum oxides, 0.4 part of ammonium polyacrylate salt copolymerized solution, 0.1
Part layered silicate synthesis class solution and 65 parts of deionized waters are added in dispersion machines, and control dispersion machine temperature is 25 DEG C, power is
2000W disperses 1.5 hours, and 4 parts of aqueous poly- propionic acid modified resins, 0.5 part of organic silicon modified by polyether surface-active are then added
Agent is into dispersion machine, and to keep the temperature of dispersion machine be 25 DEG C, power 400W, continues to disperse 1 hour and crosses 200 mesh screens, obtains
Slurry.
It takes slurry to carry out granularity, contact angle, current potential and rheological characteristic test respectively according to the step in Fig. 1, the results are shown in Table 1.
Embodiment 2
The preparation of slurry: according to parts by weight, by 25 parts of boehmites, 1 part of polyvinylpyrrolidonesolution solution, 0.6 part of methylol
Sodium cellulosate solution and 70 parts of deionized waters are added in dispersion machines, and control dispersion machine temperature is 30 DEG C, power 2500W, dispersion 1
Then 3 parts of aqueous poly- propionic acid modified resins, 0.4 part of aqueous non-ion fluorin carbons surfactant are added in a hour, keep dispersion
The temperature of machine is 30 DEG C, power 500W, continues to cross 200 mesh screens in dispersion 1 hour, obtains slurry.
It takes slurry to carry out the test of granularity, contact angle, current potential, rheological property respectively according to the step in Fig. 1, the results are shown in Table
1。
Embodiment 3
The preparation of slurry: according to parts by weight, by 28 parts of titanium dioxide, 1 part of poly-vinyl alcohol solution, 0.4 part of synthesis stratiform silicon
Acid salt solution and 65 parts of deionized waters are added in dispersion machines, and control dispersion machine temperature is 35 DEG C, power 3000W, disperse 2 small
When, 5 parts of aqueous poly- propionic acid modified resins, 0.6 part of aqueous anion fluorine carbon surfactant are then added, keep dispersion machine
Temperature is 35 DEG C, power 600W, continues to cross 300 mesh screens in dispersion 0.5 hour, obtains slurry.
Slurry is taken to carry out the test of granularity, contact angle, current potential, rheological property, test result respectively according to the step in Fig. 1
It is shown in Table 1.
It defines indices score value and is followed successively by 3 points from high in the end, 2 points, 1 point, granularity, contact angle, current potential, rheometer test account for
It is followed successively by 30%, 30%, 20%, 20% than weight, according to the test result in table 1, it can be seen that the comprehensive performance of slurry is real
It applies example 1 and is relatively better than embodiment 3 better than embodiment 2, embodiment 1 and embodiment 2, the results showed that the evaluation method in the present invention can
Quickly test evaluates the comprehensive performance of diaphragm slurry, easy to operate, and test result reliability is high, and practicability is stronger, can be with
The application for being diaphragm coating slurry under different technology conditions provides accurate reference.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. a kind of lithium ion battery separator coating size performance evaluation method, which comprises the following steps:
Testing graininess is carried out with slurry to coating, the dispersion of the coating slurry is judged according to testing graininess result and dispersion degree
Property；
Contact angle test is carried out with slurry to coating, the coating slurry and coating substrate are judged according to contact angle test result
Between levelability and wellability；
Potential test is carried out with slurry to coating, the stability of the coating slurry is judged according to potential value test result；
Rheometer test is carried out with slurry to coating, it is viscous according to the coating slurry viscosity and shear rate, the coating paste
Degree and time changing curve judge the viscosity and rheological characteristic of slurry；
It is set according to coating slurry items test result standards of grading or grade, is carried out in conjunction with the default weight of items test
Adduction, obtains the comprehensive performance of coating slurry.
2. lithium ion battery separator coating size performance evaluation method as described in claim 1, which is characterized in that the grain
Degree test use laser particle analyzer, test D10, D50 and D90 of the coating slurry respectively, by (D90-D10)/
The span R of D50 calculating slurry.
3. lithium ion battery separator coating size performance evaluation method as described in claim 1, which is characterized in that described to connect
Feeler test is measured by contact angle tester using amount supreme people's court, and fluid injection uses impregnator drop capillary in measurement process, surveys
It tries substrate and selects diaphragm face to be tested.
4. lithium ion battery separator coating size performance evaluation method as claimed in claim 3, which is characterized in that it is described to
It tests diaphragm face and is selected from one of PP basement membrane, PE basement membrane, aluminium oxide ceramics diaphragm, boehmite ceramic diaphragm, gluing diaphragm.
5. lithium ion battery separator coating size performance evaluation method as described in claim 1, which is characterized in that the electricity
Bit test use Zeta potential analysis instrument, wherein the Zeta potential range of the Zeta potential analyzer be -150mV ~
150mV, particle size range are 10nm ~ 30 μm, and conductivity range is 0 ~ 200mS/cm, and measurement angle is 90 °, and temperature range is 2 ~ 90
℃。
6. lithium ion battery separator coating size performance evaluation method as described in claim 1, which is characterized in that the stream
Become test and use rotational rheometer, it is the disk plate torque of 35mm, alternation formula shearing speed that the rotational rheometer, which selects diameter,
Rate is 1 ~ 300S-1, shearing force is 1 ~ 300Pa, shear time 100s ~ 200s.
7. lithium ion battery separator coating size performance evaluation method as described in claim 1, which is characterized in that described each
Item test result standards of grading are to be followed successively by 3 points, 2 points, 1 point from high in the end, and the default weight of every test is granularity
30%, contact angle 30%, current potential 20%, rheology 20%.
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| CN111811920A (en) * | 2020-07-24 | 2020-10-23 | 天津市捷威动力工业有限公司 | Method for detecting dispersion uniformity and stability of slurry |
| CN112525771A (en) * | 2020-11-30 | 2021-03-19 | 湖北亿纬动力有限公司 | Battery slurry storage performance evaluation method |
| CN113008942A (en) * | 2021-03-04 | 2021-06-22 | 上海恩捷新材料科技有限公司 | Method and system for detecting dispersibility of coating film coating slurry |
| CN114184523A (en) * | 2022-02-14 | 2022-03-15 | 徐州钛白化工有限责任公司 | Method for detecting titanium dioxide dispersibility |
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