CN106896271A - A kind of apparatus and method for the test of battery diaphragm electrical conductivity - Google Patents
A kind of apparatus and method for the test of battery diaphragm electrical conductivity Download PDFInfo
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- CN106896271A CN106896271A CN201710141631.9A CN201710141631A CN106896271A CN 106896271 A CN106896271 A CN 106896271A CN 201710141631 A CN201710141631 A CN 201710141631A CN 106896271 A CN106896271 A CN 106896271A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
This application discloses a kind of apparatus and method for the test of battery diaphragm electrical conductivity.The device of the application, including conductance cell housing, conductance cell lid, septum clip and conductivity meter；Conductance cell housing is barrel-shaped in one end open cylinder, and bottom interior surface has the first circular electric electric conduction electrode-plate, and outer surface has the first electrode external tapping electrically connected with the first circular electric electric conduction electrode-plate；Two electrode external tappings are used to connect conductivity meter；Conductance cell lid is removably inserted and fixed to conductance cell shell nozzle end, and inner surface has the second circular electric electric conduction electrode-plate, and outer surface has the second electrode external tapping electrically connected with the second circular electric electric conduction electrode-plate；Conductance cell housing sidewall offers vacuum valve port and fluid injection valve port respectively；Septum clip is mutual buckle type circular ring structure, and septum clip external diameter is adapted to conductance cell housing inner diameter, and central coaxial parallel with two conductance electrode pieces.The device of the application, simple structure, operation is easy, accurately can conveniently measure the electrical conductivity and resistance of barrier film.
Description
Technical field
The application is related to lithium ion battery separator test equipment field, more particularly to a kind of to be used for battery diaphragm electrical conductivity
The apparatus and method of test.
Background technology
In recent years, the development of new energy is noticeable, particularly the high speed development of lithium ion battery, as new energy industry
In focus of concern.Lithium ion battery is made up of positive pole, negative pole, barrier film and the big critical material of electrolyte four, and barrier film is located at
Between both positive and negative polarity, buffer action is played, prevent the short circuit of both positive and negative polarity directly contact, there is permission ion to turn on and prevent electronic conduction
Microcellular structure；The microcellular structure of barrier film governs the ion conduction rate of lithium ion, and then directly affects the property of lithium ion battery
Energy.Therefore, barrier film ionic conductivity turns into one of important indicator of measurement membrane properties.
In existing method of testing, more accurately measuring method is the surface resistance of measuring diaphragm, and barrier film conductance is characterized with this
Rate.Specifically, barrier film to be tested to be struck out the sample strip of suitable size, and soaked with lithium-ion electrolyte in a sealed meter environment
Barrier film to be tested；After barrier film to be tested fully infiltrates, it is clamped between two battery lead plates, and two battery lead plates is placed in lithium ion
In electrolyte；The resistance value tested between two battery lead plates, by the resistance value retouch abscissa be the barrier film number of plies, ordinate be resistance
On the coordinate system correspondence position of value；Superposition two-layer barrier film test resistance value to be tested, and gained resistance value is retouched in coordinate system pair
Answer on position；It is superimposed one layer of barrier film to be tested every time according to above-mentioned steps to be tested, and at least tests four layers of barrier film to be tested
The resistance value of superposition, and respectively retouch on coordinate system correspondence position all resistance values that measure；Coordinates computed is fastened all discrete
Point Linear Quasi is right and slope, if the Linear Quasi of all discrete points is right to be more than 0.999, by its slope substitute into formula R '=
In k × S, wherein k is slope, and S is the area of smaller clamping face, if two clamping face sizes are identical, S is the face of any clamping face
Product, R ' is the barrier film surface resistance obtained by calculating.Electrical conductivity can further be calculated by surface resistance, or directly use face
Resistance characterization ion conduction rate.
Above method, operate it is complex, it is necessary to test at least four layers resistance value of barrier film respectively, by one layer, two-layer,
Three layers and four layers of resistance value could good fit outlet linearity curve, calculating gained barrier film surface resistance；Testing time is more, operation
Process is complicated, and time-consuming for test, and testing efficiency is relatively low；It is required and test four times or more times is, it is necessary to barrier film sample size is more
Result is also the average value of polylith sample barrier film surface resistance.
The content of the invention
The purpose of the application is to provide a kind of new apparatus and method for the test of battery diaphragm electrical conductivity.
To achieve these goals, the application employs following technical scheme：
The one side of the application discloses a kind of device for the test of battery diaphragm electrical conductivity, and the device includes conductance cell
Housing 1, conductance cell lid 2, septum clip 4 and conductivity meter 5；Conductance cell housing 1 is in the cylinder barrel shaped structure of one end open, conductance
In pond housing 1, its bottom has the first circular electric electric conduction electrode-plate 11, and the outer surface of the bottom of conductance cell housing 1 has first electrode
External tapping 111, first electrode external tapping 111 is connected with the wire of the first circular electric electric conduction electrode-plate 11；Conductance cell lid 2 is removably solid
Due to the cavity for forming relative closure in the openend of conductance cell housing 1, the insertion conductance cell of conductance cell lid 2 housing 1 therewith, conductance
The outer surface that the inner surface of pond lid 2 has the second circular electric electric conduction electrode-plate 21, conductance cell lid 2 has and the second circular conductance electrode
The second electrode external tapping 211 of the wire of piece 21 connection；Conductance cell lid 2 is fixed on when in conductance cell housing 1, and the first circular electric is conductive
Pole piece 11 is parallel to each other with the second circular electric electric conduction electrode-plate 21, and both centers are on the same axis；On the side wall of conductance cell housing 1
The vacuum valve port 12 and fluid injection valve port 13 that the internal cavities of conductance cell housing 1 are in communication with the outside, vacuum valve port 12 are offered respectively
For connecting vacuumizing assembly, fluid injection valve port 13 is used to connect electrolyte solution injection component；Pass through two when conductivity meter 5 is used
Bar wire 31 and 32 is electrically connected with first electrode external tapping 111 and second electrode external tapping 211 respectively；Septum clip 4 is mutual button
Formula circular ring structure, the external diameter of septum clip 4 is adapted with the internal diameter of conductance cell housing 1, and the internal diameter of septum clip 4 is more than or equal to
Larger area in first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21；Also, when using, septum clip 4
Be parallel to each other with the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21, and three center in same axis
On.
Wherein, the external diameter of septum clip 4 is adapted with the internal diameter of conductance cell housing 1, refers to that when using, septum clip 4 is put
Entering conductance cell housing 1 can just slide, and allow electrolyte solution to be flowed through by both spaces.It is appreciated that septum clip 4
To have just need when in use and be put into conductance cell housing 1, likewise, only just needing to be connected with conductivity meter 5 when in use.
It should be noted that the battery diaphragm electric conductivity test device of the application, particular for the electrical conductivity of battery diaphragm
Test and design, using the device of the application, according to the special testing method that the application is designed, can simply obtain very much battery
The electrical conductivity of barrier film, without carrying out linear fit, without being successively superimposed test to laminated diaphragm respectively.
Preferably, between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 distance be 0.50mm~
5.00mm, preferably 0.50mm~1.00mm.
It should be noted that distance is mainly examined between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21
The factor of worry is the manufacturability and measurement accuracy of electric conductivity test device, and two distances of conductance electrode piece are more big easier
Manufacture, but, its distance is bigger, and the measuring result error of battery diaphragm is bigger.Therefore, the application limits the first circular electric conduction
Distance is 0.50mm~5.00mm between the circular electric electric conduction electrode-plate 21 of pole piece 11 and second, also, preferably 0.50mm~
The measurement accuracy of 1.00mm is higher.
Preferably, between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 distance by being arranged on electricity
The locating piece 14 led on the madial wall of pond housing 1 is fixed.
Preferably, the internal diameter of septum clip 4 is more than the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21.
It should be noted that the internal diameter of septum clip 4 is conductive more than the first circular electric electric conduction electrode-plate 11 or the second circular electric
Pole piece 21, its purpose is exactly so that the area of barrier film to be measured is more than two conductance electrode pieces because when test, be according to
The corresponding diaphragm area to be measured of two conductance electrode pieces is calculated, and the area of barrier film to be measured can be kept away more than two conductance electrode pieces
Exempt from that diaphragm edge to be measured is irregular or out-of-flatness is impacted to test result.Diaphragm area is more than two conductance electrode areas,
Can ensure that effective conductive diaphragm area is equal to conductance electrode area, it is convenient to calculate later；Diaphragm edge otherwise to be measured is not whole
Neat or out-of-flatness is impacted to test result.
Preferably, the surface of the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 is polished surface；Electricity
Lead pond lid 2 and conductance cell housing 1 is worked in coordination using fine thread and screws and outward winding.
It should be noted that two conductance electrode piece surfaces are polished surface, its purpose is to avoid rough surface shadow
Ring test result.
Preferably, conductance cell housing 1 is prepared by transparent material, and transparent material is preferably PET, PP, PVC, PC, PS and ABS
In at least one.
It should be noted that preparing conductance cell housing 1 or other components using transparent material, in order to convenient range estimation
Situation inside observation conductance cell housing 1.
Preferably, the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 are all platinum black electrode pieces.
It should be noted that platinum black electrode is electrode commonly used in the art, it will be understood that needed in some Special uses
In asking, however not excluded that can be using the conductance electrode piece of other materials.
The another side of the application discloses a kind of method for the test of battery diaphragm electrical conductivity, including using the application's
Device distinguishes the ionic conductivity K of blank testing electrolyte solution1With the ionic conductivity of the electrolyte solution containing barrier film to be measured
K2, and the electrical conductivity of barrier film to be measured is calculated according to formula one；
The K of formula oneBarrier film=d × K1×K2/(L×(K1-K2))
In formula, KBarrier filmIt is the electrical conductivity of barrier film to be measured, d is the thickness of barrier film to be measured, and L is the first circular electric electric conduction electrode-plate 11
The distance between with the second circular electric electric conduction electrode-plate 21, K1It is the ionic conductivity of blank electrolyte solution, K2It is containing barrier film to be measured
Electrolyte solution ionic conductivity.
It should be noted that the formula one of the application is actually according to ionic conductivity computing formula K=Q/R derivations
Come, wherein K is ionic conductivity, Q is conductance electrode constant, and R is resistance.Specific derivation process is as follows：
The ionic conductivity K of blank electrolyte solution1=Q/R1, R1It is blank electrolyte solution resistance；
The ionic conductivity K of the electrolyte solution containing barrier film to be measured2=Q/R2, R2It is the electrolyte solution containing barrier film to be measured
Resistance；
The electrical conductivity K of barrier film to be measuredBarrier film=QBarrier film/RBarrier film, QBarrier filmIt is barrier film conductance electrode constant, RBarrier filmIt is membrane electrical resistance；
And the resistance that the resistance for containing the electrolyte solution of barrier film to be measured is equal to blank electrolyte solution adds membrane electrical resistance, i.e.,
R2=R1+RBarrier film, so as to derive RBarrier film=R2-R1；The formula of ionic conductivity is brought into wherein, that is, obtains equation below：
RBarrier film=R2-R1=Q/K2-Q/K1=Q × (1/K2-1/K1)=Q × (K1-K2)/(K1×K2),
Therefore, KBarrier film=(QBarrier film×K1×K2)/(Q×(K1-K2))；
For a specific battery diaphragm electric conductivity test device of the application, its value is conductance electrode constant Q
Fixed, being calculated according to Q=L/A, wherein L is between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21
Distance, A is the area of area smaller in the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21, both areas
It is exactly the area of any one circular electric electric conduction electrode-plate when equal.Barrier film conductance electrode constant QBarrier film=d/ABarrier film, wherein, d be every
Film thickness, ABarrier filmIt is the effective conductive area of barrier film, the structure design of the electric conductivity test device according to the application, ABarrier film=A.Will
QBarrier filmIn the Conductivity formula that Q brings barrier film to be measured into, that is, obtain equation below：
KBarrier film=(QBarrier film×K1×K2)/(Q×(K1-K2))=d × K1×K2/(L×(K1-K2)), i.e. formula one.
Preferably, the present processes, also including calculating the resistance of barrier film to be measured according to formula two；
The R of formula twoBarrier film=Q × (K1-K2)/(K1×K2)
In formula, RBarrier filmIt is the resistance of barrier film to be measured, Q is conductance electrode constant.
It should be noted that conductance electrode constant Q is for one of the application specific battery diaphragm electrical conductivity test dress
For putting, its value is fixed, is calculated according to Q=L/A, and wherein L is the first circular electric electric conduction electrode-plate 11 and the second circular conductance
The distance between electrode slice 21, A is area smaller in the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21
Area, be exactly the area of any one circular electric electric conduction electrode-plate during both area equations.
Also, it should be noted that RBarrier filmIt is the resistance of barrier film to be measured, barrier film surface resistance=membrane electrical resistance × diaphragm area, i.e.,
Barrier film surface resistance=RBarrier film×A.Therefore, R is obtained according to the present processesBarrier filmAfterwards, barrier film surface resistance can be as needed calculated,
It is not specifically limited herein.
Preferably, in the present processes, the ionic conductivity K of blank electrolyte solution1With the electrolysis containing barrier film to be measured
The ionic conductivity K of matter solution2Test it is specific as follows, moisture be less than 20PPM, 25 DEG C ± 2 DEG C of temperature in the environment of,
Conductance cell lid 2 is tightened and fluid injection valve port 13 is closed, vacuum valve port 12 is connected with vacuum subassembly, conductance cell housing 1 is carried out
Vacuumize, until vacuum is less than -95KPa, close vacuum valve port 12, then connect fluid injection valve port 13 and electrolyte injecting assembly
Connect, conductance cell housing 1 is filled into electrolyte solution, then close fluid injection valve port 13, ion now is tested by conductivity meter 5
The ionic conductivity K of electrical conductivity, i.e. blank electrolyte solution1；Barrier film to be measured is punched or is cut into suitable septum clip 4
Size, barrier film to be measured is put into septum clip 4, it is ensured that barrier film is smooth, corrugationless, without breakage, by be placed with barrier film to be measured every
Film fixture 4 is put into conductance cell housing 1, tightens conductance cell lid 2, according to the ionic conductivity K of blank electrolyte solution1Test
Method, vacuumizes and fills identical electrolyte solution, measures ionic conductivity after standing at least 2 hours, i.e., containing barrier film to be measured
Electrolyte solution ionic conductivity K2。
Wherein, refer to treating of being punched or cut by the size that barrier film to be measured was punched or was cut into suitable septum clip 4
Survey barrier film size just can be complete loading septum clip 4 in, the inner ring of septum clip 4 is taken, and do not have it is unnecessary
Barrier film stretches out the outer shroud of septum clip 4.
Because the beneficial effect using above technical scheme, the application is：
The device for the test of battery diaphragm electrical conductivity of the application, simple structure, operation is easy, can accurately facilitate
The electrical conductivity and resistance that measure battery diaphragm.The present processes using the application device, can it is simple, convenient, quick,
Accurately measure the electrical conductivity and resistance for calculating battery diaphragm.
Brief description of the drawings
Fig. 1 is the structural representation of the device for the test of battery diaphragm electrical conductivity in the embodiment of the present application；
Fig. 2 is that the structure installed after septum clip for the device of battery diaphragm electrical conductivity test in the embodiment of the present application is shown
It is intended to.
Specific embodiment
The application is described in further detail below by specific embodiments and the drawings.Following examples are only to the application
It is further described, should not be construed as the limitation to the application.
Embodiment
The battery diaphragm electric conductivity test device of this example, as shown in figure 1, including conductance cell housing 1, conductance cell lid 2, barrier film
Fixture 4 and conductivity meter 5.
Conductance cell housing 1 is in the cylinder barrel shaped structure of one end open, and in conductance cell housing 1, its bottom has the first circle
Conductance electrode piece 11, the outer surface of the bottom of conductance cell housing 1 has a first electrode external tapping 111, first electrode external tapping 111 with
The wire of first circular electric electric conduction electrode-plate 11 is connected；Conductance cell lid 2 opens the openend for being fixed on conductance cell housing 1 unloaded, conductance
The cavity of relative closure is formed in the insertion conductance cell of pond lid 2 housing 1 therewith, the inner surface of conductance cell lid 2 has the second circular electric
Electric conduction electrode-plate 21, the outer surface of conductance cell lid 2 is with external with the second electrode that the wire of the second circular electric electric conduction electrode-plate 21 is connected
Mouth 211；Conductance cell lid 2 is fixed on when in conductance cell housing 1, the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate
21 are parallel to each other, and on the same axis, and distance between the two is fixed as 0.50mm~5.00mm at both centers；Conductance cell shell
The vacuum valve port 12 and fluid injection valve port 13 that the internal cavities of conductance cell housing 1 are in communication with the outside are offered on the side wall of body 1 respectively,
Vacuum valve port 12 is used to connect vacuumizing assembly, and fluid injection valve port 13 is used to connect electrolyte injecting assembly；When conductivity meter 5 is used
Electrically connected with first electrode external tapping 111 and second electrode external tapping 211 respectively by two wires 31 and 32；Septum clip 4
It is mutual buckle type circular ring structure, the external diameter of septum clip 4 is adapted with the internal diameter of conductance cell housing 1, and the internal diameter of septum clip 4 is more than
Or equal to larger area in the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21；Also, when using, such as scheme
Shown in 2, septum clip 4 is parallel to each other with the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21, and three
Center is on the same axis.
In the battery diaphragm electric conductivity test device of this example, the first circular electric electric conduction electrode-plate 11 and the second circular conductance electrode
Piece 21 is all platinum black electrode piece, also, the surface of the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 is throwing
Optical surface.Both first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 area equations, are area A, also,
The internal diameter of septum clip 4 is more than the first circular electric electric conduction electrode-plate 11 or the second circular electric electric conduction electrode-plate 21.
Conductance cell lid 2 and conductance cell housing 1 are worked in coordination using fine thread and screw and outward winding, the first circular conductance electrode
Distance is consolidated by the locating piece 14 being arranged on the madial wall of conductance cell housing 1 between the circular electric electric conduction electrode-plate 21 of piece 11 and second
Fixed, locating piece 14 can limit the precession depth of conductance cell lid 2.Locating piece 14 is the machine on the inwall of conductance cell shell 1
Tool locating piece, it is ensured that conductance cell lid 2 after tightening, between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21
Spacing be fixed as L.Then conductance electrode constant Q=L/A.
Conductance cell housing 1 is prepared by transparent material, such as PET, PP, PVC, PC, PS or ABS, and this example is specifically using saturating
Bright PET material prepares conductance cell housing 1.Using transparent plastic as shell, whether can be full of with clear view electrolyte solution
Conductance cell inner chamber.
The septum clip 4 of this example is in annular, is mutual buckle type plastic clamp, and material is PET, PP, PVC, PC, PS or ABS,
This example specifically uses PP materials.Before test, barrier film need to be punched or is cut into the circular sample piece of suitable size, be put into
In septum clip 4 and clamp, it is ensured that barrier film is smooth, corrugationless, without breakage.Furthermore, it is desirable to ensure diaphragm area more than platinum black electricity
The area A of conductive electrode, this example is specifically about 2cm using diaphragm area2。
The battery diaphragm electric conductivity test device simple structure of this example, it is with low cost, remove and install easily, it is easy to operate.
Using the battery diaphragm electric conductivity test device of this example, this example provides a kind of method of testing of battery diaphragm electrical conductivity, including
Device using this example distinguishes the ionic conductivity K of blank testing electrolyte solution1With the electrolyte solution containing barrier film to be measured
Ionic conductivity K2, and the electrical conductivity of barrier film to be measured is calculated according to formula one；
The K of formula oneBarrier film=d × K1×K2/(L×(K1-K2))
In formula, KBarrier filmIt is the electrical conductivity of barrier film to be measured, d is the thickness of barrier film to be measured, and L is the first circular electric electric conduction electrode-plate 11
The distance between with the second circular electric electric conduction electrode-plate 21, K1It is the ionic conductivity of blank electrolyte solution, K2It is containing barrier film to be measured
Electrolyte solution ionic conductivity.
Also, the resistance of barrier film to be measured can also be calculated according to formula two；
The R of formula twoBarrier film=Q × (K1-K2)/(K1×K2)
In formula, RBarrier filmIt is the resistance of barrier film to be measured, Q is conductance electrode constant.
Wherein, the ionic conductivity K of blank electrolyte solution1With the ionic conductivity of the electrolyte solution containing barrier film to be measured
K2Test it is specific as follows：
The conductance cell housing 1 and conductance cell lid 2 of the transparent PET plastics after cleaning-drying are screwed, and by outside first electrode
Interface 111 and second electrode external tapping 211 connect conductivity meter 5 using wire 31 and 32, place a device into moisture small
In in 20PPM, the dry glove box of 25 DEG C ± 2 DEG C of temperature；Vacuum valve port 12 is connected with vacuumizing assembly, fluid injection valve port 13 with electricity
The injecting assembly connection of solution liquid；First keep fluid injection valve port 13 to close, open vacuum valve port 12, be evacuated to very by vacuum valve port 12
Closed after reciprocal of duty cycle ＜ -95KPa, the injection electrolyte solution of fluid injection valve port 13 is then opened again, note is closed after filling electrolyte solution
Liquid valve port 13；Ionic conductivity now, i.e. the ionic conductivity K of blank electrolyte solution are tested by conductivity meter 51。
The ionic conductivity K of blank electrolyte solution1After being completed, conductance cell lid 2 is turned on, pour out electrolyte solution；
Barrier film to be measured is punched or is cut into area about 2cm2Circular sample piece, be put into the barrier film of annular mutual buckle type PP plastics
In fixture 4 clamp, it is ensured that barrier film is smooth, corrugationless, without breakage；Septate septum clip 4 will be clamped and be put into conductance cell housing 1
It is interior, cover conductance cell lid 2 and screw, moisture is placed a device into less than 20PPM, the dry glove box of 25 DEG C ± 2 DEG C of temperature
It is interior；Vacuum valve port 12 is opened, vacuum valve port 12 is closed after vacuum valve port 12 is evacuated to vacuum ＜ -95KPa, then beaten
The injection electrolyte solution of fluid injection valve port 13 is opened, fluid injection valve port 13 is closed after filling electrolyte solution；Start measurement after standing 2 hours
The ionic conductivity K of the solution of matter containing diaphragm electrolysis2。
After being completed, conductivity meter 5 is removed, turns on conductance cell lid 2, pour out electrolyte solution, take out septum clip 4,
Conductance cell housing 1, conductance cell lid 2 and septum clip 4 are cleaned up, and is put into vacuum drying chamber drying in case test next time makes
With.
In order to ensure test result, this example further, three tests has been carried out to barrier film of the same race, and require three surveys
The relative extreme difference of test result is no more than 3%, finally takes each average value of test gained barrier film electrical conductivity, and the average value is set to
The electrical conductivity of this barrier film.
On the basis of more than, this example in battery diaphragm electric conductivity test device, the first circular electric electric conduction electrode-plate 11 and
Two circular electric electric conduction electrode-plates 21 apart from L, and the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 face
Product A, the influence to device and test result is tested.Specifically, devising a series of different spacing L and platinum black electrode
The battery diaphragm electric conductivity test device of piece different area A, as shown in table 1.Also, use a series of battery diaphragm electrical conductivity
Test device is respectively that the battery diaphragm of 16 μm, 20 μm, 25 μm three specifications is tested to membrane thicknesses, in each experiment
Barrier film to being tested has carried out three retests respectively, battery diaphragm punching or will be cut into three size identicals circle
Shape sample carries out three retests, and the battery diaphragm of this example is all the microporous polypropylene membrane of dry method simple tension, and porosity is
36%~42%, be respectively ZM16 barrier films, the ZM20 barrier films that thickness is 20 μm that thickness is 16 μm, the ZD25 that thickness is 25 μm every
Film.Test result is as shown in table 1.
Measurement result of the conductance electrode piece of the different area of table 1 under different spacing
In table 1, five battery diaphragm electric conductivity test devices are devised, each device is 16 μm, 20 μm or 25 μ to thickness
The battery diaphragm of m is tested.Wherein, d is the thickness of barrier film to be measured, and unit is micron；L is the first circular electric electric conduction electrode-plate
11 and second the distance between the circular electric electric conduction electrode-plate 21, unit is millimeter；A is the area of circular electric electric conduction electrode-plate, and unit is
Square centimeter；Q is conductance electrode constant, and unit is cm-1；K1It is the ionic conductivity of blank electrolyte solution, unit is mS/
cm；K2It is the ionic conductivity of the electrolyte solution containing barrier film to be measured, unit is mS/cm；RBarrier filmIt is the resistance of barrier film to be measured, it is single
Position is Ω；KBarrier filmIt is the electrical conductivity of barrier film to be measured, unit is mS/cm.
The apparatus and method that this example is can be seen that from the test data of table 1, can easily and accurately test membrane electrical resistance
With barrier film electrical conductivity.And, it is preferable that the distance between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21
During for 0.50~1.00mm, the test of barrier film electrical conductivity is more accurate, and test error is smaller；Certainly, if for result accuracy
It is required that in the case of poor, it would however also be possible to employ between the first circular electric electric conduction electrode-plate 11 and the second circular electric electric conduction electrode-plate 21 away from
From more than 1.00mm, and it is less than or equal to the battery diaphragm electric conductivity test device of 5.00mm.
Above content is to combine the further description that specific embodiment is made to the application, it is impossible to assert this Shen
Specific implementation please is confined to these explanations.For the application person of an ordinary skill in the technical field, do not taking off
On the premise of conceiving from the application, some simple deduction or replace can also be made, should all be considered as belonging to the protection of the application
Scope.
Claims (10)
1. it is a kind of for battery diaphragm electrical conductivity test device, it is characterised in that：Including conductance cell housing (1), conductance cell lid
(2), septum clip (4) and conductivity meter (5)；
The conductance cell housing (1) in one end open cylinder barrel shaped structure, in conductance cell housing (1), its bottom has first
Circular electric electric conduction electrode-plate (11), the outer surface of conductance cell housing (1) bottom has first electrode external tapping (111), first electrode
External tapping (111) is connected with first circular electric electric conduction electrode-plate (11) wire；
The conductance cell lid (2) is detachably secured to the openend of the conductance cell housing (1), conductance cell lid (2) insertion electricity
The cavity for forming relative closure in pond housing (1) therewith is led, the inner surface of the conductance cell lid (2) has the second circular electric conductive
Pole piece (21), the outer surface of conductance cell lid (2) has the second electricity being connected with the second circular electric electric conduction electrode-plate (21) wire
Pole external tapping (211)；
Conductance cell lid (2) be fixed on conductance cell housing (1) it is interior when, the first circular electric electric conduction electrode-plate (11) and the second circular electric are conductive
Pole piece (21) is parallel to each other, and both centers are on the same axis；
Offered respectively on the side wall of the conductance cell housing (1) by conductance cell housing (1) internal cavities be in communication with the outside it is true
Empty valve port (12) and fluid injection valve port (13), the vacuum valve port (12) is for connecting vacuumizing assembly, the fluid injection valve port (13)
For connecting electrolyte solution injection component；
The conductivity meter (5), when using by two wires (31 and 32) respectively with the first electrode external tapping (111) and
Second electrode external tapping (211) electrical connection；
The septum clip (4) is mutual buckle type circular ring structure, and the external diameter of septum clip (4) is interior with the conductance cell housing (1)
Footpath is adapted, and the internal diameter of septum clip (4) is more than or equal to the first circular electric electric conduction electrode-plate (11) and second circle
Larger area in conductance electrode piece (21)；Also, when using, septum clip (4) and the first circular electric electric conduction electrode-plate (11) and
Second circular electric electric conduction electrode-plate (21) is parallel to each other, and three center on the same axis.
2. device according to claim 1, it is characterised in that：The first circular electric electric conduction electrode-plate (11) and described second
Distance is 0.50mm~5.00mm, preferably 0.50mm~1.00mm between circular electric electric conduction electrode-plate (21).
3. device according to claim 1, it is characterised in that：The first circular electric electric conduction electrode-plate (11) and described second
Distance is solid by the locating piece (14) being arranged on conductance cell housing (1) madial wall between circular electric electric conduction electrode-plate (21)
It is fixed.
4. the device according to claim 1-3, it is characterised in that：The internal diameter of the septum clip (4) is circular more than first
Conductance electrode piece (11) and the second circular electric electric conduction electrode-plate (21).
5. the device according to claim 1-3, it is characterised in that：The first circular electric electric conduction electrode-plate (11) and described
The surface of two circular electric electric conduction electrode-plates (21) is polished surface；The conductance cell lid (2) and the conductance cell housing (1) are using thin
Pitch thread is worked in coordination and screws and outward winding.
6. the device according to claim 1-3, it is characterised in that：The conductance cell housing (1) is prepared by transparent material, institute
State at least one in transparent material preferably PET, PP, PVC, PC, PS and ABS.
7. the device according to claim 1-3, it is characterised in that：The first circular electric electric conduction electrode-plate (11) and described
Two circular electric electric conduction electrode-plates (21) are all platinum black electrode pieces.
8. it is a kind of for battery diaphragm electrical conductivity test method, it is characterised in that：Including using any one of claim 1-8 institute
The device stated distinguishes the ionic conductivity K of blank testing electrolyte solution1With the ion-conductance of the electrolyte solution containing barrier film to be measured
Conductance K2, and the electrical conductivity of barrier film to be measured is calculated according to formula one；
The K of formula oneBarrier film=d × K1×K2/(L×(K1-K2))
In formula, KBarrier filmBe the electrical conductivity of barrier film to be measured, d is the thickness of barrier film to be measured, L be the first circular electric electric conduction electrode-plate (11) with
The distance between second circular electric electric conduction electrode-plate (21), K1It is the ionic conductivity of blank electrolyte solution, K2It is containing barrier film to be measured
Electrolyte solution ionic conductivity.
9. method according to claim 8, it is characterised in that：Also include being calculated according to formula two resistance of barrier film to be measured；
The R of formula twoBarrier film=Q × (K1-K2)/(K1×K2)
In formula, RBarrier filmIt is the resistance of barrier film to be measured, Q is conductance electrode constant.
10. method according to claim 8 or claim 9, it is characterised in that：The ionic conductivity K of blank electrolyte solution1With contain
The ionic conductivity K of the electrolyte solution of barrier film to be measured2Test it is specific as follows,
In the environment of moisture is less than 20PPM, 25 DEG C ± 2 DEG C of temperature, conductance cell lid (2) is tightened and fluid injection valve port is closed
(13), vacuum valve port (12) is connected with vacuum subassembly, conductance cell housing (1) is vacuumized, until vacuum less than-
95KPa, closes vacuum valve port (12), then fluid injection valve port (13) is connected with electrolyte solution injection component, by conductance cell shell
Body (1) fills electrolyte solution, then closes fluid injection valve port (13), by conductivity meter (5) test ionic conductivity now,
That is the ionic conductivity K of blank electrolyte solution1；
Barrier film to be measured is punched or is cut into the size of suitable septum clip (4), barrier film to be measured is put into septum clip (4)
In, it is ensured that barrier film is smooth, corrugationless, without breakage, the septum clip (4) of barrier film to be measured will be placed with and is put into conductance cell housing (1),
Conductance cell lid (2) is tightened, according to the ionic conductivity K of blank electrolyte solution1Method of testing, vacuumize and fill identical
Electrolyte solution, measures ionic conductivity, i.e., the ionic conductivity of the electrolyte solution containing barrier film to be measured after standing at least 2 hours
K2。
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| CN108303442A (en) * | 2017-12-18 | 2018-07-20 | 合肥国轩高科动力能源有限公司 | A kind of diaphragm closed pore temperature test method |
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| CN109031128A (en) * | 2018-05-18 | 2018-12-18 | 上海恩捷新材料科技股份有限公司 | A method of test battery diaphragm resistance |
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