CN108760827A - A kind of device and method of testing size electric conductivity - Google Patents
A kind of device and method of testing size electric conductivity Download PDFInfo
- Publication number
- CN108760827A CN108760827A CN201810774633.6A CN201810774633A CN108760827A CN 108760827 A CN108760827 A CN 108760827A CN 201810774633 A CN201810774633 A CN 201810774633A CN 108760827 A CN108760827 A CN 108760827A
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- slurry
- sealing container
- electric conductivity
- resistance
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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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
Abstract
The present invention discloses a kind of device and method of testing size electric conductivity, which includes：Sealing container with upper cover, the magnetic stirring apparatus being placed on the outside of sealing container bottom, the stirring rotator being placed in sealing container, the miniature vacuum pumping pump being connected to sealing container, two conductive current collectors being placed in sealing container bottom, the instrument for measuring DC resistance being electrically connected with two conductive current collectors, the infrared temperature measurement and control instrument for detecting sealed container interior temperature, the feeding mechanism and discharging mechanism being connected to sealing container.The present invention directly can carry out resistance test to slurry, and then judge dispersibility and electric conductivity；The method can also directly configure the different solid electrocondution slurries containing under simultaneously, do not needing large-scale mixing plant to be stirred, saving material；It, to the influence of electric conductivity, can also judge the stability of slurry from the identical slurry contained admittedly is clear that in data under different time and different temperatures, improve the accuracy evaluated to slurry electric conductivity, improve work efficiency.
Description
Technical field
The present invention relates to electrochemical technology field, more particularly to a kind of device and method of testing size electric conductivity, this hair
Bright test device and method is mainly used in the test and appraisal of pulp of lithium ion battery electric conductivity.
Background technology
In existing lithium battery, the main test resistance rate of test of slurry electric conductivity, resistivity is reflection materials conductive performance
One of important parameter.There are many method of measured resistivity, and four probe method is a kind of widely used standard method.Its advantages of
It is that equipment is simple and convenient to operate, accuracy is high, to the shape of sample without strict demand.
The most commonly used is four probes of linear type.On the same line, and spacing is equal, is all S for the needle point of four probes,
The general spacing for using 0.5mm, different probe spacings need to do corresponding correction to measurement result.
However it has the following problems when being used for the test of slurry：
(1), it is only capable of judging its electric conductivity and distribution by testing the dried pole piece of coating, it cannot be in time to slurry
The electric conductivity of material makes accurate judgement；
(2), four traditional probe test methods need replacement probe repeatedly and sample test position, hinder test effect
The promotion of rate.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of device and method of testing size electric conductivity, this hair
Bright to avoid the problem of traditional four probes directly replace probe to grout material resistivity measurement and repeatedly, it is directly right to realize
The quick test of slurry conductive material.
To achieve the above object, present invention firstly provides a kind of devices of testing size electric conductivity, including：With the close of upper cover
Envelope container, the magnetic stirring apparatus being placed on the outside of sealing container bottom, the stirring rotator being placed in sealing container and sealing container connect
Logical miniature vacuum pumping pump, two conductive current collectors being placed in sealing container bottom, be electrically connected with two conductive current collectors it is straight
Leakage resistance tester, the infrared temperature measurement and control instrument for detecting sealed container interior temperature, the feeding mechanism that is connected to sealing container and
Discharging mechanism.
Preferably, each conductive current collector is a copper coin, is equipped with several grooves linearly arranged at the top of the copper coin, often
A pair of U row spring interfaces are equipped in one groove, the connecting line of double U rows spring interfaces and instrument for measuring DC resistance 9 matches.
Preferably, the feeding mechanism includes a funnel, the sebific duct for being connected to funnel and sealing container, is arranged on sebific duct
First manual valve.
Preferably, the discharging mechanism includes a discharge nozzle and the second manual valve being arranged on discharge nozzle.
Preferably, the upper lid of the sealing container is equipped with a vacuum tube screwed union, through a vacuum-pumping tube and miniature pumping
Vacuum pump connects.
The present invention also provides the test method of above-mentioned apparatus, specific technical solution is as follows：
A kind of method of testing size electric conductivity, includes the following steps：
(1) prepared by slurry
According to the different solid electrocondution slurries containing under of the relationship of solution, solute, solvent configuration, the slurry of configuration is just full of whole
A test device；
(2) slurry electric conductivity is tested
Instrument for measuring DC resistance is opened, two conducting wires of instrument for measuring DC resistance are connected to two conductive current collectors respectively
Double U rows spring interfaces in groove；When testing the solid resistance value containing under of parallel point slurry difference and identical difference containing slurry admittedly
Between under slurry resistance variations situation, identical solid influence of the different temperatures containing slurry to slurry resistance pass through formula ρ=RS/L, σ
=1/ ρ calculates different solid resistivity and conductivity containing under, you can know slurry deployment conditions and slurry in different time and
Different temperatures and the Bu Tong solid electric conductivity containing under.
Preferably, the detailed process that prepared by step (1) slurry is as follows：
Upper cover 13 is opened, conductive agent dry powder is added in sealing container 12, dispersant is added in sealing container 12, solvent
It is added in sealing container 12 by funnel 1 and sebific duct 2, covers upper cover, be put on magnetic stirring apparatus 5, open magnetic stirring apparatus
5, rotating speed 1500rpm/s, stirring rotator 4 are stirred the substance in container, and stirring 4h is uniform to slurry dispersion mixing, i.e.,
It can terminate to stir, connect minipump 14, carry out vacuumizing 20min, remove the bubble in slurry, is prepared by electrocondution slurry
At.
Preferably, the test method that slurry difference contains admittedly in the step (2) is：
On the basis of initial slurry, part size is taken out, using carrying out calculating remaining ratio slurry by poor method, to container
Middle addition coordinative solvent or solution continue to stir to slurry after mixing, and vacuum pump line 15 and vacuum tube screwed union 16 are connect
It is good, it opens vacuum pump 14 and vacuumizes.
Existing technological means is the resistivity of traditional four probe method test material, and slurry is coated in insulating film
On, coating thickness is surveyed after drying, and the membrane impedance of electrode is surveyed with four probe method, according to THICKNESS CALCULATION resistivity, and then judges material
The electric conductivity of material, and when four probe method tests multiple sample different zones to be replaced probe and test repeatedly not
Same position, repeatedly replace probe and test position test period it is longer and to instrument be lost it is larger, while cannot to slurry into
Row is directly tested, and the loss of bigger is likely to result in normal production.
The present invention can directly solve the drawbacks of traditional four probe method cannot directly test electrocondution slurry, Ke Yizhi
It connects and resistance test is carried out to slurry, and then judge dispersibility and electric conductivity；The method can also directly configure difference and contain admittedly simultaneously
Under electrocondution slurry, do not needing large-scale mixing plant to be stirred, saving material；Phase can also be clear that from data
The stability of slurry is judged to the influence of electric conductivity under different time and different temperatures with the slurry that contains admittedly, is improved pair
The accuracy of slurry electric conductivity evaluation, improves work efficiency.
Description of the drawings
Fig. 1 is slurry test system structure figure of the present invention
Fig. 2 is conductive current collector structural schematic diagram in the present invention；
Fig. 3 is double-U-shaped spring interface structure schematic diagram in the present invention.
Specific implementation mode
Below in conjunction with the drawings and specific embodiments, the present invention is further described.
Shown in Fig. 3, present invention firstly provides a kind of devices of testing size electric conductivity, including：Band upper cover 13
Sealing container 12, the magnetic stirring apparatus 5 for being placed in 12 bottom outside of sealing container, the stirring rotator 4 being placed in sealing container 12,
The miniature vacuum pumping pump 14 that is connected to sealing container 12, two conductive current collectors 11 being placed in 12 bottom of sealing container are led with two
The infrared temperature measurement and control instrument 8 of instrument for measuring DC resistance 9, detection 12 internal temperature of sealing container that electrojet body 11 is electrically connected,
The feeding mechanism and discharging mechanism being connected to sealing container 12.
Wherein, each conductive current collector 11 is a copper coin, is equipped with several grooves linearly arranged at the top of the copper coin, often
A pair of U row spring interfaces are equipped in one groove, the connecting line of double U rows spring interfaces and instrument for measuring DC resistance 9 matches.Not
Interface is in closed state due to the elastic force of spring when test, and wire contact is inserted into test inside grooves when performing a test
When interface spring contraction under force, so that conducting wire is smoothly contacted with conductive current collector, the purpose of this interface is also to pass through bullet
Force effect allows conducting wire to be come into full contact with conductive current collector, can smoothly test the solid resistance value containing under of parallel point slurry difference and
Slurry resistance variations situation under identical solid different time containing slurry, shadow of the identical solid different temperatures containing slurry to slurry resistance
It rings.
The feeding mechanism includes a funnel 1, the sebific duct 2 for being connected to funnel 1 and sealing container 12, is arranged on sebific duct 2
First manual valve 3.
The discharging mechanism includes a discharge nozzle 7 and the second manual valve 3 being arranged on discharge nozzle 7.
The upper cover 13 of the sealing container 12 is equipped with a vacuum tube screwed union 16, through a vacuum-pumping tube 15 and miniature pumping
Vacuum pump 14 connects.
The present invention also provides a kind of methods of testing size electric conductivity, include the following steps：
(1) prepared by slurry
According to the different solid electrocondution slurries containing under of the relationship of solution, solute, solvent configuration, the slurry of configuration is just full of whole
A test device；
(2) slurry electric conductivity is tested
Instrument for measuring DC resistance is opened, two conducting wires of instrument for measuring DC resistance are connected to two conductive current collectors respectively
Double U rows spring interfaces in groove；When testing the solid resistance value containing under of parallel point slurry difference and identical difference containing slurry admittedly
Between under slurry resistance variations situation, identical solid influence of the different temperatures containing slurry to slurry resistance pass through formula ρ=RS/L, σ
=1/ ρ calculates different solid resistivity and conductivity containing under, you can know slurry deployment conditions and slurry in different time and
Different temperatures and the Bu Tong solid electric conductivity containing under.
Wherein, the detailed process that prepared by step (1) slurry is as follows：
Upper cover 13 is opened, conductive agent dry powder is added in sealing container 12, dispersant is added in sealing container 12, solvent
It is added in sealing container 12 by funnel 1 and DN15 sebific ducts 2, covers upper cover, be put on magnetic stirring apparatus 5, opened magnetic force and stir
Device 5, rotating speed 1500rpm/s are mixed, stirring rotator 4 is stirred the substance in container, and stirring 4h is equal to slurry dispersion mixing
It is even, you can to terminate stirring, connect minipump 14, carry out vacuumizing 20min, remove the bubble in slurry, electrocondution slurry system
It is standby to complete.
The test method that slurry difference contains admittedly in the step (2) is：
On the basis of initial slurry, part size is taken out, using carrying out calculating remaining ratio slurry by poor method, to container
Middle addition coordinative solvent or solution continue to stir to slurry after mixing, and vacuum pump line 15 and vacuum tube screwed union 16 are connect
It is good, it opens vacuum pump 14 and vacuumizes.
It is the specific operation of the present invention and test process below：
One, the preparation of electrocondution slurry：The different solid electrocondution slurries containing under are respectively configured using by poor method, specific ratio is as follows
Table 1：
Table 1
Embodiment 1
Fig. 1 container upper covers 13 are opened, conventional conductive agent dry powder is added in sealing container 12, sealing, which is added, in dispersant holds
In device 12, solvent be added in sealing container 12 by funnel 1 and DN15 sebific ducts 2 (sebific duct sectional area is 0.0177 square decimeter,
Flow velocity 0.1dm/s, i.e., addition solvent deionized water 10.62g per minute, the slurry solvent that 13.65min5% contains admittedly can be whole
It is added in sealing container), upper cover is covered, is put on magnetic stirring apparatus 5, magnetic stirring apparatus 5 is opened, rotating speed 1500rpm/s is stirred
It mixes rotor 4 to be stirred the substance in container, stirring 4h is uniform to slurry dispersion mixing, you can terminate stirring, connect true
Sky pump 14 vacuumizes the bubble in 20min removing slurries, and prepared by the 5% solid electrocondution slurry containing under completes；Consolidating for 4%-0.5% contains
Slurry is according to the corresponding slurry of taking-up is calculated in table 1, opening discharge valve 3 makes slurry just flow into beaker, with electronic balance 6
It carries out weighing its weight, the identical closing discharge port valve 3 of slurry weight, the amount of electronic balance is taken out until taking out and calculating every time
Journey is 0-3000g, and quantity of solvent to be added is added in precision 0.01g, closes agitating device after being stirred 15min, opens vacuum
Pump 14 vacuumizes 20min and can be obtained the uniformly mixed electrocondution slurry of following ratio.
Embodiment 2
Special conductive agent slurry how much can achieve the effect that due to not knowing specific addition and conventional electrocondution slurry 2%,
To select the ratio according to embodiment 1, admittedly containing being prepared, to obtain special electrocondution slurry from large arch dam toward low.
Two, slurry electric conductivity is tested
The test system shown in slurry combination Fig. 1 of whole container of just filling that (one) configures is connected into test device,
Instrument for measuring DC resistance 9 is opened, two conducting wires 10 of instrument for measuring DC resistance 9 are inserted into double-U-shaped contact point respectively, in spring
Conducting wire is set smoothly to be linked at the correspondence concave point of conductive current collector 11 under the action of power, and contact is more abundant, passes through infrared temperature
The degree test of measurement and control instrument 8 parallel 5 point differences in 25 ± 2 DEG C, the identical time consolidate the resistance change containing lower electrocondution slurry
Situation calculates different solid resistivity and conductivity containing under, you can know the dispersion of slurry by the ρ of formula ρ=RS/L, σ=1/
The electric conductivity of situation and the slurry slurry in identical same time, same temperature ranges stated.Instrument for measuring DC resistance range is 0-
200K Ω, precision 0.5%.
By the test result (being shown in Table 2) of embodiment 1 and embodiment 2 find, it is identical contain admittedly under special electrocondution slurry resistance
Respectively less than conventional electrocondution slurry；And by the method test data it has furthermore been found that conventional conductive agent resistance in dosage 2%
For 194 Ω, when the resistance of slurry containing when is 158 Ω to special conductive agent 2% admittedly, it is less than conventional electrocondution slurry；In order to which data are more straight
It sees obviously, increases test group, test special electrocondution slurry respectively and consolidate the resistance value containing under 1.8%, 1.6% and 1.4%,
By test it was found that when special electrocondution slurry is contained in 1.4% admittedly, slurry resistance is 190 Ω, with conventional electrocondution slurry base
This is consistent, and conductivity is not much different, and then terminates to test, obtain special electrocondution slurry 1.4% contain admittedly it is lower can reach with often
The effect for advising electrocondution slurry 2%, further demonstrates the test method that I is invented and can accurately be led with test device
Plasma-based material electric conductivity is tested；1.4% special electrocondution slurry is directly used in the normal dispensing of lithium battery, entire test process does not have
It is recycling to have waste, slurry.
Table 2
Three, slurry test method application
This method is used for testing size conductive agent electric conductivity in positive blending process
Positive conductive is substantially to be played the role of by positive conductive agent, and the method can be generalized to positive blending process
In, the resistivity of anode sizing agent can be directly tested in positive dispensing tested viscosity, can tentatively judge the conduction of conductive agent
Performance, and without all having surveyed until entire battery performance and just can see result (it is longer that entire performance has surveyed the period), can be with
The test and appraisal time is saved, working efficiency is improved.
This method can also be generalized to cathode blending process deionized water add after carry out testing size conductive agent and lead
Electrical property；Graphite is conductive in cathode, we can test and assess by contrast groups and by poor method, and it is conventional to calculate production
The solid of conductive agent contains (conductive agent+graphite+binder+dispersant+solvent) during cathode blending, setting contrast groups (conductive agent+
Dispersant+solvent), it is identical to ensure that it contains admittedly, under the premise of other materials all same, the electricity of two groups of slurries is tested using the method
It hinders, contains graphite in negative electrode slurry, conductive, theoretically the resistance of cathode slurry can be less than the electricity of the pure conductive agent of contrast groups
Resistance calculates graphite resistance (graphite resistance=pure conductive agent resistance-negative electrode slurry resistance) using by poor method, calculates resistivity,
The preliminary judgement that can directly carry out electric conductivity to cathode conductive agent in the case where not changing negative material, is equally also saved
Test and appraisal times improve working efficiency.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the scope of the invention, every at this
Under the inventive concept of invention, using equivalent structure transformation made by description of the invention and accompanying drawing content, or directly/use indirectly
In the scope of patent protection that other related technical areas are included in the present invention.
Claims (8)
1. a kind of device of testing size electric conductivity, which is characterized in that including：Sealing container with upper cover is placed in sealing container
The magnetic stirring apparatus of bottom outside, the miniature vacuum pumping pump being connected to sealing container, is set the stirring rotator being placed in sealing container
In in sealing container bottom two conductive current collectors, with two conductive current collectors be electrically connected instrument for measuring DC resistance, detection it is close
The infrared temperature measurement and control instrument for sealing container internal temperature, the feeding mechanism and discharging mechanism being connected to sealing container.
2. the device of testing size electric conductivity according to claim 1, which is characterized in that each conductive current collector is
One copper coin, copper coin top are equipped with several grooves linearly arranged, a pair of U row spring interfaces, double U rows are equipped in each groove
The connecting line of spring interface and instrument for measuring DC resistance matches.
3. the device of testing size electric conductivity according to claim 1, which is characterized in that the feeding mechanism includes a leakage
Bucket, the sebific duct for being connected to funnel and sealing container, the first manual valve being arranged on sebific duct.
4. the device of testing size electric conductivity according to claim 1, which is characterized in that the discharging mechanism goes out including one
Expects pipe and the second manual valve being arranged on discharge nozzle.
5. according to the device of claim 1-4 any one of them testing size electric conductivity, which is characterized in that the sealing container
Upper lid be equipped with a vacuum tube screwed union, connect with miniature vacuum pumping pump through a vacuum-pumping tube.
6. a kind of method of testing size electric conductivity, which is characterized in that include the following steps：
(1) prepared by slurry
According to the different solid electrocondution slurries containing under of the relationship of solution, solute, solvent configuration, the slurry of configuration is just full of entire survey
Trial assembly is set；
(2) slurry electric conductivity is tested
Instrument for measuring DC resistance is opened, two conducting wires of instrument for measuring DC resistance are connected to the groove of two conductive current collectors respectively
Interior double U rows spring interfaces；It tests under the solid resistance value containing under of parallel point slurry difference and identical different time containing slurry admittedly
Slurry resistance variations situation, identical solid influence of the different temperatures containing slurry to slurry resistance pass through formula ρ=RS/L, σ=1/
ρ calculates different solid resistivity and conductivity containing under, you can know slurry deployment conditions and slurry in different time and difference
Temperature and the Bu Tong solid electric conductivity containing under.
7. the method for testing size electric conductivity according to claim 6, which is characterized in that prepared by step (1) slurry
Detailed process it is as follows：
Upper cover is opened, conductive agent dry powder is added in sealing container, dispersant is added in sealing container, solvent by funnel and
Sebific duct is added in sealing container, covers upper cover, is put on magnetic stirring apparatus, opening magnetic stirring apparatus, rotating speed 1500rpm/s,
Stirring rotator is stirred the substance in container, and stirring 4h is uniform to slurry dispersion mixing, you can terminates stirring, connects micro-
Type vacuum pump carries out vacuumizing 20min, removes the bubble in slurry, and prepared by electrocondution slurry completes.
8. the method for testing size electric conductivity according to claim 6, which is characterized in that slurry is not in the step (2)
It is with the test method contained admittedly：
On the basis of initial slurry, take out part size, using carrying out calculating remaining ratio slurry by poor method, into container plus
Enter coordinative solvent or solution continues to stir to slurry after mixing, vacuum pump line and vacuum tube screwed union are connected, opened
Vacuum pump vacuumizes.
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| CN201810774633.6A CN108760827A (en) | 2018-07-13 | 2018-07-13 | A kind of device and method of testing size electric conductivity |
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|---|---|---|---|
| CN201810774633.6A CN108760827A (en) | 2018-07-13 | 2018-07-13 | A kind of device and method of testing size electric conductivity |
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| CN109752416A (en) * | 2019-03-20 | 2019-05-14 | 宁波石墨烯创新中心有限公司 | Slurry uniformity detection method and application |
| CN111307870A (en) * | 2019-11-26 | 2020-06-19 | 国联汽车动力电池研究院有限责任公司 | Method and device for evaluating uniformity of lithium ion battery slurry |
| CN115453252A (en) * | 2022-10-25 | 2022-12-09 | 江苏华永烯科技有限公司 | Conductive performance testing device for conductive paste |
| CN116165458A (en) * | 2022-12-07 | 2023-05-26 | 湖南烯能新材料有限公司 | Device and method for detecting conductivity of graphene conductive paste |
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| CN115453252B (en) * | 2022-10-25 | 2023-01-31 | 江苏华永烯科技有限公司 | Conductive performance testing device for conductive paste |
| CN116165458A (en) * | 2022-12-07 | 2023-05-26 | 湖南烯能新材料有限公司 | Device and method for detecting conductivity of graphene conductive paste |
| CN116165458B (en) * | 2022-12-07 | 2023-11-07 | 湖南烯能新材料有限公司 | Device and method for detecting conductivity of graphene conductive paste |
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Application publication date: 20181106 |