CN106370930A - Lithium ion battery separator electrical performance testing device and method - Google Patents

Lithium ion battery separator electrical performance testing device and method Download PDF

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Publication number
CN106370930A
CN106370930A CN201610847712.6A CN201610847712A CN106370930A CN 106370930 A CN106370930 A CN 106370930A CN 201610847712 A CN201610847712 A CN 201610847712A CN 106370930 A CN106370930 A CN 106370930A
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China
Prior art keywords
electrode
lithium ion
ion battery
resistivity
battery separator
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Withdrawn
Application number
CN201610847712.6A
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Chinese (zh)
Inventor
陈夏雨
刘丽菲
黄梦欣
许辉
饶睦敏
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Shenzhen OptimumNano Energy Co Ltd
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Shenzhen OptimumNano Energy Co Ltd
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Priority to CN201610847712.6A priority Critical patent/CN106370930A/en
Publication of CN106370930A publication Critical patent/CN106370930A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R27/00Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
    • G01R27/02Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Secondary Cells (AREA)

Abstract

The present invention provides a lithium ion battery separator electrical performance testing device and a lithium ion battery separator electrical performance testing method. The device comprises a transparent sample container, a movable electrode, a fixed electrode and electrode leads. The device can be used for measuring the ionic conductivity and resistivity of separator samples. The device can be directly connected with an existing resistivity measuring instrument which satisfies measurement accuracy. The device is simple in structure and low in cost. After the resistance values or resistivity of different layers of separator samples are tested a plurality of numbers of times, testing results are linearly fitted; obtained slopes are the resistance values of the separator samples. With the method adopted, the influence of external factors is eliminated, and testing accuracy can be improved; when a plurality of times of measurement is carried out, it only needs to remove the movable electrode, the disassembly and reassembly of the device are not required, and therefore, measurement can be simple and quick, and can be carried out continuously; after an electrolyte is injected into a sample chamber, the resistivity of the electrolyte can be measured, and a Mac-Mullin value can be optimized; and the resistivity of the separator samples and the electrolyte under the same condition can be obtained, so that measurement errors can be reduced.

Description

A kind of lithium ion battery separator electric performance testing device and its method
[technical field]
The invention belongs to cell art, more particularly, to a kind of lithium ion battery separator electric performance testing device and its side Method.
[background technology]
Lithium ion battery is usually to be made up of positive electrode, graphite cathode material, nonaqueous electrolyte and barrier film.Wherein, every Film is the important component part of battery, is to ensure that one of key building block of lithium battery security performance, it has electronic isolation Property, therefore can isolate both positive and negative polarity, it is to avoid the two poles of the earth contact short circuit phenomenon occurs;There is ionic conductivity simultaneously it is ensured that electricity The chemical property in pond.The ionic conductivity of barrier film, resistivity and mac-mullin number be characterize barrier film ion permeability Important parameter, reflects the impact to ion motion for the barrier film, reflects the impact to lithium ion battery chemical property for the barrier film.Cause This, membrane properties quality directly affects the combination property of lithium ion battery, the correct electricity evaluating diaphragm for lithium ion battery Chemical property, and then the use barrier film of science, are to improve one of effective way of battery combination property.
At present, the unified standard of the domestic detecting instrument not yet being formed with regard to lithium battery diaphragm and detection method, many passes Detection project in its physical property has been applied mechanically the product standard of the industries such as plastic sheeting, paper products, textile and has been measured, and closes Just less in the standard of the test of diaphragm electrochemical performance, for the state of development of current diaphragm examination criteria, need one kind Simple and practical lithium ion battery separator electric performance testing device and method of testing.
[content of the invention]
The present invention proposes a kind of lithium ion battery separator electric performance testing device and its method, has simple to operate, cost Cheap, data is accurate, practical the advantages of.
A kind of lithium ion battery separator electric performance testing device that the present invention provides, including transparent shuttle, activity Electrode, fixed electrode and electrode outlet line;Described shuttle is provided with rule;Described float electrode and described fixed electrode set It is placed in described shuttle and coordinates with described shuttle, and described float electrode is placed in parallel with described fixed electrode; Described shuttle, float electrode and fixed electrode surround sample room;Described electrode outlet line respectively with described float electrode and Described fixed electrode is connected.
In a preferred embodiment, described shuttle is cylinder.
In a preferred embodiment, described float electrode and described fixed electrode are that size identical is circular.
In a preferred embodiment, described electrode outlet line is additionally coupled to Instrument Measuring Resistivity of Carbon Products.
The lithium ion battery separator electric performance test method that the present invention provides, can be used in the ionic conductivity of measuring diaphragm And resistivity, comprise the following steps: (1) produces multilamellar size identical barrier film sample according to the diameter of shuttle;(2) by institute State barrier film sample to soak in the electrolytic solution;(3) the described barrier film sample after the immersion of the different numbers of plies is laid in described sample room Interior;(4) electrode export line described in a pair is connected with the p-wire of Instrument Measuring Resistivity of Carbon Products respectively;(5) measure the leaching of the different numbers of plies The resistance value of the described barrier film sample after bubble.
In a preferred embodiment, also include step (6) and measure bath resistance rate.
In a preferred embodiment, also include step (7) to be calculated according to membrane electrical resistance rate and bath resistance rate Mac-mullin value;Mac-mullin value refers to the ratio of membrane electrical resistance rate and bath resistance rate, uses symbol nmRepresent, nm= ρse, ρ in formulasFor membrane electrical resistance rate, ρeFor bath resistance rate.
A kind of lithium ion battery separator electric performance testing device and its method that the present invention provides, can directly survey with meeting The determining instrument of the existing Instrument Measuring Resistivity of Carbon Products of accuracy of measurement or electrochemical workstation is attached, and structure is simple, and measurement cost is low; Described shuttle is provided with rule, can carry out direct measurement to height of specimen or thickness;When taking multiple measurements, only need to take out Float electrode, need not carry out disassembling and resetting of device, and test process simple and fast can be continuous;Barrier film electricity to the different numbers of plies After resistance or resistivity are repeatedly tested, test result is carried out linear fit, the slope tried to achieve is this membrane electrical resistance value rBarrier film, intercept is (rElectrode+rOther), thus eliminating the impact of extrinsic factor, improve test accuracy;After sample room injection electrolyte, The determination of resistivity of electrolyte can also be carried out, obtain barrier film sample and electrolyte resistivity under the same conditions, reduce and survey Amount error.
[brief description]
Fig. 1 is lithium ion battery separator electric performance testing device schematic diagram of the present invention.
Fig. 2 is the resistivity linear fit result of different number of plies barrier film samples in one embodiment.
Fig. 3 is the resistivity linear fit result that differing heights electrolyte measures in one embodiment.
[specific embodiment]
As shown in figure 1, the present invention provide a kind of lithium ion battery separator electric performance testing device 10, including shuttle 1, Float electrode 2, fixed electrode 3 and electrode outlet line 4.Described shuttle 1 is provided with rule 5.Described float electrode 2 and described Fixed electrode 3 is arranged in described shuttle 1 and is coordinated with described shuttle 1;Described float electrode 2 and described fixing electricity Pole 3 is placed in parallel.Described shuttle 1, float electrode 2 and fixed electrode 3 surround sample room 6.Described electrode outlet line 4 is respectively It is connected with described float electrode 2 and described fixed electrode 3.
In present embodiment, described shuttle 1 is made of clear material, for example, transparent glass or plastics.Described Shuttle 6 is cylinder, and described float electrode 2 and described fixed electrode 3 are that size identical is circular.In other embodiment In, described shuttle 1 can also adopt the other shapes such as right prism.Described electrode outlet line is additionally coupled to determination of resistivity Instrument.
The present invention also provides a kind of method of testing using described lithium ion battery separator electric performance testing device 10, this survey The basic step of method for testing and Principle of Process are as follows:
Diameter according to shuttle using punching sampler produce multilamellar size identical barrier film sample and by be measured every Membrane sample soaks in the electrolytic solution, then the barrier film sample tweezers after soaking is laid in sample room, finally will using fixture A pair of electrodes export line is coupled together with the p-wire of Instrument Measuring Resistivity of Carbon Products, you can carry out resistivity or testing impedance, can obtain To resistivity value or the resistance value of barrier film sample, and then the ionic conductivity of barrier film is estimated.The calculating of ionic conductivity Formula is:
σ = 1 ρ s
Wherein ρsFor membrane electrical resistance rate.
Contacting including internal resistance at electrode and surface of mensure is actually by the result that above method is tested As a result, the resistivity recording is by rAlwaysCome to change, and now rAlways=rBarrier film+(rElectrode+rOther).In order to eliminate (rElectrode+rOther) Impact, repeatedly would generally be tested to the resistance value of the barrier film of the different numbers of plies when carrying out membrane electrical resistance rate or resistance test, And test result is carried out linear fit, in the hope of slope value as this membrane electrical resistance value rBarrier film, intercept is (rElectrode+rOther), from And eliminate the impact of the extrinsic factor such as electrode resistance and surface contacted resistance, improve the accuracy of test.
The determination of resistivity that sample room carries out electrolyte can also be injected the electrolyte into, obtain barrier film with electrolyte identical Under the conditions of resistivity value, reduce measurement error, draw more accurate barrier film mac-mullin value.Mac-mullin value refers to Membrane electrical resistance rate and the ratio of bath resistance rate, use symbol nmRepresent, computing formula is:
n m = ρ s ρ e
Wherein ρsFor membrane electrical resistance rate;ρeFor bath resistance rate.
A kind of lithium ion battery separator electric performance testing device and its method that the present invention provides, can directly survey with meeting The determining instrument of the existing Instrument Measuring Resistivity of Carbon Products of accuracy of measurement or electrochemical workstation is attached, and structure is simple, and measurement cost is low; Described shuttle is provided with rule, can carry out direct measurement to height of specimen or thickness;When taking multiple measurements, only need to take out Float electrode, need not carry out disassembling and resetting of device, and test process simple and fast can be continuous;Barrier film electricity to the different numbers of plies After resistance or resistivity are repeatedly tested, test result is carried out linear fit, the slope tried to achieve is this membrane electrical resistance value rBarrier film, intercept is (rElectrode+rOther), thus eliminating the impact of extrinsic factor, improve test accuracy;After sample room injection electrolyte, The determination of resistivity of electrolyte can also be carried out, obtain barrier film sample and electrolyte resistivity under the same conditions, reduce and survey Amount error.
In a specific embodiment, by barrier film to be measured with sampling with described sample room 6 diameter identical punching sampler, Prepare barrier film sample about 40-50 piece, and be soaked in appropriate electrolyte.After barrier film sample Electolyte-absorptive saturation, take off institute State float electrode 2, with tweezers, barrier film sample is laid in described sample room 6, the quantity of record barrier film sample, then institute is installed State float electrode 2, and promote described float electrode 2 and barrier film sample good contact.Finally by described electrode outlet line 4 and resistance The test connecting line of rate analyzer is connected and starts to test, and records test result.After the completion of test, described float electrode 2 is taken Go out, continue to add the barrier film of respective numbers in described sample room 6, repeated measure operation, records next test result afterwards.Survey The resistivity of the different number of plies barrier film samples obtaining is as shown in table 1:
The resistivity value that the different number of plies barrier film of table 1. measures
Resistivity table 1 repeatedly being tested the different number of plies barrier film samples obtaining carries out linear fit, result such as Fig. 2 Shown, the slope obtaining is 1.299, shows that the resistivity of barrier film sample is 1.299m ω cm.In addition, in sample interior injection The electrolyte of differing heights, the resistivity obtaining as shown in table 2 and Fig. 3 it is known that this bath resistance rate be 0.15m ω cm, So the n of this barrier filmm=1.299/0.15=8.66.
The resistivity value that table 2. differing heights electrolyte measures
The electrical conductivity of generally electrolyte adopts conductivity measuring instrument direct measurement, the resistivity of the electrolyte that the present invention obtains Obtain under identical conditions with membrane electrical resistance rate, decrease the measurement error being caused by the difference of determining instrument, improve measurement Accuracy.
The foregoing is only presently preferred embodiments of the present invention, be to institute of the present invention with reference to specific preferred implementation Make further describe it is impossible to assert the present invention be embodied as be confined to these explanations.All spirit in the present invention and Any modification, equivalent and improvement of being made within principle etc., should be included in protection scope of the present invention.

Claims (7)

1. a kind of lithium ion battery separator electric performance testing device is it is characterised in that include transparent shuttle, flexible lamp Pole, fixed electrode and electrode outlet line;Described shuttle is provided with rule;Described float electrode and the setting of described fixed electrode Coordinate in described shuttle and with described shuttle, and described float electrode is placed in parallel with described fixed electrode;Institute State shuttle, float electrode and fixed electrode and surround sample room;Described electrode outlet line respectively with described float electrode and institute State fixed electrode to be connected.
2. lithium ion battery separator electric performance testing device as claimed in claim 1 is it is characterised in that described shuttle is Cylindrical.
3. lithium ion battery separator electric performance testing device as claimed in claim 1 it is characterised in that described float electrode and Described fixed electrode is that size identical is circular.
4. lithium ion battery separator electric performance testing device as claimed in claim 1 is it is characterised in that described electrode outlet line It is additionally coupled to Instrument Measuring Resistivity of Carbon Products.
5. a kind of lithium ion battery separator electric performance test method of utilization claim 1 described device, can be used in measure every The ionic conductivity of film and resistivity are it is characterised in that comprise the following steps: (1) produces multilamellar according to the diameter of shuttle Size identical barrier film sample;(2) described barrier film sample is soaked in the electrolytic solution;(3) by the institute after the immersion of the different numbers of plies State barrier film sample and be laid in described sample interior;(4) by the test with Instrument Measuring Resistivity of Carbon Products respectively of electrode export line described in a pair Line is connected;(5) measure the resistance value of the described barrier film sample after the immersion of the different numbers of plies.
6. a kind of lithium ion battery separator electric performance test method as claimed in claim 5 is it is characterised in that also include step (6) measure bath resistance rate.
7. a kind of lithium ion battery separator electric performance test method as claimed in claim 6 is it is characterised in that also include step (7) mac-mullin value is calculated according to membrane electrical resistance rate and bath resistance rate;Mac-mullin value refers to membrane electrical resistance rate With the ratio of bath resistance rate, use symbol nmRepresent, nmse, ρ in formulasFor membrane electrical resistance rate, ρeFor bath resistance Rate.
CN201610847712.6A 2016-09-23 2016-09-23 Lithium ion battery separator electrical performance testing device and method Withdrawn CN106370930A (en)

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Cited By (10)

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CN106896271A (en) * 2017-03-10 2017-06-27 深圳中兴创新材料技术有限公司 A kind of apparatus and method for the test of battery diaphragm electrical conductivity
CN108051645A (en) * 2017-12-26 2018-05-18 宁夏钜晶源晶体科技有限公司 A kind of lithium tantalate, lithium niobate crystal chip resistivity measurement device and test method
CN108318822A (en) * 2017-12-18 2018-07-24 合肥国轩高科动力能源有限公司 Method and system for measuring conductivity of lithium battery pole piece and diaphragm
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
CN111220850A (en) * 2019-11-18 2020-06-02 深圳新恒业电池科技有限公司 Battery diaphragm resistance value measuring method and device
WO2021075778A1 (en) * 2019-10-14 2021-04-22 주식회사 엘지화학 Method and system for evaluating insulation and lithium ion conductivity characteristics of separator for electrochemical device
CN113687144A (en) * 2021-07-30 2021-11-23 蜂巢能源科技有限公司 Testing device and testing method for diaphragm ionic conductivity
CN114236239A (en) * 2021-12-15 2022-03-25 湖北亿纬动力有限公司 Testing device and testing method for diaphragm ionic conductivity
CN114755155A (en) * 2022-03-15 2022-07-15 宁德卓高新材料科技有限公司 Water resistance testing method for coated diaphragm
CN116773607A (en) * 2023-08-24 2023-09-19 宁德时代新能源科技股份有限公司 Method and equipment for detecting lithium supplementing quantity

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CN105158566A (en) * 2015-08-12 2015-12-16 深圳市星源材质科技股份有限公司 Test device and method for closed-pore film rupture temperature and ion conductivity of cell diaphragm

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CN106896271B (en) * 2017-03-10 2023-03-28 深圳中兴新材技术股份有限公司 Device and method for testing conductivity of battery diaphragm
CN106896271A (en) * 2017-03-10 2017-06-27 深圳中兴创新材料技术有限公司 A kind of apparatus and method for the test of battery diaphragm electrical conductivity
CN108318822A (en) * 2017-12-18 2018-07-24 合肥国轩高科动力能源有限公司 Method and system for measuring conductivity of lithium battery pole piece and diaphragm
CN108051645A (en) * 2017-12-26 2018-05-18 宁夏钜晶源晶体科技有限公司 A kind of lithium tantalate, lithium niobate crystal chip resistivity measurement device and test method
CN108051645B (en) * 2017-12-26 2023-10-27 宁夏钜晶源晶体科技有限公司 Lithium tantalate and lithium niobate wafer resistivity testing device and testing method
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
WO2021075778A1 (en) * 2019-10-14 2021-04-22 주식회사 엘지화학 Method and system for evaluating insulation and lithium ion conductivity characteristics of separator for electrochemical device
CN111220850A (en) * 2019-11-18 2020-06-02 深圳新恒业电池科技有限公司 Battery diaphragm resistance value measuring method and device
CN113687144A (en) * 2021-07-30 2021-11-23 蜂巢能源科技有限公司 Testing device and testing method for diaphragm ionic conductivity
CN114236239A (en) * 2021-12-15 2022-03-25 湖北亿纬动力有限公司 Testing device and testing method for diaphragm ionic conductivity
CN114236239B (en) * 2021-12-15 2024-02-02 湖北亿纬动力有限公司 Testing device and testing method for ion conductivity of diaphragm
CN114755155A (en) * 2022-03-15 2022-07-15 宁德卓高新材料科技有限公司 Water resistance testing method for coated diaphragm
CN116773607A (en) * 2023-08-24 2023-09-19 宁德时代新能源科技股份有限公司 Method and equipment for detecting lithium supplementing quantity
CN116773607B (en) * 2023-08-24 2024-04-12 宁德时代新能源科技股份有限公司 Method and equipment for detecting lithium supplementing quantity

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