CN105699270A - Method for testing porosity of lithium-ion battery separator - Google Patents
Method for testing porosity of lithium-ion battery separator Download PDFInfo
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- CN105699270A CN105699270A CN201610110619.7A CN201610110619A CN105699270A CN 105699270 A CN105699270 A CN 105699270A CN 201610110619 A CN201610110619 A CN 201610110619A CN 105699270 A CN105699270 A CN 105699270A
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- ion battery
- battery separator
- sample
- porosity
- lithium ion
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000012360 testing method Methods 0.000 title claims abstract description 37
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 30
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000004080 punching Methods 0.000 abstract description 9
- 238000005303 weighing Methods 0.000 abstract description 5
- 238000004364 calculation method Methods 0.000 abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 7
- 230000004888 barrier function Effects 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 7
- 238000010998 test method Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
- G01N15/0893—Investigating volume, surface area, size or distribution of pores; Porosimetry by measuring weight or volume of sorbed fluid, e.g. B.E.T. method
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to a method for testing the porosity of a lithium-ion battery separator. The method comprises the steps of obtaining samples through punching on the lithium-ion battery separator to be tested by means of a punching machine, and recording the diameter of the samples as d; placing the samples in a drying oven to be dried, lowering temperature to indoor temperate, and measuring the thickness delta and quality M1 of each sample; selecting the sample with uniform thickness, and soaking the sample in hexadecane; adsorbing residual liquid on the surface of the sample with filter paper, weighing the sample after the surface of the filter paper does not change any more, conducting adsorption again with the filter paper, weighing the sample again till weights obtained at two successive times are equal, and recording data M2; obtaining the porosity of the lithium-ion battery separator through a calculation formula according to mass change before and after soaking. Instruments and materials adopted in the testing process are inexpensive, testing is easy and convenient, and the accuracy rate is as high as 99.99%.
Description
(1) technical field
The present invention relates to lithium ion battery electrode material field, particularly to the method for testing of a kind of lithium ion battery separator porosity。
(2) background technology
Barrier film is the important component part of lithium ion battery cell, act primarily as the conduction of ion and the insulating effect of electronics, and the conduction of ion and the internal many miniature aperture existed of barrier film have much relations, so porosity is Con trolling index important in barrier film manufacture process。When the porosity of barrier film is too low, permeability is poor, causes the problems such as electrical conductivity is low, and barrier film porosity is too high, causes the puncture reduced capability of barrier film, shrinkage factor to increase and mechanical property is deteriorated, there is potential safety hazard。At present, though the method for test porosity has a lot, but process is loaded down with trivial details and tests instrument and consumptive material costly。
Therefore, cost during test barrier film porosity, reduce loaded down with trivial details test process, reducing institute's use instrument and consumptive material becomes technical staff's problem demanding prompt solution。
(3) summary of the invention
The present invention is in order to make up the deficiencies in the prior art, it is provided that the method for testing of a kind of lithium ion battery separator porosity, the method overcomes owing to test process is loaded down with trivial details in prior art, the test process high in cost of production problem that test instrument and consumptive material costliness cause。
The present invention is achieved through the following technical solutions:
A kind of method of testing of lithium ion battery separator porosity, it is characterized in that and comprises the following steps:
(1) on lithium ion battery separator to be measured, utilizing sheet-punching machine to go out sample, specimen finish is designated as d；
(2) being placed in by sample in drying baker dry, temperature is down to room temperature, surveys its thickness δ and mass M 1；
(3) choose sample in uniform thickness, be immersed in hexadecane；
(4) with the remaining liquid of Adsorption of Filter Paper specimen surface, treat that its surface is unchanged, weigh, again with Adsorption of Filter Paper, again weigh, till the weight of adjacent twice is the same, record data M2；
(5) according to the mass change before and after soaking, the porosity of lithium ion battery separator can be drawn by computing formula,
The computing formula of lithium ion battery separator porosity is:
Wherein,
Φ is lithium ion battery separator porosity, and unit is %；
Quality after M1 and M2 respectively samples dried and after immersion absorption；
D is the circular specimen diameter that puncher is gone out；
ρ is the density of hexadecane；
δ is sample thickness。
In step (2), drying baker temperature is 50-80 DEG C, dry 3-8 hour, it is preferable that dry 4 hours at 60 DEG C。
In step (3), sample is immersed in hexadecane 24-50 hour, it is preferable that 48 hours。
Beneficial effects of the present invention: in test process of the present invention, instrument and consumptive material are cheap, the method for the test lithium battery diaphragm porosity provided, test process is simple, convenient, accuracy rate is up to 99.99%。
(4) Figure of description
Below in conjunction with accompanying drawing, the present invention is further illustrated。
Accompanying drawing 1 is flow chart of the present invention。
(5) detailed description of the invention
Below in conjunction with the accompanying drawing in the invention process case, the technical scheme in the invention process case is carried out clear, complete description, it is clear that described case study on implementation is only a part for case of the present invention, and not all embodiment。Based on the case study on implementation of the present invention, the every other embodiment that those skilled in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention。
Embodiment 1
The invention discloses the method for testing of a kind of lithium ion battery separator voidage, according to formulaCarrying out the calculating of voidage, test process is simple, convenient accurately, it addition, instrument and consumptive material are less expensive in test process。
The instrument used in process of the present invention and medicine: sheet-punching machine, precision balance (0.0001g), accurate calibrator (± 0.1 μm), filter paper, tweezers, drying baker。
Refer to accompanying drawing 1, for the method for testing flow chart of a kind of lithium battery diaphragm porosity of disclosure；
The method of testing of a kind of lithium battery diaphragm porosity, comprises the following steps:
A (), for the lithium ion battery separator PP film of 20 μm and 40 μ m thick, intercepts one section of sample at micro-pore septum to be measured, utilizes sheet-punching machine to go out the identical circular specimen of diameter d=16mm 3 respectively, it is ensured that material stable and facilitate follow-up measuring and calculation。
B (), in the drying baker of 60 DEG C, is taken out after freeze-day with constant temperature 4h, is surveyed its quality respectively M1a, M1b, M1c, M1d, M1e, M1f, survey its thickness respectively δ 1, δ 2 under room temperature；
C MEMBRANEA sample to be measured is completely soaked in hexadecane by (), after 48h, with the remaining liquid of Adsorption of Filter Paper specimen surface, treat that its surface is unchanged, utilize scales/electronic balance weighing, again with Adsorption of Filter Paper, again weigh, till the weight of adjacent twice is the same, record data M2a, M2b, M2c, M2d, M2e, M2f；
D data are substituted into lithium ion battery separator porosity computing formula by ():Test result is following table such as:
Embodiment 2
The invention discloses the method for testing of a kind of lithium ion battery separator voidage, according to formulaCarrying out the calculating of voidage, test process is simple, convenient accurately, it addition, instrument and consumptive material are less expensive in test process。
The instrument used in process of the present invention and medicine: sheet-punching machine, precision balance (0.0001g), accurate calibrator (± 0.1 μm), filter paper, tweezers, drying baker。
Refer to accompanying drawing 1, for the method for testing flow chart of a kind of lithium battery diaphragm porosity of disclosure；
The method of testing of a kind of lithium battery diaphragm porosity, comprises the following steps:
A (), for the lithium ion battery separator PP film of 20 μm and 40 μ m thick, intercepts one section of sample at micro-pore septum to be measured, utilizes sheet-punching machine to go out the identical circular specimen of diameter d=18mm 3 respectively, it is ensured that material stable and facilitate follow-up measuring and calculation。
B (), in the drying baker of 50 DEG C, is taken out after freeze-day with constant temperature 8h, is surveyed its quality respectively M1a, M1b, M1c, M1d, M1e, M1f, survey its thickness respectively δ 1, δ 2 under room temperature；
C MEMBRANEA sample to be measured is completely soaked in hexadecane by (), after 24h, with the remaining liquid of Adsorption of Filter Paper specimen surface, treat that its surface is unchanged, utilize scales/electronic balance weighing, again with Adsorption of Filter Paper, again weigh, till the weight of adjacent twice is the same, record data M2a, M2b, M2c, M2d, M2e, M2f；
D data are substituted into lithium ion battery separator PP membrane porosity computing formula by ():Test result is following table such as:
Embodiment 3
The invention discloses the method for testing of a kind of lithium ion battery separator voidage, according to formulaCarrying out the calculating of voidage, test process is simple, convenient accurately, it addition, instrument and consumptive material are less expensive in test process。
The instrument used in process of the present invention and medicine: sheet-punching machine, precision balance (0.0001g), accurate calibrator (± 0.1 μm), filter paper, tweezers, drying baker。
Refer to accompanying drawing 1, for the method for testing flow chart of a kind of lithium battery diaphragm porosity of disclosure；
The method of testing of a kind of lithium battery diaphragm porosity, comprises the following steps:
A (), for the lithium ion battery separator PE film of 20 μm and 40 μ m thick, intercepts one section of sample at micro-pore septum to be measured, utilizes sheet-punching machine to go out the identical circular specimen of diameter d=18mm 3 respectively, it is ensured that material stable and facilitate follow-up measuring and calculation。
B (), in the drying baker of 80 DEG C, is taken out after freeze-day with constant temperature 3h, is surveyed its quality respectively M1a, M1b, M1c, M1d, M1e, M1f, survey its thickness respectively δ 1, δ 2 under room temperature；
C MEMBRANEA sample to be measured is completely soaked in hexadecane by (), after 50h, with the remaining liquid of Adsorption of Filter Paper specimen surface, treat that its surface is unchanged, utilize scales/electronic balance weighing, again with Adsorption of Filter Paper, again weigh, till the weight of adjacent twice is the same, record data M2a, M2b, M2c, M2d, M2e, M2f；
D data are substituted into lithium ion battery separator PE membrane porosity computing formula by ():Test result is following table such as:
Being not difficult to find out from above test result, the method test data of the present invention are more accurate, and error is less, simple to operate, and equipment requirements is relatively low。
It is above the method for testing of micro-pore septum porosity of the present invention is set forth; it is adapted to assist in and understands the present invention; but embodiments of the present invention are also not restricted to the described embodiments; any without departing from the change made under the principle of the invention, amendment, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention。
Claims (3)
1. the method for testing of a lithium ion battery separator porosity, it is characterised in that: comprise the following steps:
(1) on lithium ion battery separator to be measured, utilizing puncher to go out sample, specimen finish is designated as d；
(2) being placed in by sample in drying baker dry, temperature is down to room temperature, surveys its thickness δ and mass M 1；
(3) choose sample in uniform thickness, be immersed in hexadecane；
(4) with the remaining liquid of Adsorption of Filter Paper specimen surface, treat that its surface is unchanged, weigh, again with Adsorption of Filter Paper, again weigh, till the weight of adjacent twice is the same, record data M2；
(5) according to the mass change before and after soaking, the porosity of lithium ion battery separator can be drawn by computing formula,
The computing formula of lithium ion battery separator porosity is:
Φ=× 100,
Wherein,
Φ is lithium ion battery separator porosity, and unit is %；
Quality after M1 and M2 respectively samples dried and after immersion absorption；
D is the circular specimen diameter that puncher is gone out；
ρ is the density of hexadecane；
δ is sample thickness。
2. the method for testing of lithium ion battery separator porosity according to claim 1, it is characterised in that: in step (2), drying baker temperature is 50-80 DEG C, dry 3-8 hour。
3. the method for testing of lithium ion battery separator porosity according to claim 1, it is characterised in that: in step (3), sample is immersed in hexadecane 24-50 hour。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610110619.7A CN105699270A (en) | 2016-02-29 | 2016-02-29 | Method for testing porosity of lithium-ion battery separator |
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| CN201610110619.7A CN105699270A (en) | 2016-02-29 | 2016-02-29 | Method for testing porosity of lithium-ion battery separator |
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| CN105699270A true CN105699270A (en) | 2016-06-22 |
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| CN201610110619.7A Pending CN105699270A (en) | 2016-02-29 | 2016-02-29 | Method for testing porosity of lithium-ion battery separator |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758777A (en) * | 2016-03-02 | 2016-07-13 | 南京国轩电池有限公司 | Porosity test method for ceramic coating of lithium battery composite membrane |
| CN106769599A (en) * | 2016-12-03 | 2017-05-31 | 合肥国轩高科动力能源有限公司 | A kind of method of testing of electrodes of lithium-ion batteries porosity |
| CN108760604A (en) * | 2018-07-12 | 2018-11-06 | 华南理工大学 | A kind of liquid water open porosity test method of bamboo wood |
| CN108931467A (en) * | 2018-08-06 | 2018-12-04 | 福建省致格新能源电池科技有限公司 | A kind of test method of lithium ion battery separator porosity |
| CN112461701A (en) * | 2020-12-04 | 2021-03-09 | 中国航空工业集团公司成都飞机设计研究所 | Composite material durability-oriented post-impact water seepage test method |
| CN113654939A (en) * | 2020-05-12 | 2021-11-16 | 北京福田康明斯发动机有限公司 | Method for evaluating processing quality of honing reticulate pattern |
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| CN103115857A (en) * | 2013-01-22 | 2013-05-22 | 合肥国轩高科动力能源股份公司 | Method for testing porosity of battery diaphragm coated alumina ceramic coating |
| CN103134744A (en) * | 2011-12-02 | 2013-06-05 | 天津市捷威动力工业有限公司 | Method of testing porosity of pole piece |
| CN103512837A (en) * | 2013-09-13 | 2014-01-15 | 深圳市星源材质科技有限公司 | Testing method of porosity of lithium battery diaphragm |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105758777A (en) * | 2016-03-02 | 2016-07-13 | 南京国轩电池有限公司 | Porosity test method for ceramic coating of lithium battery composite membrane |
| CN106769599A (en) * | 2016-12-03 | 2017-05-31 | 合肥国轩高科动力能源有限公司 | A kind of method of testing of electrodes of lithium-ion batteries porosity |
| CN108760604A (en) * | 2018-07-12 | 2018-11-06 | 华南理工大学 | A kind of liquid water open porosity test method of bamboo wood |
| CN108931467A (en) * | 2018-08-06 | 2018-12-04 | 福建省致格新能源电池科技有限公司 | A kind of test method of lithium ion battery separator porosity |
| CN108931467B (en) * | 2018-08-06 | 2021-10-01 | 福建省致格新能源电池科技有限公司 | Method for testing porosity of lithium ion battery diaphragm |
| CN113654939A (en) * | 2020-05-12 | 2021-11-16 | 北京福田康明斯发动机有限公司 | Method for evaluating processing quality of honing reticulate pattern |
| CN112461701A (en) * | 2020-12-04 | 2021-03-09 | 中国航空工业集团公司成都飞机设计研究所 | Composite material durability-oriented post-impact water seepage test method |
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Application publication date: 20160622 |
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