CN109238937A - A kind of test method of lithium ion battery ceramic diaphragm porosity - Google Patents
A kind of test method of lithium ion battery ceramic diaphragm porosity Download PDFInfo
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- CN109238937A CN109238937A CN201811095526.7A CN201811095526A CN109238937A CN 109238937 A CN109238937 A CN 109238937A CN 201811095526 A CN201811095526 A CN 201811095526A CN 109238937 A CN109238937 A CN 109238937A
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- ion battery
- lithium ion
- ceramic diaphragm
- battery ceramic
- porosity
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- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 45
- 238000010998 test method Methods 0.000 title claims abstract description 21
- 238000005259 measurement Methods 0.000 claims abstract description 10
- 238000011549 displacement method Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 2
- 239000010432 diamond Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 235000019988 mead Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 238000012360 testing method Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 7
- 210000004379 membrane Anatomy 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229920000098 polyolefin Polymers 0.000 description 5
- 239000004743 Polypropylene Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000005524 ceramic coating Methods 0.000 description 4
- 210000002469 basement membrane Anatomy 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229920005822 acrylic binder Polymers 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000013139 quantization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (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)
- Secondary Cells (AREA)
Abstract
The present invention relates to a kind of test methods of lithium ion battery ceramic diaphragm porosity, belong to lithium ion battery process material evaluation field.The test method of lithium ion battery ceramic diaphragm porosity of the invention, comprising the following steps: the apparent volume of measurement lithium ion battery ceramic diaphragm sample is recorded as V0；Using Archimedes principle-gas expansion displacement method measurement lithium ion battery ceramic diaphragm sample skeleton volume, it is denoted as V1；The porosity of the diaphragm: P=(V is calculated according to the following formula0‑V1)/V0* 100%.The test method of lithium ion battery ceramic diaphragm porosity of the invention, easy to operate, process is easy to standardize and quantify, and test equipment and condition requirement are low, can relatively accurately measure the porosity of ceramic diaphragm, strong operability.
Description
Technical field
The present invention relates to a kind of test methods of lithium ion battery ceramic diaphragm porosity, belong to lithium ion battery process material
Expect evaluation field.
Background technique
Diaphragm is the important component of lithium ion battery, mainly plays ion conducting and electronic isolation, existing production
The polyethylene or polypropylene diaphragm of industry, because thickness, intensity and porosity etc. cannot integrally be taken into account, high temperature resistant and resistance to high current are filled
Discharge performance is poor, so as to cause there are huge security risks on dynamic lithium battery is applied.Not for existing membrane properties
Foot, research institution of various countries and enterprise are actively working to the development of high-performance power lithium battery diaphragm.Wherein, it is coated in membrane surface
One layer of Al2O3、SiO2Or other heat resistant type inorganic matter ceramic particles, it is handled through special process and bond matrix is close, it will be organic
The flexibility and the good thermal stability of inorganic matter of object are combined together into mainstream development trend.Inorganic coat on the one hand can be with
Thermal runaway caused by PP, PE diaphragm are heat-shrinked is solved to cause the safety problem of cells burst, explosion, on the other hand, due to
The ability that Ceramic Composite diaphragm and electrolyte and positive and negative pole material have good infiltration and imbibition to protect liquid, can increase substantially battery
Service life.
The porosity of diaphragm is too low, leads to poor air permeability, and conductivity is low, and porosity is excessively high, and the puncture ability of diaphragm subtracts
Weak, shrinking percentage increases and mechanical property is deteriorated, and there are security risks, therefore diaphragm porosity is in diaphragm production and use process
Important Con trolling index, but composite diaphragm is difficult with traditional weight method since the density of different materials is not quite similar come quasi-
The really porosity of measurement ceramic diaphragm.
Currently, there are many method of the porosity of test ceramic coating membrane, but process is cumbersome and test process is without regulation
Model and quantization, subjective factor are affected to test result.
Summary of the invention
The object of the present invention is to provide it is a kind of be simple to operate and friendly to environment, lithium ion battery ceramics that testing efficiency is high every
The test method of membrane porosity.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
A kind of test method of lithium ion battery ceramic diaphragm porosity, comprising the following steps:
The apparent volume for measuring lithium ion battery ceramic diaphragm sample, is recorded as V0；
The skeleton volume of lithium ion battery ceramic diaphragm sample is measured using Archimedes principle-gas expansion displacement method,
It is denoted as V1；
The porosity of the lithium ion battery ceramic diaphragm is calculated according to the following formula:
P=(V0-V1)/V0* 100%.
The test method of lithium ion battery ceramic diaphragm porosity of the invention, easy to operate, process is easy to standardize and measure
Change, test equipment and condition requirement are low, can relatively accurately measure the porosity of ceramic diaphragm, strong operability.It needs to illustrate
It is heretofore described skeleton volume containing closed pore volume.
The present invention measures Archimedes principle-gas expansion used by lithium ion battery ceramic diaphragm sample skeleton volume
Displacement method is the inert gas Bohr law (PV=nRT) under certain condition using small molecule diameter, by measurement due to
The skeleton volume that the reduction that sample test chamber is put into sample test chamber gas capacity caused by sample accurately to measure sample (contains
Closed pore), the as true volume of ceramic diaphragm.Gas expansion displacement method is the body for replacing liquid assay sample to be discharged with gas
Product eliminates a possibility that immersion method dissolves sample, has the advantages that not damage sample.Since gas can penetrate into pole in sample
The irregular hole of small hole and surface, therefore the sample volume measured is closer to the skeleton volume of sample.
Preferably, the lithium ion battery ceramic diaphragm sample is regular shape on the surface in vertical thickness direction.Such as, institute
Stating regular shape is rectangle, circle or diamond shape.Apparent body is convenient for using the lithium ion battery ceramic diaphragm sample of regular shape
Long-pending calculating；As regular shape be rectangle when, according to the thickness of rectangular length and width and sample, according to V0=long × wide ×
Thickness can calculate the apparent volume of sample.The apparent volume of sample is using measuring tools such as calibrator, rulers to the ruler of style
After very little measurement, in order to guarantee the measuring accuracy of sample apparent volume, the precision of calibrator is at least 1 μm.In order to improve measurement
Accuracy can also use other more accurate measuring instruments.
Preferably, the skeleton volume for measuring lithium ion battery ceramic diaphragm sample carries out in real density instrument.
Preferably, the test method of above-mentioned lithium ion battery ceramic diaphragm porosity further includes using Archimedes principle-
Before gas expansion displacement method measures the skeleton volume of lithium ion battery ceramic diaphragm sample, lithium ion battery ceramic diaphragm is carried out
Heating and thermal insulation processing.The purpose for carrying out heating and thermal insulation processing is the moisture for removing possible remaining in ceramic diaphragm sample hole, is mentioned
The accuracy of height test.More preferred, heating and thermal insulation processing should carry out after test apparent volume is completed.
Preferably, the temperature of the heating and thermal insulation processing is 50~80 DEG C.The time of heating and thermal insulation processing is 0.5~
2h。
The ceramic diaphragm includes basement membrane and is arranged in epilamellar ceramic coating.
Preferably, the basement membrane is polyolefin film.The ceramic coating includes ceramic particle and binder.
Preferably, the ceramic coating is aluminum oxide coating layer.
It is further preferred that the polyolefin film is PP film.
Detailed description of the invention
Fig. 1 is the flow chart of the test method of lithium ion battery ceramic diaphragm porosity in embodiment 1.
Specific embodiment
Below in conjunction with specific embodiment, the following further describes the technical solution of the present invention.
The real density instrument used in specific embodiment is Ultra PYC 1200e (Kang Ta instrument company of the U.S.).
The preparation method of lithium ion battery ceramic diaphragm in specific embodiment, comprising the following steps:
1) raw material PP is subjected to melting extrusion, is heat-treated to obtain polyolefin film after cooling；The hole of polyolefin film
Diameter is between 40~100nm；
2) vertical and horizontal stretching is carried out to polyolefin film respectively, is cut, is wound after thermal finalization；
3) basement membrane after winding is placed on coating machine, by ceramic slurry be coated in membrane surface obtain ceramic coated every
Film to get；Ceramic slurry includes alumina particle and binder, and the mass ratio of alumina particle and binder is 99:1, is adopted
Binder is aqueous polyacrylamide acrylic binders；The average grain diameter of alumina particle is 0.5 μm.
Embodiment 1
The test method of the lithium ion battery ceramic diaphragm porosity of the present embodiment, flow chart is as shown in Figure 1, specifically include
Following steps:
1) lithium ion battery ceramic diaphragm is taken, cuts the cuboid lithium ion battery ceramics of appropriate size along straight steel ruler with knife
Diaphragm is as sample to be tested；
Length, the width that rectangular-shape sample to be tested is measured with straight steel ruler, with miking rectangular-shape sample to be tested
Thickness (thickness is repeatedly measured and is averaged), according to V0=length × width x thickness calculates the apparent volume V of sample to be tested0；
2) sample to be tested is placed in 60 DEG C of air dry oven and keeps the temperature 1h, it is cold to be placed in progress nature in drier
But, sample to be tested is put in real density instrument, carries out the measurement of true volume, the true volume measured is denoted as V1, i.e. bone
Frame body product (contains closed pore)；
3) according to formula P=(V0-V1)/V0* 100%, calculate the porosity of sample to be tested to get.
Embodiment 2
The lithium ion battery ceramic diaphragm that thickness is about 20 μm, 18 μm and 16 μm three kinds of different sizes is chosen respectively, according to
The test method of lithium ion battery ceramic diaphragm porosity in embodiment 1, the porosity data tested are shown in Table 1.
The porosity of the lithium ion battery ceramic diaphragm of 1 three kinds of different sizes of table
The test method of lithium ion battery ceramic diaphragm porosity of the invention is obtained it can be seen from upper table data
Data error is smaller, and data are more acurrate, and test process is simple, convenient, fast, lower to equipment requirement, illustrates the present invention
Ceramic diaphragm porosity test method it is stable, reliable.
Claims (6)
1. a kind of test method of lithium ion battery ceramic diaphragm porosity, it is characterised in that: the following steps are included:
The apparent volume for measuring lithium ion battery ceramic diaphragm sample, is recorded as V0；
Using Archimedes principle-gas expansion displacement method measurement lithium ion battery ceramic diaphragm sample skeleton volume, it is denoted as
V1；
The porosity of the lithium ion battery ceramic diaphragm is calculated according to the following formula:
P=(V0-V1)/V0* 100%.
2. the test method of lithium ion battery ceramic diaphragm porosity according to claim 1, it is characterised in that: the lithium
Ion battery ceramic diaphragm sample is regular shape on the surface in vertical thickness direction.
3. the test method of lithium ion battery ceramic diaphragm porosity according to claim 2, it is characterised in that: the rule
Then shape is rectangle, circle or diamond shape.
4. the test method of lithium ion battery ceramic diaphragm porosity according to claim 1, it is characterised in that: measurement lithium
The skeleton volume of ion battery ceramic diaphragm sample carries out in real density instrument.
5. the test method of lithium ion battery ceramic diaphragm porosity according to claim 1, it is characterised in that: using Ah
Before base Mead principle-gas expansion displacement method measurement lithium ion battery ceramic diaphragm sample skeleton volume, by lithium ion battery
Ceramic diaphragm carries out heating and thermal insulation processing.
6. the test method of lithium ion battery ceramic diaphragm porosity according to claim 5, it is characterised in that: described to add
The temperature of hot isothermal holding is 50~80 DEG C, and the time is 0.5~2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811095526.7A CN109238937A (en) | 2018-09-19 | 2018-09-19 | A kind of test method of lithium ion battery ceramic diaphragm porosity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811095526.7A CN109238937A (en) | 2018-09-19 | 2018-09-19 | A kind of test method of lithium ion battery ceramic diaphragm porosity |
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| CN109238937A true CN109238937A (en) | 2019-01-18 |
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| CN201811095526.7A Pending CN109238937A (en) | 2018-09-19 | 2018-09-19 | A kind of test method of lithium ion battery ceramic diaphragm porosity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111398127A (en) * | 2020-04-26 | 2020-07-10 | 安徽科达新材料有限公司 | Method for testing porosity of lithium ion battery pole piece |
| CN112098301A (en) * | 2020-09-22 | 2020-12-18 | 国联汽车动力电池研究院有限责任公司 | Method for testing porosity of diaphragm |
| CN112362549A (en) * | 2019-12-25 | 2021-02-12 | 万向一二三股份公司 | Method for measuring porosity of lithium ion battery pole piece |
| CN114221046A (en) * | 2021-11-16 | 2022-03-22 | 天津力神电池股份有限公司 | Method for testing residual space volume in hard-shell lithium ion battery |
| CN114646731A (en) * | 2022-03-10 | 2022-06-21 | 欣旺达电动汽车电池有限公司 | Decomposition method for irreversible expansion of battery pole piece |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362549A (en) * | 2019-12-25 | 2021-02-12 | 万向一二三股份公司 | Method for measuring porosity of lithium ion battery pole piece |
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| CN112098301A (en) * | 2020-09-22 | 2020-12-18 | 国联汽车动力电池研究院有限责任公司 | Method for testing porosity of diaphragm |
| CN114221046A (en) * | 2021-11-16 | 2022-03-22 | 天津力神电池股份有限公司 | Method for testing residual space volume in hard-shell lithium ion battery |
| CN114221046B (en) * | 2021-11-16 | 2023-08-25 | 天津力神电池股份有限公司 | Method for testing residual space volume in hard shell lithium ion battery |
| CN114646731A (en) * | 2022-03-10 | 2022-06-21 | 欣旺达电动汽车电池有限公司 | Decomposition method for irreversible expansion of battery pole piece |
| CN114646731B (en) * | 2022-03-10 | 2023-10-20 | 欣旺达动力科技股份有限公司 | Decomposition method for irreversible expansion of battery pole piece |
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Address after: 454191 Industrial Cluster Area, Jiaozuo City, Henan Province, Standardized Workshop Area on the North Side of Xinyuan Road, West Park Applicant after: Multi-fluorine New Energy Technology Co., Ltd. Address before: 454191 Henan Jiaozuo industrial agglomeration area, West Park, Xinyuan Road, north side of the standardization workshop. Applicant before: Duofuduo (Jiaozuo) Amperex Technology Limited |
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Application publication date: 20190118 |