CN107478546A - Method for testing wettability of lithium battery diaphragm - Google Patents
Method for testing wettability of lithium battery diaphragm Download PDFInfo
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- CN107478546A CN107478546A CN201710578609.0A CN201710578609A CN107478546A CN 107478546 A CN107478546 A CN 107478546A CN 201710578609 A CN201710578609 A CN 201710578609A CN 107478546 A CN107478546 A CN 107478546A
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- lithium battery
- standard
- battery diaphragm
- extract
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 30
- 238000012360 testing method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 239000003792 electrolyte Substances 0.000 claims abstract description 18
- 238000004817 gas chromatography Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 15
- 238000010790 dilution Methods 0.000 claims description 9
- 239000012895 dilution Substances 0.000 claims description 9
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012086 standard solution Substances 0.000 abstract 2
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 abstract 1
- 239000011521 glass Substances 0.000 abstract 1
- 230000008595 infiltration Effects 0.000 abstract 1
- 238000001764 infiltration Methods 0.000 abstract 1
- 238000012544 monitoring process Methods 0.000 abstract 1
- 238000011002 quantification Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 235000019439 ethyl acetate Nutrition 0.000 description 14
- 230000004888 barrier function Effects 0.000 description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 230000005611 electricity Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- -1 stands 3h Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material 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 invention discloses a method for testing wettability of a lithium battery diaphragm, which comprises the following steps: cutting a lithium battery diaphragm to obtain a rectangular first sample; suspending a first sample above the battery electrolyte, immersing one end of the sample in the length direction into the battery electrolyte, standing, taking out, and airing to obtain a second sample; cutting the second sample at equal intervals in the length direction to obtain a third sample; respectively placing the third samples in glass bottles, adding ethyl acetate, sealing and carrying out ultrasonic treatment to obtain extract liquor; and respectively carrying out gas chromatography tests on the extraction liquid and the standard solution under the same gas chromatography condition, comparing the chromatographic peak areas of the extraction liquids, and drawing a standard curve according to the standard solution, thereby calculating the content of the vinyl carbonate in the extraction liquid. The method is easy to operate, accurate in quantification, capable of rapidly analyzing the infiltration effect of the lithium battery diaphragm in different environments and different working conditions, and capable of monitoring the opening and closing hole degrees of the diaphragm at different stages in the later stage.
Description
Technical field
The present invention relates to lithium battery technical field of measurement and test, more particularly to a kind of method of lithium battery diaphragm wellability test.
Background technology
In recent years, with the development in new energy technology and market, it is most important that lithium ion battery has become electric automobile
One of electrical source of power.Lithium ion battery typically all includes four electrode, electrolyte, barrier film and shell elements.Barrier film
One of important composition of lithium ion battery, in the progress of lithium battery technology, such as energy density lifting, improved safety, times
Rate performance improves and high temperature performance improves etc., except the exploitation by novel electrode system, also be unable to do without membrane technique
Support.Barrier film is usually placed between battery the two poles of the earth, and main effect is to prevent positive and negative interpolar from forming electronic conduction circuit, and is permitted
Perhaps ion turns on.Battery is very strict to the performance requirement of barrier film, and its quality directly affects the chemical property and peace of battery
Full performance, therefore the test to membrane properties is to weigh the important means for judging that a barrier film is good and bad.
Lithium-ion battery electrolytes use ethylene carbonate as solvent, therefore are tested in lithium ion battery separator wellability past
Quantitative analysis is carried out toward using ethylene carbonate.The wellability test of barrier film is measured using immersion solvent ocular estimate at present,
Influenceed by human factor and environmental factor, the uniformity and reappearance of test result are all poor；To sample in test process
The processing mode of product is relatively rough, and the human error so introduced to test result is larger.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of side of lithium battery diaphragm wellability test
Method, it is easily operated, it is quantitative accurate, without the miscellaneous equipment using expensive complex operation, it can quickly analyze lithium-ion electric
Effect of impregnation of the pond barrier film under varying environment and different operating modes, and the later stage can be for different phase barrier film opening and closing hole degree
It is monitored, has great importance for lithium battery research and development, barrier film evaluation and failure analysis.
A kind of method of lithium battery diaphragm wellability test proposed by the present invention, comprises the following steps：
S1, lithium battery diaphragm is cut out to obtain rectangular first sample；
S2, the first sample is hung on to battery electrolyte top, battery electricity is immersed into one end on the length direction of sample
Stood in solution liquid, take out, dry to obtain the second sample；
S3, the second sample carried out in the longitudinal direction equidistant to cut out to obtain the 3rd sample；
S4, the 3rd sample is respectively placed in vial, adds ethyl acetate, be ultrasonically treated after sealing and obtain extract；
S5, extract and standard liquid be subjected to gas-chromatography test under identical GC conditions respectively, will be each
Extract chromatographic peak area is compared, and standard curve is drawn according to standard liquid, so as to calculate ethylene carbonate in extract
Content.
Preferably, in S1, the width of the first sample is 2 ± 0.1cm, and the length of the first sample is 20 ± 1cm.
Preferably, in S2, the depth that the first sample immerses battery electrolyte is 1 ± 0.1cm, stands 2.8-3.2h.
Preferably, in S3, the length of the 3rd sample is 4 ± 0.2cm.
Preferably, in S4, ultrasonic time 28-32min.
Preferably, in S4, the 3rd sample is respectively placed in 20mL vials, adds 2mL ethyl acetate, poly- four will be carried
After the lid of PVF pad covers tightly sealing, supersound process obtains extract
Preferably, in S4, standard liquid is configured as follows：Ethyl acetate is added to ethylene carbonate standard items
Dilution, constant volume obtain standard liquid.
Preferably, in S4, standard liquid is configured as follows：Second is added to 100 μ L ethylene carbonates standard items
Acetoacetic ester dilutes, and is settled to 10mL and obtains standard specimen storing solution；It is dilute that ethyl acetate is separately added into 10-1000 μ L standard specimen storing solutions
Release, be settled to 10mL respectively and obtain the standard liquid that concentration is 10-1000mg/L.
Preferably, in S4, the concrete operations that standard curve is drawn according to standard liquid are as follows：It is 10-1000mg/ by concentration
L standard liquid carries out gas-chromatography test, then with the mass concentration (mg/L) of ethylene carbonate for abscissa, corresponding color
Spectral peak area normalization value is ordinate, draws standard curve.
Preferably, in S4, the content of ethylene carbonate in extract is calculated as follows：
K1=C1V×10-6
In formula：K1For the content of ethylene carbonate in sample, unit mL；
C1For the concentration of ethylene carbonate in the extract that is obtained by standard curve, unit is μ L/L；
V is extract volume, unit mL.
Barrier film wellability accurate judging method, easily operated used in the present invention, quantitative accurate, without using expensive behaviour
Make complicated miscellaneous equipment, can quickly analyze effect of impregnation of the lithium ion battery separator under varying environment and different operating modes,
And the later stage can be directed to different phase barrier film opening and closing hole degree and be monitored, and evaluate and fail for lithium battery research and development, barrier film
Analysis has great importance.
Brief description of the drawings
Fig. 1 is the gas chromatogram that the sample introduction of the embodiment of the present invention 4 analyzes test result.
Fig. 2 is the canonical plotting of gained ethylene carbonate in the embodiment of the present invention 4.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of method of lithium battery diaphragm wellability test proposed by the present invention, comprises the following steps：
S1, lithium battery diaphragm is cut out to obtain rectangular first sample；
S2, the first sample is hung on to battery electrolyte top, battery electricity is immersed into one end on the length direction of sample
Stood in solution liquid, take out, dry to obtain the second sample；
S3, the second sample carried out in the longitudinal direction equidistant to cut out to obtain the 3rd sample；
S4, the 3rd sample is respectively placed in vial, adds ethyl acetate, be ultrasonically treated after sealing and obtain extract；
S5, extract and standard liquid be subjected to gas-chromatography test under identical GC conditions respectively, will be each
Extract chromatographic peak area is compared, and standard curve is drawn according to standard liquid, so as to calculate ethylene carbonate in extract
Content.
Embodiment 2
A kind of method of lithium battery diaphragm wellability test proposed by the present invention, comprises the following steps：
S1, lithium battery diaphragm being cut out to obtain rectangular first sample, the width of the first sample is 1.9cm,
The length of one sample is 21cm；
S2, the first sample is hung on to battery electrolyte top, battery electricity is immersed into one end on the length direction of sample
2.8h is stood in solution liquid, the depth that the first sample immerses battery electrolyte is 1.1cm, takes out, dries to obtain the second sample；
S3, the second sample carried out in the longitudinal direction it is equidistant cut out to obtain the 3rd sample, the length of the 3rd sample is
4.2cm；
S4, the 3rd sample is respectively placed in vial, adds ethyl acetate, 28min is ultrasonically treated after sealing and is extracted
Take liquid；
S5, extract and standard liquid be subjected to gas-chromatography test under identical GC conditions respectively, will be each
Extract chromatographic peak area is compared, and standard curve is drawn according to standard liquid, so as to calculate ethylene carbonate in extract
Content.
Standard liquid is configured as follows：Ethyl acetate dilution is added to ethylene carbonate standard items, constant volume obtains
To standard liquid.
Embodiment 3
A kind of method of lithium battery diaphragm wellability test proposed by the present invention, comprises the following steps：
S1, lithium battery diaphragm being cut out to obtain rectangular first sample, the width of the first sample is 2.1cm,
The length of one sample is 19cm；
S2, the first sample is hung on to battery electrolyte top, battery electricity is immersed into one end on the length direction of sample
3.2h is stood in solution liquid, the depth that the first sample immerses battery electrolyte is 0.9cm, takes out, dries to obtain the second sample；
S3, the second sample carried out in the longitudinal direction it is equidistant cut out to obtain the 3rd sample, the length of the 3rd sample is
3.8cm；
S4, the 3rd sample is respectively placed in vial, adds ethyl acetate, 28-32min is ultrasonically treated after sealing and is obtained
Extract；
S5, extract and standard liquid be subjected to gas-chromatography test under identical GC conditions respectively, will be each
Extract chromatographic peak area is compared, and standard curve is drawn according to standard liquid, so as to calculate ethylene carbonate in extract
Content.
Standard liquid is configured as follows：Ethyl acetate dilution is added to 100 μ L ethylene carbonates standard items, it is fixed
Hold to 10mL and obtain standard specimen storing solution；Into 10 μ L, 20 μ L, 50 μ L, 100 μ L, 200 μ L, 500 μ L, 1mL standard specimen storing solutions respectively
Ethyl acetate dilution is added, 10mL is settled to respectively and obtains the standard liquid that concentration is 10-1000mg/L.
Embodiment 4
A kind of method of lithium battery diaphragm wellability test proposed by the present invention, comprises the following steps：
S1, two different lithium battery diaphragm is cut out to obtain 2cm × 20cm lengthy motion picture, is respectively designated as sample
A and sample b；
S2, sample a and sample b are hung on to identical battery electrolyte top respectively, by sample a length direction
One end, which is immersed in battery electrolyte, stands 3h, and one end on sample b length direction, which is immersed in battery electrolyte, stands 3h, sample
The depth that a and sample b immerses battery electrolyte is 1cm, takes out, dries；
S3, will dry rear sample a carry out in the longitudinal direction it is equidistant cut out, from immerse end to away from immerse extreme direction on
Sample a1, sample a2, sample a3, sample a4, sample a5 are named as successively；Rear sample b is dried to carry out in the longitudinal direction equidistantly
From cutting out, sample b1, sample b2, sample b3, sample b4, sample are named as successively on away from immersion extreme direction from immersing end
b5；Wherein sample a1, sample a2, sample a3, sample a4, sample a5, sample b1, sample b2, sample b3, sample b4, sample b5
Length be 4cm；
S4, by sample a1, sample a2, sample a3, sample a4, sample a5, sample b1, sample b2, sample b3, sample b4,
Sample b5 is respectively placed in 20mL vials, is separately added into 2mL chromatogram pure ethyl acetates, will carry teflon gasket respectively
Lid cover tightly, respectively be ultrasonically treated 30min obtain extract a1, extract a2, extract a3, extract a4, extract a5,
Extract b1, extract b2, extract b3, extract b4, extract b5；
S5, gas-chromatography test condition are as follows：Chromatographic column：Elite-wax(30m×0.25mm×0.25μm)；Injection port
Temperature：260 DEG C, 50 DEG C of chromatographic column initial temperature, 2min is kept, 230 DEG C of holdings are then risen to 10 DEG C/min heating rates
3min；Carrier gas：Nitrogen (N2), (purity >=99.99%), flow velocity 1.0mL/min；Detector：Flame ionization ditector；Enter
Sample volume：1μL；
Standard liquid is configured as follows：Ethyl acetate dilution is added to 100 μ L ethylene carbonates standard items, it is fixed
Hold to 10mL and obtain standard specimen storing solution；Into 10 μ L, 20 μ L, 50 μ L, 100 μ L, 200 μ L, 500 μ L, 1mL standard specimen storing solutions respectively
Ethyl acetate dilution is added, 10mL is settled to respectively and obtains the standard liquid that concentration is 10-1000mg/L；
Under above-mentioned GC conditions, the reference retention time of solvent ethyl acetate is 3.22min, ethylene carbonate mark
The reference retention time of quasi- thing is 16.35min, as shown in figure 1, Fig. 1 is the gas that the sample introduction of the embodiment of the present invention 4 analyzes test result
Phase chromatogram；
With the mass concentration (mg/L) of ethylene carbonate for abscissa, corresponding chromatographic peak area normalized value is sat to be vertical
Mark, draw standard curve；Sample in sample goes out peak area, and its mass concentration is corresponded in standard curve, so that it is determined that
Ethylene carbonate content in sample；Gained standard curve is as shown in Fig. 2 Fig. 2 is the gained ethylene carbonate of the embodiment of the present invention 4
Canonical plotting；
From Fig. 1 and Fig. 2：Ethylene carbonate standard liquid in 10-1000mg/L concentration range, its concentration with it is right
The peak area ratio answered is presented good linear relationship, and the linear equation of ethylene carbonate is y=20.566x+86.846, phase relation
Number is R2=0.9971；
S6, under above-mentioned identical GC conditions, by extract a1, extract a2, extract a3, extract a4,
Extract a5, extract b1, extract b2, extract b3, extract b4, extract b5 carry out gas-chromatography test respectively；Meter
The peak area and concentration of the ethylene carbonate of each extract are calculated, concrete outcome is as shown in the table：
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (8)
- A kind of 1. method of lithium battery diaphragm wellability test, it is characterised in that comprise the following steps：S1, lithium battery diaphragm is cut out to obtain rectangular first sample；S2, the first sample is hung on to battery electrolyte top, battery electrolyte is immersed into one end on the length direction of sample Middle standing, take out, dry to obtain the second sample；S3, the second sample carried out in the longitudinal direction equidistant to cut out to obtain the 3rd sample；S4, the 3rd sample is respectively placed in vial, adds ethyl acetate, be ultrasonically treated after sealing and obtain extract；S5, extract and standard liquid be subjected to gas-chromatography test under identical GC conditions respectively, by each extraction Liquid chromatography peak area is compared, and standard curve is drawn according to standard liquid, so as to calculate containing for ethylene carbonate in extract Amount.
- 2. the method for lithium battery diaphragm wellability test according to claim 1, it is characterised in that in S1, the first sample Width is 2 ± 0.1cm, and the length of the first sample is 20 ± 1cm.
- 3. the method for lithium battery diaphragm wellability test according to claim 1 or claim 2, it is characterised in that in S2, the first sample The depth for immersing battery electrolyte is 1 ± 0.1cm, stands 2.8-3.2h.
- 4. the method tested according to any one of the claim 1-3 lithium battery diaphragm wellabilities, it is characterised in that in S3, the The length of three samples is 4 ± 0.2cm.
- 5. the method tested according to any one of the claim 1-4 lithium battery diaphragm wellabilities, it is characterised in that in S4, surpass The sound time is 28-32min.
- 6. the method tested according to any one of the claim 1-5 lithium battery diaphragm wellabilities, it is characterised in that in S4, mark Quasi- solution is configured as follows：Ethyl acetate dilution is added to ethylene carbonate standard items, constant volume obtains standard liquid.
- 7. the method tested according to any one of the claim 1-6 lithium battery diaphragm wellabilities, it is characterised in that in S4, mark Quasi- solution is configured as follows：Ethyl acetate dilution is added to 100 μ L ethylene carbonates standard items, 10mL is settled to and obtains To standard specimen storing solution；Be separately added into 10-1000 μ L standard specimen storing solutions ethyl acetate dilution, be settled to respectively 10mL obtain it is dense Spend the standard liquid for 10-1000mg/L.
- 8. the method tested according to any one of the claim 1-7 lithium battery diaphragm wellabilities, it is characterised in that according to standard The concrete operations that solution draws standard curve are as follows：Standard liquid is subjected to gas-chromatography test, then with ethylene carbonate Mass concentration is abscissa, and corresponding chromatographic peak area normalized value is ordinate, draws standard curve.
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| CN201710578609.0A CN107478546A (en) | 2017-07-10 | 2017-07-10 | Method for testing wettability of lithium battery diaphragm |
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Cited By (3)
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| CN109142451A (en) * | 2018-09-06 | 2019-01-04 | 惠州亿纬锂能股份有限公司 | A kind of wetting velocity appraisal procedure of battery electrolyte |
| CN115541735A (en) * | 2022-06-15 | 2022-12-30 | 广东微电新能源有限公司 | Detection method of lithium battery electrolyte |
| CN117705650A (en) * | 2024-02-06 | 2024-03-15 | 深圳海辰储能科技有限公司 | Diaphragm wettability testing method and diaphragm wettability testing device |
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| CN117705650B (en) * | 2024-02-06 | 2024-05-14 | 深圳海辰储能科技有限公司 | Diaphragm wettability testing method and diaphragm wettability testing device |
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