CN109682735A - The test method of electrodes of lithium-ion batteries coating porosity - Google Patents
The test method of electrodes of lithium-ion batteries coating porosity Download PDFInfo
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- CN109682735A CN109682735A CN201811572462.5A CN201811572462A CN109682735A CN 109682735 A CN109682735 A CN 109682735A CN 201811572462 A CN201811572462 A CN 201811572462A CN 109682735 A CN109682735 A CN 109682735A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000576 coating method Methods 0.000 title claims abstract description 32
- 238000010998 test method Methods 0.000 title claims abstract description 17
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 239000011888 foil Substances 0.000 claims abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 5
- 230000003068 static effect Effects 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011149 active material Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000006258 conductive agent Substances 0.000 claims description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000002562 thickening agent Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 2
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 claims description 2
- 239000006255 coating slurry Substances 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- -1 volume V are taken3 Substances 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 3
- 239000007924 injection Substances 0.000 abstract description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052753 mercury Inorganic materials 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000005030 aluminium foil Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000012956 testing procedure Methods 0.000 description 2
- 239000005955 Ferric phosphate Substances 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000243 solution Substances 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)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of test methods of electrodes of lithium-ion batteries coating porosity, belong to field of lithium.Test method of the present invention takes pole piece to calculate its coating volume, foil volume the following steps are included: prepare pole piece；A certain amount of solvent is taken, solvent is put into the container of closed vacuum-pumping, while pole piece being also placed in the container, but pole piece is not contacted with solvent；Container is vacuumized, when vacuum degree reaches -0.09MPa, pole piece is immersed in solvent；It is static to carry out vacuum breaker after ten minutes and vacuumize, wherein using nitrogen or argon gas protection when vacuum breaker；Pole piece is immersed in solvent, is shelved under protective atmosphere 12 ~ 36 hours；It reads pole piece and immerses the volume after solvent；Finally calculate porosity.The present invention passes through the test of pole coating porosity, can accurately more test out porosity profiles, and compared with conventional mercury injection apparatus test method, this method has testing efficiency height, the low advantage of measurement cost.
Description
Technical field
The present invention relates to a kind of test methods of electrodes of lithium-ion batteries coating porosity, belong to field of lithium.
Background technique
Since lithium ion battery has many advantages, such as that energy density is high, self discharge is small, cycle performance is superior, lithium ion battery is wide
It is general be applied to backup power source, energy storage device, electric car, electric bicycle, in electric tool.Lithium battery mainly has positive, negative
Pole, diaphragm, electrolyte and five part of shell composition.Cycle performance, inner resistance of battery etc. have important phase with battery liquid-filling amount
Guan Xing, and the number of battery liquid-filling amount, it is related with the compacted density of battery and porosity.The porosity and compacting and material of pole piece
Self character it is related.Therefore test pole piece coating porosity rationally controls reservoir quantity and is conducive to the property such as battery later cycles
Energy.Since positive and negative pole material matching type is very more, need to take the test method of simple and effective pole coating porosity.
Summary of the invention
The present invention provides a kind of test method of electrodes of lithium-ion batteries coating porosity, solves pole coating porosity
Test problem.
To achieve the above object, the technical solution adopted by the present invention is that:
The test method of electrodes of lithium-ion batteries coating porosity, comprising the following steps:
1) foil, is prepared, in foil surface coating slurry, roll-in is carried out to the foil for being coated with slurry and forms pole piece,
1) takes pole piece to calculate its coating volume V1, foil volume V2；
2) takes a certain amount of solvent, volume V3, solvent is put into the container of closed vacuum-pumping, while by pole piece
It is put into the container, but pole piece is not contacted with solvent；
3) vacuumizes container, and when vacuum degree reaches -0.09MPa, pole piece is immersed in solvent；
4) is static after ten minutes, carries out vacuum breaker and vacuumizes, is wherein protected when vacuum breaker using nitrogen or argon gas；
5) pole piece is immersed in solvent, is shelved under protective atmosphere 12 ~ 36 hours；
6) reads the volume V after pole piece immersion solvent4；
7) porosity ηHole=(V1+V2+V3-V4)/V1×100%。
Preferably, carrying out vacuum breaker and vacuumizing to be carried out continuously 10 ~ 20 times.
Preferably, slurry is coated in foil according to cell size recipe requirements progress slurry preparation by slurry in step 1)
It is dried to form pole piece after on material, control pole piece moisture content is less than 800ppm, and carrying out roll-in to pole piece after drying makes to apply
Lamination is real, ultimately forms pole piece.
Preferably, including: active material, conductive agent, binder, solvent in slurry in step 1).
Preferably, there are also thickener or dispersing agents in slurry.
It is further preferably, in cell size active material be LiFePO4, nickel-cobalt-manganese ternary material, cobalt acid lithium material,
One of lithium manganate material, graphite, silicon-carbon cathode material, the conductive agent are carbon black, carbon nanotube, one in active carbon
Kind, the binder is one of PVDF, SBR, and the thickener is CMC, and dispersing agent is polyvinylpyrrolidone, described molten
Agent is N-methyl pyrrolidones, in deionized water, dehydrated alcohol, acetone, dimethyl carbonate, diethyl carbonate, ethylene carbonate
One or more mixing.
The present invention passes through the test of pole coating porosity, realizes the careful design that additional amount is needed to electrolyte, coating
Porosity test calculation method is to immerse solvent test to pole piece after roll-in, can accurately more test out porosity profiles, can be with
The influence for reducing some uncertain factors, compared with conventional mercury injection apparatus test method, this method has testing efficiency high, measures
Advantage at low cost.
Specific embodiment
The present invention is further described combined with specific embodiments below, and the present invention includes but is not limited to following implementation case
Example.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material,
It can be obtained from commercialization approach.
Embodiment 1,
By taking ferric phosphate lithium cell as an example, anode pole piece step is prepared:
1) according to battery recipe requirements, slurry preparation is carried out.It include: LiFePO 4 material, carbon black, PVDF, NMP in slurry；
2) slurry is coated on foil, and is dried and forms pole piece, aluminium foil surface density is 42g/m2, aluminum foil thickness is 16 μ
M, control pole piece coat side density are 330g/m2, control pole piece moisture content is less than 800ppm；
3) carrying out roll-in to pole piece after drying is compacted coating, and roll-in thickness is at 152 μm, compacted density 2.39g/cm3,
Calculate the testing procedure of coating porosity are as follows:
1) pole piece width is 56mm, pole coating volume V after roll-in1=724mm × 56mm × (0.153mm-0.016mm/(1+
0.56%)=5558.14mm3, aluminium foil volume V2=724mm × 56mm × 0.016mm/(1+0.56%)=645.1mm3。
2) a certain amount of solvent dimethyl carbonate, volume V are taken3=8000mm3。
3) solvent is put into the container of closed vacuum-pumping, while pole piece being also placed in the container, but pole piece not with
Solvent contact.
4) container is vacuumized, when vacuum degree reaches -0.09MPa, pole piece is immersed in solvent.
5) static to carry out vacuum breaker after ten minutes and vacuumize, continuous 15 times.Nitrogen or argon gas are wherein used when vacuum breaker
Protection.
6) pole piece is immersed in solvent, is shelved under protective atmosphere 12 hours.
7) it reads pole piece and immerses the volume V after solvent4=12092mm3。
8) porosity
ηHole=(V1+V2+V3-V4)/V1=(5558.14mm3+645.1mm3+8000mm3-12092mm3)/5558.14mm3×100%=
37.98%,
I.e. the porosity of positive plate coating is 37.98%.
Embodiment 2
By taking graphite cathode as an example, cathode pole piece step is prepared:
1) according to battery recipe requirements, slurry preparation is carried out.It include: artificial graphite, carbon black, CMC, SBR, deionization in slurry
Water；
2) slurry is coated on foil, and is dried and forms pole piece, copper foil surface density is 73g/m2, copper thickness is 8 μm,
Control pole piece coat side density is 220g/m2, control pole piece moisture content is less than 800ppm；
3) carrying out roll-in to pole piece after drying is compacted coating, and roll-in is compacted with a thickness of 141 μm as 1.58g/cm3。
Calculate the testing procedure of coating porosity are as follows:
1) pole piece width is 58mm, pole coating volume after roll-in
V1=761mm × 58mm × (0.141mm-0.008mm/(1+0.13%)=5870.81mm3,
Copper foil volume
V2=761mm × 58mm × 0.008mm/(1+0.13%)=352.65mm3。
2) a certain amount of solvent dimethyl carbonate, volume V are taken3=9000mm3。
3) solvent is put into the container of closed vacuum-pumping, while pole piece being also placed in the container, but pole piece not with
Solvent contact.
4) container is vacuumized, when vacuum degree reaches -0.09MPa, pole piece is immersed in solvent.
5) static to carry out vacuum breaker after ten minutes and vacuumize, continuous 18 times.Nitrogen or argon gas are wherein used when vacuum breaker
Protection.
6) pole piece is immersed in solvent, is shelved under protective atmosphere 12 hours.
7) it reads pole piece and immerses the volume V after solvent4=13078mm3。
8) porosity
ηHole=(V1+V2+V3-V4)/V1
=(5870.81mm3+352.65mm3+9000mm3-13078mm3)/5870.81mm3×100%
=36.54%,
I.e. the porosity of negative electrode tab coating is 36.54%.
By the test of pole coating porosity, the careful design that additional amount is needed to electrolyte, coating porosity are realized
Measuring and calculation, be to after roll-in pole piece immerse solvent test, can accurately more test out porosity profiles, it is possible to reduce it is some not
Determine the influence of factor.Compared with conventional mercury injection apparatus test method, this method has that testing efficiency is high, low excellent of measurement cost
Point.
Claims (6)
1. a kind of test method of electrodes of lithium-ion batteries coating porosity, which comprises the following steps:
1) foil is prepared, in foil surface coating slurry, roll-in is carried out to the foil for being coated with slurry and forms pole piece,
2) pole piece is taken to calculate its coating volume V1, foil volume V2；
3) a certain amount of solvent, volume V are taken3, solvent is put into the container of closed vacuum-pumping, while pole piece also being put
Enter in the container, but pole piece is not contacted with solvent；
4) container is vacuumized, when vacuum degree reaches -0.09MPa, pole piece is immersed in solvent；
5) static to carry out vacuum breaker after ten minutes and vacuumize, wherein using nitrogen or argon gas protection when vacuum breaker；
6) pole piece is immersed in solvent, is shelved under protective atmosphere 12 ~ 36 hours；
7) it reads pole piece and immerses the volume V after solvent4；
8) porosity ηHole=(V1+V2+V3-V4)/V1×100%。
2. the test method of electrodes of lithium-ion batteries coating porosity according to claim 1, which is characterized in that carry out brokenly true
It is empty and vacuumize and be carried out continuously 10 ~ 20 times.
3. the test method of electrodes of lithium-ion batteries coating porosity according to claim 1, which is characterized in that in step 1)
Slurry carries out slurry preparation according to cell size recipe requirements, is dried to form pole piece after slurry is coated on foil,
It controls pole piece moisture content and is less than 800ppm, carrying out roll-in to pole piece after drying is compacted coating, ultimately forms pole piece.
4. the test method of electrodes of lithium-ion batteries coating porosity according to claim 3, which is characterized in that in step 1)
Slurry in include: active material, conductive agent, binder, solvent.
5. the test method of electrodes of lithium-ion batteries coating porosity according to claim 4, which is characterized in that in slurry also
There are thickener or dispersing agent.
6. the test method of electrodes of lithium-ion batteries coating porosity according to claim 5, which is characterized in that cell size
Middle active material is LiFePO4, in nickel-cobalt-manganese ternary material, cobalt acid lithium material, lithium manganate material, graphite, silicon-carbon cathode material
One kind, the conductive agent is one of carbon black, carbon nanotube, active carbon, and the binder is one of PVDF, SBR,
The thickener is CMC, and dispersing agent is polyvinylpyrrolidone, and the solvent is N-methyl pyrrolidones, deionized water, anhydrous
One of ethyl alcohol, acetone, dimethyl carbonate, diethyl carbonate, ethylene carbonate or a variety of mixing.
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Cited By (6)
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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 |
| 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 |
| CN113959899A (en) * | 2021-10-11 | 2022-01-21 | 常州市大成真空技术有限公司 | Wet coating layer surface density measuring method and measuring system and electronic equipment |
| CN116625907A (en) * | 2023-07-24 | 2023-08-22 | 中国矿业大学(北京) | Method for testing porosity of lithium ion battery diaphragm |
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| 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 |
| CN113959899A (en) * | 2021-10-11 | 2022-01-21 | 常州市大成真空技术有限公司 | Wet coating layer surface density measuring method and measuring system and electronic equipment |
| CN116625907A (en) * | 2023-07-24 | 2023-08-22 | 中国矿业大学(北京) | Method for testing porosity of lithium ion battery diaphragm |
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