CN112362549A - Method for measuring porosity of lithium ion battery pole piece - Google Patents
Method for measuring porosity of lithium ion battery pole piece Download PDFInfo
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- CN112362549A CN112362549A CN201911356964.9A CN201911356964A CN112362549A CN 112362549 A CN112362549 A CN 112362549A CN 201911356964 A CN201911356964 A CN 201911356964A CN 112362549 A CN112362549 A CN 112362549A
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- 238000000034 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 19
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 19
- 239000011261 inert gas Substances 0.000 claims abstract description 10
- 239000004482 other powder Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- 239000011888 foil Substances 0.000 claims description 14
- 239000001307 helium Substances 0.000 claims description 12
- 229910052734 helium Inorganic materials 0.000 claims description 12
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 12
- 238000004364 calculation method Methods 0.000 claims description 8
- 239000011149 active material Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000012360 testing method Methods 0.000 abstract description 15
- 239000007773 negative electrode material Substances 0.000 abstract description 3
- 239000007774 positive electrode material Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 17
- 239000011148 porous material Substances 0.000 description 14
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 13
- 229910052753 mercury Inorganic materials 0.000 description 11
- 238000001179 sorption measurement Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 3
- 238000013178 mathematical model Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011236 particulate material Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229940008718 metallic mercury Drugs 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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 invention discloses a method for measuring the porosity of a lithium ion battery pole piece, which comprises the following steps: taking an object to be measured, and measuring its volume V0(ii) a Injecting a certain amount of inert gas into a sample cell of the true density instrument; placing an object to be measured into a sample cell of a true density instrument, and measuring to obtain a true volume V; and calculating to obtain the porosity of the pole piece. The technical scheme is based on the Bohr's law of inert gases under certain conditions, and the true volume of the sample is accurately measured by means of a true density instrument, so that the true density is obtained, and the method is safe, nontoxic, simple, convenient and effective in the test process and low in test cost, and is used for measuring the porosity of the positive and negative electrode plates, the blocky regular solid and the diaphragm of the positive and negative electrode materials in the lithium ion battery and the porosity of any other powder or solid with an apparent volume known.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a method for measuring the porosity of a lithium ion battery pole piece.
Background
Data show that in the production process of the lithium ion battery, the porosity of the pole piece and the porosity of the raw material are obviously different through the processes of slurry preparation, coating, pole piece rolling, slitting, drying and the like, and the porosity performance of the raw material cannot represent the porosity of the final pole piece. The compacted density of the pole piece subjected to the rolling process is improved, and the volume energy density and the weight energy density of the pole are increased. However, if the pressure in the rolling process is too high, the porosity of the pole piece is reduced, so that the electrolyte is difficult to permeate into the pole piece, and the utilization rate of the specific capacity of the pole piece material is reduced. The polarization degree of the battery with poor liquid retention capacity in the circulation process is also increased, the attenuation is accelerated, and the internal resistance is obviously increased. Therefore, the porosity of the pole piece is critical to the battery performance.
The common methods for measuring porosity are mercury intrusion methods and gas adsorption methods. Mercury intrusion methods use mercury intrusion gauges to characterize most particulate and solid materials. By pressurizing, liquid mercury is injected into the hole, the size of the pore diameter is in a function relationship with the applied pressure, and information such as the size, the pore diameter distribution, the volume and the like of the pore in the material can be deduced according to the measured pressure. The metallic mercury used in the measurement process is extremely toxic and volatile, and the mercury vapor entering the air can cause serious health hazards after being inhaled by a human body. Meanwhile, when the positive and negative electrode plates of the lithium ion battery are measured by a mercury pressing method, aluminum foil or copper foil in the electrode plates can generate an amalgam reaction with mercury, and the measurement result of the porosity of the electrode plates is influenced. Therefore, the method for measuring the porosity of the pole piece by using the mercury intrusion instrument has the problems of safety, test accuracy and the like.
Gas adsorption processes are generally applicable to particulate materials. The adsorption capacity of the material to gas under different pressures is measured under isothermal condition to obtain an adsorption curve, and the pore volume of the material is calculated by applying a proper mathematical model. In order to achieve sufficient adsorption of the gas onto the solid surface, the solid must generally be cooled to the boiling point of the adsorbed gas at the time of measurement. When measuring porosity by a gas adsorption method, a mathematical model BET analytic adsorption curve of a polymolecular layer adsorption theory is commonly used, so that the pore volume is calculated. However, the BET model is generally only applicable to adsorption curves generated by mesoporous solids or non-porous, macroporous solids. Meanwhile, the upper limit of measurement of the gas adsorption method is lower than 500nm, the effective analysis range is only 100nm, and most of macropores and gaps among particles cannot be covered. The method is also limited to porosity determination of powder solids and cannot be used for bulk solids.
Chinese patent document CN103278438B discloses a method for testing the effective pore volume and porosity of a lithium ion battery pole piece. The effective pore volume and porosity of the pole piece are calculated by testing the total pore volume and the real volume of the pole piece after the pores are filled with liquid, and the method comprises the following steps: the method comprises the steps of firstly testing the total pore volume Vt of a pole piece, testing the true volume Vz of the pole piece, and then calculating the effective pore volume and the effective porosity. According to the technical scheme, the enlargement of gaps caused by the volume expansion of the pole piece in the pole piece soaking process is ignored, and the quality reduction caused by the volatilization of the soaking solution after the pole piece is taken out is also ignored, so that the real porosity of the pole piece is influenced.
Disclosure of Invention
The invention mainly solves the technical problem that the original immersion liquid influences the real porosity of a pole piece, and provides a method for measuring the porosity of a lithium ion battery pole piece.
The technical problem of the invention is mainly solved by the following technical scheme: the invention comprises the following steps:
(1) taking an object to be measured, and measuring its volume V0(ii) a Measuring the apparent volume V of an object to be measured0For calculating the porosity.
(2) Injecting a certain amount of inert gas into a sample cell of the true density instrument; inert gas is used to avoid reaction with the object to be measured and influence the pore state of the object to be measured before and after measurement.
(3) Placing an object to be measured into a sample cell of a true density instrument, and measuring to obtain a true volume V;
(4) and calculating to obtain the porosity of the pole piece.
Preferably, the object to be measured in step (1) comprises positive and negative electrode plates, blocky regular solids of positive and negative electrode materials, a diaphragm and any other powder or solid with a known apparent volume. Based on the Bohr's law of inert gas under certain conditions, the true density instrument can accurately measure the true volume of a sample by measuring the change of the gas volume of the sample cell caused by the sample placed in the sample cell, so that the true density is obtained, the true density instrument has no requirement on the shape state of an object to be measured, and the true density instrument has wide application range.
Preferably, the apparent volume V of the solid with regular apparent shape in the step (1) is obtained by a volume calculation formula0。
Preferably, the inert gas in step (2) is helium. Compared with nitrogen, helium has smaller molecular diameter and wider accessible pore range, so that the measured real volume is more accurate.
Preferably, the helium gas pressure in step (2) is 18 PSI. The helium gas pressure is set to 18PSI, so that helium gas is prevented from escaping to influence the measurement result.
Preferably, the step (3) sets a plurality of groups of objects to be measured to respectively perform measurement. And a plurality of groups of objects to be measured are arranged to obtain an average value, so that the accuracy of the measured porosity is ensured, and the error is reduced.
Preferably, said step (3) is performed at room temperature while measuring the true volume V. The state of the pole piece is closer to the state of normal work during measurement, and the measured real volume V is more accurate.
Preferably, in the step (4), the porosity p calculated by the plurality of groups of objects to be measured is averaged to obtain a final result, and the calculation formula of the porosity p is as follows:
wherein, V0Apparent volume of the pole piece, including activity on the pole pieceVolume of material and volume of aluminum foil, V0' is the apparent volume of active material on the pole piece, i.e. the apparent volume V0The difference in volume from the aluminum foil. By default there are no voids in the aluminum foil, several sets of data were measured and averaged to reduce error.
The invention has the beneficial effects that: based on the Bohr's law of inert gases under certain conditions, the real volume of a sample is accurately measured by a real density instrument, so that the real density is obtained, and the method is safe, non-toxic, simple, convenient and effective in the test process and low in test cost, and is used for measuring the porosity of positive and negative pole pieces, blocky regular solids of positive and negative pole materials, diaphragms and other powder or solids with known apparent volumes in lithium ion batteries.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments.
Comparative example: the method for measuring the porosity of the lithium ion battery pole piece comprises the following steps:
(1) taking an object to be measured, and measuring its volume V0Wherein the object to be measured comprises positive and negative electrode plates, blocky regular solid of positive and negative electrode materials, a diaphragm and any other powder or solid with an appreciable volume, and the apparent volume V of the solid with the regular apparent shape is obtained by a volume calculation formula0. The pole piece comprises an active material and an aluminum foil, when the porosity of the active material on the pole piece is calculated, the volume of the aluminum foil needs to be removed, and no gap is reserved in the aluminum foil. Based on the Bohr's law of inert gas under certain conditions, the true density instrument can accurately measure the true volume of a sample by measuring the change of the gas volume of the sample cell caused by the sample placed in the sample cell, so that the true density is obtained, the true density instrument has no requirement on the shape state of an object to be measured, and the true density instrument has wide application range.
(2) The pressure of helium gas injected into the sample cell of the true densitometer was 18 PSI. Compared with nitrogen, helium has smaller molecular diameter and wider accessible pore range, so that the measured real volume is more accurate. The helium gas pressure is set to 18PSI, so that helium gas is prevented from escaping to influence the measurement result.
(3) And arranging a plurality of groups of objects to be measured, sequentially placing the objects to be measured into a sample cell of the true density instrument at room temperature, and measuring to obtain the true volume V. And a plurality of groups of objects to be measured are arranged to obtain an average value, so that the accuracy of the measured porosity is ensured, and the error is reduced. The test at room temperature makes the state of the pole piece closer to the state of normal work when in measurement, and the measured real volume V is more accurate.
(4) And averaging the porosity p calculated by a plurality of groups of objects to be detected to obtain a final result. The porosity p is calculated as:
wherein, V0Is the apparent volume of the pole piece, including the volume of active material on the pole piece and the volume of aluminum foil, V0' is the apparent volume of active material on the pole piece, i.e. the apparent volume V0The difference in volume from the aluminum foil.
Comparative example 1:
taking a positive pole piece with the width of 20cm and the length of 30cm, and measuring the thickness h of the positive pole piece by using a micrometer0The thickness measurement points are evenly distributed. Taking the raw material aluminum foil of the pole piece, and measuring the thickness h of the raw material aluminum foil by using a micrometer1The thickness measurement points are evenly distributed. 3 pole piece samples with the width of 2cm and the length of 30cm are cut by using a cutting knife. The real volume V of each of the 3 pole piece samples was measured using a Contareal densitometer Upyc 1200 e. The test conditions of the true density instrument are as follows: the test was performed at room temperature using a small sample cell using helium gas pressure 18Psi, with the test results averaged 3 runs and the deviation range set to 0.05. The porosity p is calculated as:
and n is the number of pole pieces in single measurement.
The porosity of the pole piece obtained by measurement and calculation is shown in the following table.
TABLE-porosity measurement results
Comparative example 2:
the difference between the comparative example 2 and the comparative example 1 is that 6 pole piece samples are cut and divided into 3 groups, each group comprises 2 pole pieces, and the sample amount of 1 group is tested once. The other processes are the same as those of comparative example 1, and the same sample of the positive electrode sheet was used.
The porosity of the pole piece obtained by measurement and calculation is shown in the following table.
TABLE II porosity measurement results
Comparative example 3:
comparative example 3 differs from comparative example 1 in that 12 pole piece samples were cut into 3 groups of 4 pole pieces each, and 1 group of sample size was tested in a single run. The other processes are the same as those of comparative example 1, and the same sample of the positive electrode sheet was used.
The porosity of the pole piece obtained by measurement and calculation is shown in the following table.
TABLE TRI-POROSITY MEASUREMENT RESULTS
From the results of comparative example 1, comparative example 2 and comparative example 3, the porosity results were obtained by measuring the porosity of the pole piece by a true densitometer. When the sample amount in the determination process is 2 pole piece samples with the width of 2cm and the length of 30cm, stable and effective porosity results can be obtained, and the standard deviation of the porosity is 0.05%.
The same positive electrode sheet sample of the example was used and the sample was cut to a size of less than 4mm x 5 mm. 3 samples with a mass of about 1.3g were weighed. And testing the porosity of the pole piece by a mercury porosimeter. The mercury porosimeter is model number American microphone AutoPore IV 9510. The porosity of the pole pieces obtained by the test is shown in the following table.
TABLE four porosity measurement results
As can be seen from comparative example 4, the measurement result of the mercury porosimeter is greater than that of comparative example 1, comparative example 2 and comparative example 3, and the result stability is poor, possibly due to the reaction of the aluminum foil with mercury.
Claims (8)
1. A method for measuring the porosity of a lithium ion battery pole piece is characterized by comprising the following steps:
(1) taking an object to be measured, and measuring its volume V0；
(2) Injecting a certain amount of inert gas into a sample cell of the true density instrument;
(3) placing an object to be measured into a sample cell of a true density instrument, and measuring to obtain a true volume V;
(4) and calculating to obtain the porosity of the pole piece.
2. The method for measuring the porosity of the lithium ion battery pole piece according to claim 1, wherein the objects to be measured in the step (1) comprise positive and negative pole pieces, blocky regular solids of positive and negative pole materials, a diaphragm and any other powder or solid with an apparent volume known.
3. The method for measuring the porosity of the lithium ion battery pole piece according to claim 2, wherein the solid with regular apparent shape in the step (1) is tabulated through a volume calculation formulaVolume V0。
4. The method for measuring the porosity of the lithium ion battery pole piece according to claim 1, wherein the inert gas in the step (2) is helium.
5. The method of claim 4, wherein the helium gas pressure in step (2) is 18 PSI.
6. The method for determining the porosity of the lithium ion battery pole piece according to claim 2, wherein the step (3) is implemented by setting a plurality of groups of objects to be measured respectively.
7. The method for measuring the porosity of the lithium ion battery pole piece according to claim 2, wherein the step (3) is performed at room temperature when the real volume V is measured.
8. The method for measuring the porosity of the lithium ion battery pole piece according to claim 2, wherein in the step (4), the porosity p calculated by a plurality of groups of objects to be measured is averaged to obtain a final result, and the calculation formula of the porosity p is as follows:
wherein, V0Is the apparent volume of the pole piece, including the volume of active material and the volume of aluminum foil, V'0Is the apparent volume of active material on the pole piece, i.e. the apparent volume V0The difference in volume from the aluminum foil.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113607624A (en) * | 2021-09-02 | 2021-11-05 | 山东圣阳电源股份有限公司 | Porosity measurement method, device, equipment and system |
| CN113945502A (en) * | 2021-10-22 | 2022-01-18 | 蜂巢能源科技有限公司 | Porosity testing tool and testing method thereof |
| CN113959902A (en) * | 2021-09-14 | 2022-01-21 | 陕西创普斯新能源科技有限公司 | Method for measuring true density of lithium iron phosphate powder |
| 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 |
| CN115112544A (en) * | 2022-08-29 | 2022-09-27 | 江苏时代新能源科技有限公司 | Method for detecting porosity of substance to be detected |
| JP7409221B2 (en) | 2020-05-14 | 2024-01-09 | Dic株式会社 | Method for measuring surface unevenness distribution |
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| CN115112544A (en) * | 2022-08-29 | 2022-09-27 | 江苏时代新能源科技有限公司 | Method for detecting porosity of substance to be detected |
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