CN114136849A - Granularity test method of ternary cathode material - Google Patents
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- 239000010406 cathode material Substances 0.000 title claims abstract description 35
- 238000010998 test method Methods 0.000 title abstract description 12
- 238000012360 testing method Methods 0.000 claims abstract description 71
- 239000002245 particle Substances 0.000 claims abstract description 58
- 239000006185 dispersion Substances 0.000 claims abstract description 32
- 239000010405 anode material Substances 0.000 claims abstract description 18
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims abstract description 17
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims abstract description 17
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 11
- 239000007774 positive electrode material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001507 sample dispersion Methods 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910013716 LiNi Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process 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
- 229910052744 lithium Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means
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- Chemical & Material Sciences (AREA)
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Abstract
The invention provides a granularity testing method of a ternary cathode material. The test method comprises the following steps: mixing and dispersing the ternary anode material to be detected, sodium hexametaphosphate and a solvent to obtain a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid, and carrying out laser diffraction test to obtain the granularity of the ternary anode material to be detected. According to the invention, sodium hexametaphosphate and the ternary cathode material are mixed and dispersed, so that the agglomeration phenomenon among particles can be better broken under the premise of not damaging the particle morphology of a sample, the dispersion effect is more stable, and the accuracy of particle size testing is further improved.
Description
Technical Field
The invention belongs to the technical field of powder particle size testing, and relates to a particle size testing method of a ternary cathode material.
Background
With the increasingly prominent problems of energy crisis, environmental pollution and the like, the development of sustainable new energy becomes urgent for building a low-carbon society. Lithium ion batteries are receiving much attention as a new type of high-energy green batteries. The lithium battery has the advantages of high voltage and high capacity, and has long cycle life, low cost and other features.
The anode material has a bottleneck that restricts the large-scale popularization and application of the lithium ion battery due to high price and low specific capacity, and the structural stability of the single crystal material can not only improve the cycle stability of the battery, but also is very important for the safety of the battery. Under this requirement, an important factor, i.e., the particle size of the material in the electrode, must be considered in the battery design, as this helps determine the power and capacity of the battery.
The electrical property and the processing property of the lithium ion battery anode material are influenced by the physical properties of the lithium ion battery anode material, and particularly, the size of the particle size distribution has great influence on the safety performance of the battery and the compaction density of a pole piece.
In order to obtain the correct data on primary particle size, it is often necessary to break up agglomerated particles, form the particle monomers and disperse them uniformly in the medium in the particle size test, where the requirement for particle dispersion is "dispersion without segregation".
In the prior art, the problems exist in the test by adopting the laser diffraction technology, the anode material is not easy to disperse, bubbles are easy to generate in the ultrasonic process, the dispersion effect is unstable, and the data fluctuation is large; the requirement on the particle size is obviously limited, and the particles less than 5 mu m are greatly influenced by a dispersion method in the aspect of the particle size.
CN107565098A provides a method for rapidly evaluating the stability of a lithium ion battery anode material, which comprises the following steps: (1) assembling a battery, circulating a small current at normal temperature, and recharging to a test voltage; (2) taking out the pole piece from the glove box, cleaning and drying; rapidly measuring electrolyte according to a certain active substance/electrolyte ratio, putting the electrolyte into a closed container, adding the cleaned pole piece, and sealing; placing the closed container at a set temperature for a certain time; (3) after the placement, putting the closed container into a glove box, taking out the electrolyte, transferring the electrolyte into a centrifugal tube, moving out of the glove box, and performing centrifugal separation; (4) taking a small amount of supernatant, digesting, transferring digestion liquid to a volumetric flask for constant volume, and testing the ion concentration by adopting ICP. The method needs to manufacture the anode material into a finished battery, has a long manufacturing period, needs to use an organic solvent in the testing process, has high cost, can cause environmental pollution, and is not suitable for industrial rapid detection.
CN106092837A discloses a method for effectively evaluating dispersion consistency of material components in a positive electrode plate of a battery, which comprises scraping powder from the positive electrode plate after coating the positive electrode, sampling, testing, comparing particle size distribution and particle size of raw materials, and comparing particle size distribution and particle size consistency of main active material in the positive electrode plate to evaluate consistency of the positive electrode plate of the battery. In the document, bubbles are easily generated in the ultrasonic process, so that the dispersion effect is unstable and the data fluctuation is large.
Therefore, how to improve the accuracy of the particle size test of the cathode material is a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a particle size testing method of a ternary cathode material. According to the invention, sodium hexametaphosphate and the ternary cathode material are mixed and dispersed, so that the agglomeration phenomenon among particles can be better broken under the premise of not damaging the particle morphology of a sample, the dispersion effect is more stable, and the accuracy of particle size testing is further improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a particle size testing method of a ternary cathode material, which comprises the following steps:
mixing and dispersing the ternary anode material to be detected, sodium hexametaphosphate and a solvent to obtain a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid, and carrying out laser diffraction test to obtain the granularity of the ternary anode material to be detected.
According to the invention, sodium hexametaphosphate and the ternary cathode material are mixed and dispersed, so that the agglomeration phenomenon among particles can be better broken on the premise of not damaging the particle morphology of a sample, the dispersion effect is more stable, then ultrasonic dispersion and laser diffraction test are carried out, the sample dispersion effect and data stability are obviously improved, and the accuracy of particle size test is further improved.
According to the testing method provided by the invention, if the lithium iron phosphate anode material is tested, agglomeration appears.
Preferably, the mass ratio of the ternary cathode material to be tested to the sodium hexametaphosphate is (2.5-6.5): 1, such as 2.5:1, 2.8:1, 3:1, 3.3:1, 3.5:1, 3.8:1, 4:1, 4.3:1, 4.5:1, 4.8:1, 5:1, 5.3:1, 5.5:1, 5.8:1, 6:1, 6.3:1 or 6.5: 1.
In the invention, the mass ratio of the ternary anode material to be tested to the sodium hexametaphosphate is too small, which is not beneficial to the dispersion of the materials, and the mass ratio is too large, which can cause the increase of the bubble content and the deviation of the test result.
Preferably, the solvent comprises water.
Preferably, the dispersion has a mass concentration of 5 to 10%, for example, 5%, 6%, 7%, 8%, 9%, 10%, or the like.
Preferably, the power of the ultrasound is 100-200W, such as 100W, 110W, 120W, 130W, 140W, 150W, 160W, 170W, 180W, 190W or 200W.
Preferably, the frequency of the ultrasound is 28 to 53HZ, such as 28HZ, 30HZ, 33HZ, 35HZ, 38HZ, 40HZ, 43HZ, 45HZ, 48HZ, 50HZ or 53HZ, and the like.
Preferably, the time of the ultrasonic treatment is 3-8 min, such as 3min, 4min, 5min, 6min, 7min or 8 min.
In the invention, the ultrasonic time is too short, which is not beneficial to the full dispersion of materials, the agglomeration of small particles and large particles can not be broken, and the too long ultrasonic time can cause more bubbles in the solution, thus the data is unstable.
Preferably, the light shielding degree in the laser diffraction test is 11-13%, such as 11%, 11.5%, 12%, 12.5% or 13%.
Preferably, in the laser diffraction test, the sample test snap number and the background test snap number are not set.
According to the invention, the arrangement can better avoid the occurrence of tail dragging peak, the repeatability and reproducibility of data can be well shown, the result is more authentic, repeated tests are avoided, and the purpose of saving resources is achieved.
Preferably, the stirring speed in the laser diffraction test is 2000 to 3000rpm, such as 2000rpm, 2100rpm, 2200rpm, 2300rpm, 2400rpm, 2500rpm, 2600rpm, 2700rpm, 2800rpm, 2900rpm, 3000rpm, or the like.
Preferably, the ternary positive electrode material includes a single crystal material and a polycrystalline material.
As a preferred technical solution, the test method includes:
mixing and dispersing a ternary cathode material to be tested, sodium hexametaphosphate and a solvent to obtain a dispersion liquid with the mass concentration of 5-10%, carrying out ultrasonic treatment on the dispersion liquid for 3-8 min at the ultrasonic power of 100-200W and the frequency of 28-53 HZ, carrying out laser diffraction test after ultrasonic treatment, canceling setting of a sample test snap number and a background test snap number, setting the stirring speed to be 2000-3000 rpm in the test process, and setting the light shielding degree to be 11-13%, so as to obtain the granularity of the ternary cathode material to be tested;
the mass ratio of the ternary anode material to be detected to the sodium hexametaphosphate is (2.5-6.5): 1, and the ternary anode material comprises a single crystal material and a polycrystalline material.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, sodium hexametaphosphate and the ternary cathode material are mixed and dispersed, so that the agglomeration phenomenon among particles can be better broken on the premise of not damaging the particle morphology of a sample, the dispersion effect is more stable, then ultrasonic dispersion and laser diffraction test are carried out, the sample dispersion effect and data stability are obviously improved, the accuracy of particle size test is further improved, the relative standard deviation in the D99 particle size range can be reduced to below 1.4%, and the method is suitable for actual production.
Drawings
Fig. 1 is a particle size distribution diagram of a ternary cathode material to be tested obtained by the test method provided in example 1.
Fig. 2 is a particle size distribution diagram of the ternary cathode material to be tested obtained by the test method provided in comparative example 1.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This implementationExample provides a single crystal ternary positive electrode material (LiNi) to be tested0.8Co0.1Mn0.1O2) The particle size test method of (a), the test method comprising:
(1) taking 0.2g of single crystal ternary cathode material to be detected, adding 1ml of sodium hexametaphosphate solution with the mass concentration of 5% for dispersion (the mass ratio of the ternary cathode material to be detected to the sodium hexametaphosphate is 4.5:1), dissolving with 60ml of pure water to obtain dispersion liquid, and then placing a beaker filled with the dispersion liquid in an ultrasonic machine for ultrasonic treatment at the ultrasonic frequency of 40HZ for 5min at the ultrasonic power of 160W;
(2) directly pouring the solution after ultrasonic treatment into a test beaker, washing with a wash bottle for auxiliary sample injection to ensure that the light shielding degree is 11-13%, stirring by a stirrer at the rotating speed of 2500rpm, canceling the arrangement of a sample test snap number and a background test snap number, setting the background test time for 10s, keeping three significant figures of test results, testing three times to obtain the result of each test, wherein the particle size data are shown in table 1, D10, D50, D90 and D99 of the single crystal ternary cathode material to be tested are respectively measured, and then further calculating to obtain the average value of the three tests, the Standard Deviation (SD) of the sample and the Relative Standard Deviation (RSD) of the sample, wherein the Relative Standard Deviation (RSD) is the Standard Deviation (SD)/the arithmetic average value (X) of the calculated result.
Comparative example 1
In this comparative example, the single crystal ternary positive electrode material to be tested was kept the same as in example 1. The test method comprises the following steps:
(1) dissolving 0.1g of the material in 20ml of pure water to obtain a dispersion, and performing ultrasonic treatment on the dispersion for 5min at the ultrasonic frequency of 53KHZ and the power of 120W;
(2) setting the test snap number to be 6000times and the background test snap number to be 6000times, setting the rotating speed of a stirrer to be 3000rpm, washing the auxiliary sample by using a sample spoon and a wash bottle to ensure that the light shading degree is between 8 and 12 percent, carrying out the test, wherein the particle size data are shown in table 2, respectively measuring D10, D50, D90 and D99 of the single crystal ternary cathode material to be tested, and further calculating to obtain the average value of three tests, the Standard Deviation (SD) of the sample and the Relative Standard Deviation (RSD) of the sample, wherein the Relative Standard Deviation (RSD) is the Standard Deviation (SD)/the arithmetic average value (X) of the calculated result.
Fig. 1 and 2 show particle size distribution diagrams of ternary cathode materials to be tested obtained by the test methods provided in example 1 and comparative example 1, respectively, and in comparison with fig. 1 and 2, the particle size distribution sample in comparative example 1 has unstable dispersion fluctuation and a tail peak of nearly 100 μm at the tail end, and the D99 data has large fluctuation; the method provided by the invention has the advantages that the particle size distribution consistency is good, the tailing peak at the tail end disappears, the D99 result is relatively stable, the repeatability and reproducibility of the D10, D50, D90 and D99 data are good, and the data are more authentic, so that repeated tests are avoided, and the purpose of saving resources is achieved.
Tables 1 and 2 are listed below, respectively:
TABLE 1
TABLE 2
The production uses the D99 (the volume content of the particles smaller than the grain diameter accounts for 99 percent of the total particles) index which is frequently used as the reference value of the grain diameter of the largest grain of the single crystal ternary cathode material.
As can be seen from the data results in tables 1 and 2, the data fluctuation of the test method provided by the present invention is small in different particle size ranges, and it can be seen that the data fluctuation is more and more obvious in the conventional test method as the range from D10 is gradually enlarged, and the test accuracy is more and more unstable.
And by comprehensively comparing D99 of example 1 and comparative example 1 and the standard deviation of the comparison, the particle size testing method provided by the invention realizes uniform dispersion of samples, the fluctuation of the testing result is small each time, and the testing accuracy is obviously improved.
In conclusion, the sodium hexametaphosphate and the ternary cathode material are mixed and dispersed, so that the agglomeration phenomenon among particles can be better broken on the premise of not damaging the particle morphology of a sample, the dispersion effect is more stable, ultrasonic dispersion and laser diffraction test are performed, the sample dispersion effect and the data stability are obviously improved, the accuracy of particle size test is improved, the relative standard deviation in the D99 particle size range can be reduced to below 1.4%, and the method is suitable for actual production.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A particle size testing method for a ternary cathode material is characterized by comprising the following steps:
mixing and dispersing the ternary anode material to be detected, sodium hexametaphosphate and a solvent to obtain a dispersion liquid, carrying out ultrasonic treatment on the dispersion liquid, and carrying out laser diffraction test to obtain the granularity of the ternary anode material to be detected.
2. The method for testing the particle size of the ternary cathode material as claimed in claim 1, wherein the mass ratio of the ternary cathode material to be tested to sodium hexametaphosphate is (2.5-6.5): 1;
preferably, the solvent comprises water.
3. The method for testing the particle size of the ternary positive electrode material according to claim 1 or 2, wherein the dispersion liquid has a mass concentration of 5 to 10%.
4. The method for testing the particle size of the ternary cathode material according to any one of claims 1 to 3, wherein the power of the ultrasound is 100 to 200W.
5. The method for testing the particle size of the ternary cathode material according to any one of claims 1 to 4, wherein the frequency of the ultrasound is 28 to 53 HZ.
6. The method for testing the particle size of the ternary cathode material according to any one of claims 1 to 5, wherein the time for the ultrasonic treatment is 3 to 8 min.
7. The method for testing the particle size of the ternary cathode material according to any one of claims 1 to 6, wherein the light shielding degree in the laser diffraction test is 11 to 13%;
preferably, in the laser diffraction test, the sample test snap number and the background test snap number are not set.
8. The method for testing the particle size of the ternary cathode material according to any one of claims 1 to 7, wherein the stirring speed in the laser diffraction test is 2000 to 3000 rpm.
9. The method for testing the grain size of a ternary cathode material according to any of claims 1 to 8, wherein the ternary cathode material comprises a single crystal material and a polycrystalline material.
10. The method for testing the particle size of a ternary positive electrode material according to any one of claims 1 to 9, characterized in that it comprises:
mixing and dispersing a ternary cathode material to be tested, sodium hexametaphosphate and a solvent to obtain a dispersion liquid with the mass concentration of 5-10%, carrying out ultrasonic treatment on the dispersion liquid for 3-8 min at the ultrasonic power of 100-200W and the frequency of 28-53 HZ, carrying out laser diffraction test after ultrasonic treatment, canceling setting of a sample test snap number and a background test snap number, setting the stirring speed to be 2000-3000 rpm in the test process, and setting the light shielding degree to be 11-13%, so as to obtain the granularity of the ternary cathode material to be tested;
the mass ratio of the ternary anode material to be detected to the sodium hexametaphosphate is (2.5-6.5): 1, and the ternary anode material comprises a single crystal material and a polycrystalline material.
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