CN109904430B - Mixing method of graphite cathode slurry - Google Patents
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Abstract
The invention provides a mixing method of graphite cathode slurry, which comprises a first graphite material, a second graphite material and a third graphite material, wherein the average particle size of the first graphite material is d1, the average particle size of the second graphite material is d2, the average particle size of the third graphite material is d3, d1< d2< d3, and d2 ═ k (d1+ d 3); the k is a, (c1+ c3)/(c2+0.5), the a is an equilibrium constant, 1.1 is equal to or less than 1.3, the c1, c2 and c3 are the respective component percentages of the first graphite material, the second graphite material and the third graphite material, c1+ c2+ c3 is equal to 1, and c1+ c2 is equal to or less than c 3. The mixing method comprises the steps of mixing a first graphite material, a second graphite material and a third graphite material respectively to obtain three kinds of slurry, and then mixing the three kinds of slurry according to a specific sequence to obtain the graphite cathode slurry with good dispersity. The graphite cathode slurry has the advantages of high graphite dispersity, no agglomeration, no sedimentation, high storage stability, high energy density and good rate capability.
Description
Technical Field
The invention relates to the technical field of lithium ion battery production, in particular to a mixing method of graphite cathode slurry.
Background
The power battery has the advantages of high energy density, high power, environmental protection and the like, and is commonly used in the field of electric vehicles. The negative electrode of the power battery is generally a graphite negative electrode, and the requirements on the graphite negative electrode are high in energy density and good in rate capability, researchers find that the negative electrode with higher compaction density can be obtained by mixing graphite particles with different average particle sizes to prepare a mixed negative electrode, so that the energy density of the negative electrode is improved, but the slurry of the power battery has the problems that the mixing process is difficult due to the existence of the graphite particles with various particle sizes, the dispersion is not uniform easily, the sedimentation phenomenon is obvious, and the coating quality is influenced.
Disclosure of Invention
The inventors have found through studies that a graphite material having a plurality of particle sizes and having a component content within a specific range, which can be smoothly blended and which does not cause the phenomena of agglomeration and sedimentation, is excellent in dispersibility and is extremely high in stability, is provided.
On the basis, the invention provides a mixing method of graphite cathode slurry, the graphite cathode slurry comprises a first graphite material, a second graphite material and a third graphite material, wherein the average particle size of the first graphite material is d1, the average particle size of the second graphite material is d2, the average particle size of the third graphite material is d3, d1< d2< d3, and d2 ═ k (d1+ d 3); the k is a (c1+ c3)/(c2+0.5), the a is an equilibrium constant, 1.1 is equal to or less than 1.3, the c1, c2 and c3 are the respective component percentages of the first graphite material, the second graphite material and the third graphite material, c1+ c2+ c3 is equal to 1, and c1+ c2 is equal to or less than c 3. The mixing method comprises the steps of mixing a first graphite material, a second graphite material and a third graphite material respectively to obtain three kinds of slurry, and then mixing the three kinds of slurry according to a specific sequence to obtain the graphite cathode slurry with good dispersity. The graphite cathode slurry has the advantages of high graphite dispersity, no agglomeration, no sedimentation, high storage stability, high energy density and good rate capability.
The specific scheme is as follows:
a method of compounding a graphite anode slurry comprising a first graphite material, a second graphite material, a third graphite material, wherein the first graphite material has an average particle size of d1, the second graphite material has an average particle size of d2, the third graphite material has an average particle size of d3, wherein d1< d2< d3, and d2 ═ k (d1+ d 3); the k is a (c1+ c3)/(c2+0.5), the a is an equilibrium constant, 1.1 is equal to or less than 1.3, the c1, c2 and c3 are the first graphite material, the second graphite material and the third graphite material respectively, the c1+ c2+ c3 is equal to 1, and the c1+ c2 is equal to or less than c3, and the method comprises the following steps:
1) adding a solvent into a first stirring kettle, adding a binder, and stirring; adding the three graphite materials into a first stirring kettle according to the mass ratio, stirring, then adding the first graphite material into the first stirring kettle according to the mass ratio, and stirring to obtain first slurry;
2) adding the solvent into a second stirring kettle, adding the binder, and stirring; adding the second graphite material and the conductive agent into a second stirring kettle according to the mass ratio, and stirring to obtain second slurry;
3) and adding the first slurry into the second slurry according to the mass ratio under the condition of keeping the continuous stirring of the second stirring kettle, and stirring to obtain the graphite cathode slurry.
Further, the d1 is 0.5-1 micron, and the d3 is 6-6.5 micron.
Furthermore, c1 is more than or equal to 0.05 and less than or equal to 0.1, and c3 is more than or equal to 0.1 and less than or equal to 0.3.
Further, the conductive agent is carbon nanotubes or carbon nanofibers.
Further, the length of the carbon nano tube or the carbon nano fiber is 5-15 micrometers.
Further, wherein the mass ratio in the graphite slurry is such that the ratio of the graphite material: conductive agent: the binder is 100:4-6: 3-5.
Further, the solvent is water, and the binder is SBR.
The invention has the following beneficial effects:
1) the inventor finds that when the particle size and the component content of the graphite are in a specific range, the graphite can be mixed smoothly, and agglomeration and sedimentation phenomena cannot occur;
2) through multiple experiments, the inventor finds that in the material mixing process, the first graphite particles and the third graphite particles are firstly mixed to prepare slurry, and then the slurry prepared by the second graphite particles is mixed to better realize dispersion;
3) the linear conductive agent is used as the conductive agent, so that the stability of the slurry is improved, and the conductive agent is mixed with the second graphite particles with the largest weight part, so that the dispersion of the linear conductive agent is facilitated;
4) the invention has simple material mixing process, easy operation, high stability of the prepared slurry and good coating performance.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
Providing a first graphite material, a second graphite material and a third graphite material, wherein the average particle size d1 of the first graphite material is 1 micron, the average particle size d2 of the second graphite material is 3 microns, the average particle size d3 of the third graphite material is 6 microns, the percentage content c1 of the first graphite material is 10%, the percentage content c2 of the second graphite material is 60%, and the percentage content c3 of the third graphite material is 30%;
1) adding water into the first stirring kettle, adding SBR, and stirring for 4 hours; adding the three graphite materials into a first stirring kettle according to the mass ratio, stirring for 6 hours, then adding the first graphite material into the first stirring kettle according to the mass ratio, and stirring for 6 hours to obtain first slurry;
2) adding water into a second stirring kettle, adding SBR, and stirring for 4 hours; adding the second graphite material and the carbon nano tubes with the length of 15 micrometers into a second stirring kettle according to the mass ratio, and stirring for 6 hours to obtain second slurry;
3) and adding the first slurry into the second slurry according to the mass ratio under the condition of keeping the continuous stirring of the second stirring kettle, and stirring for 4 hours to obtain graphite cathode slurry, wherein the mass ratio of the graphite slurry is as follows: carbon nanotube: binder 100:4: 5.
Example 2
Providing a first graphite material, a second graphite material and a third graphite material, wherein the average particle size d1 of the first graphite material is 0.5 microns, the average particle size d2 of the second graphite material is 1.7 microns, the average particle size d3 of the third graphite material is 6.5 microns, the percentage content c1 of the first graphite material is 5%, the percentage content c2 of the second graphite material is 75%, and the percentage content c3 of the third graphite material is 20%;
1) adding water into the first stirring kettle, adding SBR, and stirring for 4 hours; adding the three graphite materials into a first stirring kettle according to the mass ratio, stirring for 6 hours, then adding the first graphite material into the first stirring kettle according to the mass ratio, and stirring for 6 hours to obtain first slurry;
2) adding water into a second stirring kettle, adding SBR, and stirring for 4 hours; adding the second graphite material and the carbon nano tubes with the length of 5-15 micrometers into a second stirring kettle according to the mass ratio, and stirring for 6 hours to obtain second slurry;
3) and adding the first slurry into the second slurry according to the mass ratio under the condition of keeping the continuous stirring of the second stirring kettle, and stirring for 4 hours to obtain graphite cathode slurry, wherein the mass ratio of the graphite slurry is as follows: carbon nanotube: binder 100:6: 3.
Example 3
Providing a first graphite material, a second graphite material and a third graphite material, wherein the average particle size d1 of the first graphite material is 1 micron, the average particle size d2 of the second graphite material is 2.1 microns, the average particle size d3 of the third graphite material is 6 microns, the percentage content c1 of the first graphite material is 10%, the percentage content c2 of the second graphite material is 70%, and the percentage content c3 of the third graphite material is 20%;
1) adding water into the first stirring kettle, adding SBR, and stirring for 4 hours; adding the three graphite materials into a first stirring kettle according to the mass ratio, stirring for 6 hours, then adding the first graphite material into the first stirring kettle according to the mass ratio, and stirring for 6 hours to obtain first slurry;
2) adding water into a second stirring kettle, adding SBR, and stirring for 4 hours; adding the second graphite material and the carbon nano tubes with the length of 10 micrometers into a second stirring kettle according to the mass ratio, and stirring for 6 hours to obtain second slurry;
3) and adding the first slurry into the second slurry according to the mass ratio under the condition of keeping the continuous stirring of the second stirring kettle, and stirring for 4 hours to obtain graphite cathode slurry, wherein the mass ratio of the graphite slurry is as follows: carbon nanotube: binder 100:5: 4.
Example 4
Providing a first graphite material, a second graphite material and a third graphite material, wherein the average particle size d1 of the first graphite material is 1 micron, the average particle size d2 of the second graphite material is 3 microns, the average particle size d3 of the third graphite material is 6 microns, the percentage content c1 of the first graphite material is 10%, the percentage content c2 of the second graphite material is 60%, and the percentage content c3 of the third graphite material is 30%;
1) adding water into the first stirring kettle, adding SBR, and stirring for 4 hours; adding the three graphite materials into a first stirring kettle according to the mass ratio, stirring for 6 hours, then adding the first graphite material into the first stirring kettle according to the mass ratio, and stirring for 6 hours to obtain first slurry;
2) adding water into a second stirring kettle, adding SBR, and stirring for 4 hours; adding the second graphite material and the carbon nano tubes with the length of 10 micrometers into a second stirring kettle according to the mass ratio, and stirring for 6 hours to obtain second slurry;
3) and adding the first slurry into the second slurry according to the mass ratio under the condition of keeping the continuous stirring of the second stirring kettle, and stirring for 4 hours to obtain graphite cathode slurry, wherein the mass ratio of the graphite slurry is as follows: carbon nanotube: binder 100:5: 4.
Comparative example 1
A second graphite material was provided having an average particle size d2 of 2 microns with the same parameters as in example 1.
Comparative example 2
A second graphite material was provided having an average particle size d2 of 4 microns with the same parameters as in example 1.
Comparative example 3
Providing a first graphite material, a second graphite material and a third graphite material, wherein the average particle size d1 of the first graphite material is 1 micron, the average particle size d2 of the second graphite material is 3 microns, the average particle size d3 of the third graphite material is 6 microns, the percentage content c1 of the first graphite material is 10%, the percentage content c2 of the second graphite material is 60%, and the percentage content c3 of the third graphite material is 30%;
adding water into a stirring kettle, adding SBR, and stirring for 4 hours; adding the graphite material into the stirring kettle according to the mass ratio, and stirring for 16 hours to obtain graphite cathode slurry, wherein the mass ratio of the graphite material in the graphite slurry is as follows: carbon nanotube: binder 100:4: 5.
Test and results
The slurry of the adjusting example and the slurry of the comparative example are both around 50%, the solid content of the slurry 5cm below the top layer is measured at room temperature, and then the solid content of the slurry 5cm below the top layer is measured after the slurry is placed for 5 hours, 10 hours and 15 hours, the data are shown in table 1, and the slurry prepared by the method provided by the invention has good dispersibility and stability. The component content and particle size range of the graphite have a large influence on the stability of the slurry, and the mixing method of the invention also has a certain positive effect on the stability of the slurry.
TABLE 1
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.
Claims (5)
1. A mixing method of graphite cathode slurry, wherein the graphite cathode slurry comprises a first graphite material, a second graphite material and a third graphite material, wherein the average particle size of the first graphite material is d1, the average particle size of the second graphite material is d2, the average particle size of the third graphite material is d3, the d1 is 0.5-1 micron, and the d3 is 6-6.5 microns; wherein d1< d2< d3, and said d2 ═ k (d1+ d 3); the k is a, (c1+ c3)/(c2+0.5), a is an equilibrium constant, 1.1 is equal to or less than 1.3, c1, c2 and c3 are the first graphite material, the second graphite material and the third graphite material respectively in percentage, wherein 0.05 is equal to or less than c1 and equal to or less than 0.1, and 0.1 is equal to or less than c3 and equal to or less than 0.3; c1+ c2+ c3 ≦ c1+ c3 ≦ c2, comprising the steps of:
1) adding a solvent into a first stirring kettle, adding a binder, and stirring; adding the third graphite material into a first stirring kettle according to the mass ratio, stirring, then adding the first graphite material into the first stirring kettle according to the mass ratio, and stirring to obtain first slurry;
2) adding the solvent into a second stirring kettle, adding the binder, and stirring; adding the second graphite material and the conductive agent into a second stirring kettle according to the mass ratio, and stirring to obtain second slurry;
3) and adding the first slurry into the second slurry according to the mass ratio under the condition of keeping the continuous stirring of the second stirring kettle, and stirring to obtain the graphite cathode slurry.
2. The method of claim 1, wherein the conductive agent is carbon nanotubes or carbon nanofibers.
3. The method of claim 2, wherein the carbon nanotubes or carbon nanofibers have a length of 5 to 15 microns.
4. The method of claim 1, wherein the ratio by mass in the graphite slurry of the graphite material: conductive agent: the binder is 100:4-6: 3-5.
5. The method of claim 1, wherein the solvent is water and the binder is SBR.
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| CN110323411B (en) * | 2019-07-11 | 2020-12-11 | 泰州纳新新能源科技有限公司 | Preparation method of carbon cathode slurry |
| CN110492066B (en) * | 2019-08-01 | 2022-01-11 | 深圳市比克动力电池有限公司 | Lithium ion battery negative plate capable of being charged quickly and preparation method thereof |
| CN110649249B (en) * | 2019-10-14 | 2020-12-18 | 泰州纳新新能源科技有限公司 | Silicon-carbon composite electrode slurry and preparation method of electrode thereof |
| CN110690409B (en) * | 2019-10-17 | 2020-12-11 | 泰州纳新新能源科技有限公司 | Preparation method of natural graphite-based negative electrode |
| CN110707322B (en) * | 2019-10-18 | 2020-12-11 | 泰州纳新新能源科技有限公司 | Preparation method of natural graphite slurry |
| CN111370670B (en) * | 2020-03-19 | 2021-07-02 | 江西迪比科股份有限公司 | Mixing method of negative electrode slurry |
| CN113161525A (en) * | 2021-04-20 | 2021-07-23 | 山东精工电子科技有限公司 | Preparation method of lithium ion battery cathode slurry |
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