CN111430673A - Preparation method of negative electrode - Google Patents
Preparation method of negative electrode Download PDFInfo
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- CN111430673A CN111430673A CN202010274207.3A CN202010274207A CN111430673A CN 111430673 A CN111430673 A CN 111430673A CN 202010274207 A CN202010274207 A CN 202010274207A CN 111430673 A CN111430673 A CN 111430673A
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention provides a preparation method of a negative electrode, wherein an active substance of the negative electrode comprises carbon-silicon composite particles and graphite particles, the carbon-silicon composite particles are carbon-coated silicon particles, and the carbon content in the carbon-silicon composite particles is 10-12%; the average particle size of the carbon-silicon composite particles is 150-200nm, and the average particle size of the graphite particles is 2.5-2.7 mu m. The preparation method comprises the steps of screening graphite particles, mixing the materials according to different particle size ranges, mixing and pulping part of the graphite particles with different particle sizes to obtain first slurry, mixing and pulping part of the graphite particles and carbon-silicon composite particles to obtain second slurry, sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode. The cathode slurry is high in stability, and the obtained cathode is stable in structure and good in cyclicity.
Description
Technical Field
The invention relates to a preparation method of a negative electrode, in particular to a preparation method of a carbon-silicon composite material and graphite mixed negative electrode.
Background
With the updating of energy technology, meeting the increasing energy demand in various fields such as electronics, renewable energy systems, electric vehicles and the like is more and more urgent. Lithium ion batteries are considered to be a new type of power source that meets the increasing energy demands of portable electronic devices, electric and hybrid vehicles due to their higher capacity and stable cycle life. In different cathode materials, the theoretical specific capacity of silicon is 10 times of that of the traditional carbon cathode, which attracts great attention, and the lithium ion battery can obtain higher power due to the lower de-intercalation lithium potential of silicon. However, silicon anode materials are not attractive for use in lithium batteries because of their low conductivity and severe volume expansion, cracking and pulverization of the silicon particles, resulting in slow kinetics and short cycle life due to loss of active material and poor electrical contact. Graphite and porous carbon have relatively small volume changes during lithiation. And has good cycle stability and conductivity, thus becoming a potential cathode material. Carbon materials have similar properties to silicon materials and they can be tightly bound, so carbon materials are naturally selected as substrate materials for dispersing silicon particles. Through silicon-carbon compounding, the lithium ion battery can obtain higher specific capacity, better conductivity and cycling stability.
Disclosure of Invention
The invention provides a preparation method of a negative electrode, wherein an active substance of the negative electrode comprises carbon-silicon composite particles and graphite particles, the carbon-silicon composite particles are carbon-coated silicon particles, and the carbon content in the carbon-silicon composite particles is 10-12%; the average particle size of the carbon-silicon composite particles is 150-200nm, and the average particle size of the graphite particles is 2.5-2.7 mu m. The preparation method comprises the steps of screening graphite particles, mixing the materials according to different particle size ranges, mixing and pulping part of the graphite particles with different particle sizes to obtain first slurry, mixing and pulping part of the graphite particles and carbon-silicon composite particles to obtain second slurry, sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode. The cathode slurry is high in stability, and the obtained cathode is stable in structure and good in cyclicity.
The specific scheme is as follows:
a preparation method of a negative electrode comprises the following steps that active materials of the negative electrode comprise carbon-silicon composite particles and graphite particles, the carbon-silicon composite particles are carbon-coated silicon particles, and the carbon content in the carbon-silicon composite particles is 10-12%; the average particle size of the carbon-silicon composite particles is 150-200nm, the average particle size of the graphite particles is 2.5-2.7 mu m, and the preparation method comprises the following steps:
1) sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4-4.2 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.5-2.7 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1-1.2 mu m; collecting material above the third screen, and material below the third screen;
4) adding a binder into a solvent of a stirring kettle, uniformly stirring, then adding a conductive agent, uniformly stirring, adding a material on a third screen, uniformly stirring, and then adding a material on a second screen to obtain first slurry, wherein the mass ratio of the materials to the active substances is as follows: adhesive: the conductive agent is 100:3-6: 3-5;
5) adding a binder into a solvent of a stirring kettle, uniformly stirring, then adding a conductive agent, uniformly stirring, adding a material below a third screen, uniformly stirring, and then adding carbon-silicon composite particles to obtain a second slurry, wherein the mass ratio of the active substances is as follows: adhesive: the conductive agent is 100:3-6: 3-5;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode.
Further wherein the mass ratio in the first slurry, material on the second screen/material on the third screen satisfies the relationship k ═ k (second screen aperture/third screen aperture), k ═ 1.15 to 1.18.
Further, the mass ratio of the second slurry to the material/carbon-silicon composite particles under the third screen is 0.14-0.16.
Further, the solvent is deionized water.
Further, the binder is an aqueous binder, preferably SBR.
Further, the conductive agent is selected from conductive carbon black, conductive metal particles, conductive ceramic particles, conductive high molecular polymers and the like.
Further, the composite cathode slurry is prepared by the method, wherein the coating thickness of the first slurry is 10-15 μm, and the coating thickness of the second slurry is 45-50 μm.
The invention has the following beneficial effects:
1) researchers find that when the graphite material in the first slurry meets the specific proportion in the invention, namely, the material on the second screen/the material on the third screen is k (the aperture of the second screen/the aperture of the third screen), the slurry with high dispersibility and good stability can be obtained, and the structural strength of the graphite layer can be improved, and the cycle life can be prolonged.
2) The surface layer is compounded by adopting a silicon-carbon composite material and a part of graphite material, the stability of the slurry can be improved by limiting the particle size distribution of graphite and the mass ratio of the graphite to the silicon-carbon composite material, and meanwhile, the stability of the electrolyte on the surface layer is higher, so that the improvement of the cycle performance of the electrode is facilitated.
3) The carbon-silicon composite material and the graphite material are used for obtaining the composite electrode, so that the electrode with higher energy density, rate capability and cycle life can be obtained, and the cost is lower.
4) The graphite material has better rate performance and lower cost, and the silicon-carbon composite material has larger energy density and electrolyte stability, thereby being beneficial to prolonging the cycle life.
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. The carbon-silicon composite material used in the invention is 10% of carbon-coated silicon particles, the average particle size of the carbon-silicon composite particles is 180nm, and the average particle size of the graphite particles is 2.6 μm.
Example 1
1) Sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.5 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1 mu m; collecting material above the third screen, and material below the third screen;
4) adding SBR to the deionized water of stirred tank, the stirring, then adding acetylene black, the stirring, add the material on the third screen cloth, the stirring, add the material on the second screen cloth again, obtain first thick liquids, wherein the mass ratio, material on the second screen cloth/material on the third screen cloth 2.9, active material: SBR: acetylene black 100:3: 3;
5) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material below a third screen, uniformly stirring, adding carbon-silicon composite particles, and obtaining a second slurry, wherein the mass ratio of the material/the carbon-silicon composite particles below the third screen is 0.14, and active substances: SBR: acetylene black 100:3: 3;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode, wherein the coating thickness of the first slurry is 10 micrometers, and the coating thickness of the second slurry is 50 micrometers.
Example 2
1) Sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4.1 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.6 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1.1 mu m; collecting material above the third screen, and material below the third screen;
4) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material on a third screen, uniformly stirring, then adding a material on a second screen, and obtaining a first slurry, wherein the mass ratio of the material on the second screen to the material on the third screen is 2.75, and the active substances are as follows: SBR: acetylene black 100:4: 4;
5) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material below a third screen, uniformly stirring, adding carbon-silicon composite particles, and obtaining a second slurry, wherein the mass ratio of the material/carbon-silicon composite particles below the third screen is 0.15, and active substances: SBR: acetylene black 100:4: 4;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode, wherein the coating thickness of the first slurry is 15 micrometers, and the coating thickness of the second slurry is 45 micrometers.
Example 3
1) Sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4.2 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.7 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1.2 mu m; collecting material above the third screen, and material below the third screen;
4) adding SBR to the deionized water of stirred tank, the stirring, then adding acetylene black, the stirring, add the material on the third screen cloth, the stirring, add the material on the second screen cloth again, obtain first thick liquids, wherein the mass ratio, material on the second screen cloth/material on the third screen cloth 2.6, active material: SBR: acetylene black 100:6: 5;
5) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material below a third screen, uniformly stirring, adding carbon-silicon composite particles, and obtaining a second slurry, wherein the mass ratio of the material/the carbon-silicon composite particles below the third screen is 0.16, and active substances: SBR: acetylene black 100:6: 5;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode, wherein the coating thickness of the first slurry is 12 micrometers, and the coating thickness of the second slurry is 48 micrometers.
Comparative example 1
1) Sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4.2 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.7 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1.2 mu m; collecting material above the third screen, and material below the third screen;
4) adding SBR to the deionized water of stirred tank, the stirring, then adding acetylene black, the stirring, the material on the third screen cloth of adding, the stirring, add the material on the second screen cloth again, obtain first thick liquids, wherein the mass ratio, material on the second screen cloth/the material on the third screen cloth is 3, active material: SBR: acetylene black 100:6: 5;
5) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material below a third screen, uniformly stirring, adding carbon-silicon composite particles, and obtaining a second slurry, wherein the mass ratio of the material/carbon-silicon composite particles below the third screen is 0.3, and active substances: SBR: acetylene black 100:6: 5;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode, wherein the coating thickness of the first slurry is 12 micrometers, and the coating thickness of the second slurry is 48 micrometers.
Comparative example 2
1) Sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4.2 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.7 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1.2 mu m; collecting material above the third screen, and material below the third screen;
4) adding SBR to the deionized water of stirred tank, the stirring, then adding acetylene black, the stirring, the material on the third screen cloth of adding, the stirring, add the material on the second screen cloth again, obtain first thick liquids, wherein the mass ratio, material on the second screen cloth/the material on the third screen cloth 2, active material: SBR: acetylene black 100:6: 5;
5) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material below a third screen, uniformly stirring, adding carbon-silicon composite particles, and obtaining a second slurry, wherein the mass ratio of the material/carbon-silicon composite particles below the third screen is 0.1, and active substances: SBR: acetylene black 100:6: 5;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode, wherein the coating thickness of the first slurry is 12 micrometers, and the coating thickness of the second slurry is 48 micrometers.
Comparative example 3
1) Sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4.2 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.7 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1.2 mu m; collecting material above the third screen, and material below the third screen;
4) adding SBR to the deionized water of stirred tank, the stirring, then adding acetylene black, the stirring, add the material on the third screen cloth, the stirring, add the material on the second screen cloth again, obtain first thick liquids, wherein the mass ratio, material on the second screen cloth/material on the third screen cloth 2.6, active material: SBR: acetylene black 100:6: 5;
6) and coating the first slurry on a negative electrode current collector, and drying to obtain the negative electrode, wherein the coating thickness of the slurry is 60 microns.
Comparative example 4
1) Sieving graphite particles by using a third screen, wherein the aperture of the third screen is 1.2 mu m; collecting material under the third screen;
2) adding SBR into the deionized water of a stirring kettle, uniformly stirring, then adding acetylene black, uniformly stirring, adding a material below a third screen, uniformly stirring, adding carbon-silicon composite particles, and obtaining a second slurry, wherein the mass ratio of the material/the carbon-silicon composite particles below the third screen is 0.16, and active substances: SBR: acetylene black 100:6: 5;
3) and sequentially coating the second slurry on a negative current collector, and drying to obtain the negative electrode, wherein the coating thickness of the second slurry is 60 micrometers.
Test and results
The solids contents of the first and second slurries of examples 1 to 3 and comparative examples 1 to 2 were adjusted to 50%, and then left to stand for 6 hours, and the solids content 5cm below the surface layer was measured to measure the stability of the slurries, and the results are shown in table 1.
The negative electrodes of examples 1 to 3 and comparative examples 1 to 4 were combined with lithium sheets to constitute test cells, and charge and discharge cycles were performed 300 times at currents of 0.5C and 2C to measure the capacity retention rate of the negative electrode, and the results are shown in table 2.
TABLE 1
TABLE 2
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 (7)
1. A preparation method of a negative electrode comprises the following steps that active materials of the negative electrode comprise carbon-silicon composite particles and graphite particles, the carbon-silicon composite particles are carbon-coated silicon particles, and the carbon content in the carbon-silicon composite particles is 10-12%; the average particle size of the carbon-silicon composite particles is 150-200nm, the average particle size of the graphite particles is 2.5-2.7 mu m, and the preparation method comprises the following steps:
1) sieving graphite particles by using a first screen, wherein the aperture of the first screen is 4-4.2 mu m, and collecting materials below the first screen;
2) sieving the material collected in the step 1 by using a second sieve, wherein the pore diameter of the second sieve is 2.5-2.7 mu m; collecting material above the second screen, and material below the second screen;
3) sieving the material collected in the step 2 under the two screens by using a third screen, wherein the aperture of the third screen is 1-1.2 mu m; collecting material above the third screen, and material below the third screen;
4) adding a binder into a solvent of a stirring kettle, uniformly stirring, then adding a conductive agent, uniformly stirring, adding a material on a third screen, uniformly stirring, and then adding a material on a second screen to obtain first slurry, wherein the mass ratio of the materials to the active substances is as follows: adhesive: the conductive agent is 100:3-6: 3-5;
5) adding a binder into a solvent of a stirring kettle, uniformly stirring, then adding a conductive agent, uniformly stirring, adding a material below a third screen, uniformly stirring, and then adding carbon-silicon composite particles to obtain a second slurry, wherein the mass ratio of the active substances is as follows: adhesive: the conductive agent is 100:3-6: 3-5;
6) and sequentially coating the first slurry and the second slurry on a negative current collector, and drying to obtain the negative electrode.
2. The method of claim, wherein the mass ratio of the first slurry to the second screen/the third screen satisfies the relationship k ═ k (second screen aperture/third screen aperture) and k ═ 1.15 to 1.18.
3. The production method according to the above claim, wherein the mass ratio of the material under the third screen/the carbon silicon composite particles in the second slurry is 0.14 to 0.16.
4. The method of claim, wherein the solvent is deionized water.
5. The method of the above claim, wherein the binder is an aqueous binder, preferably SBR.
6. The production method according to the above claim, wherein the conductive agent is selected from conductive carbon black, conductive metal particles, conductive ceramic particles, conductive high molecular polymers and the like.
7. A composite positive electrode slurry prepared by the method according to any one of claims 1 to 6, wherein the first slurry is coated to a thickness of 10 to 15 μm and the second slurry is coated to a thickness of 45 to 50 μm.
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| WO2022057668A1 (en) * | 2020-09-21 | 2022-03-24 | 珠海冠宇电池股份有限公司 | Negative electrode plate, preparation method therefor, and battery |
| CN114709367A (en) * | 2022-04-07 | 2022-07-05 | 珠海冠宇电池股份有限公司 | Negative plate, lithium ion battery and preparation method of negative plate |
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