CN114530582B - Negative electrode slurry, preparation method thereof, negative electrode plate and secondary battery - Google Patents
Negative electrode slurry, preparation method thereof, negative electrode plate and secondary battery Download PDFInfo
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Abstract
The invention belongs to the technical field of secondary batteries, and particularly relates to negative electrode slurry and a preparation method thereof, a negative electrode plate and a secondary battery, wherein the negative electrode slurry comprises the following steps: step S1, weighing a silica material, dopamine hydrochloride and tris (hydroxymethyl) aminomethane, sequentially adding the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane into a solvent, stirring and dispersing, centrifuging, washing and drying to obtain a dopamine modified silica material; s2, weighing thickener glue solution, polyacrylic acid binder and carbon nanotubes, adding part of polyacrylic acid binder into the thickener glue solution, stirring, adding the carbon nanotubes, stirring, adding dopamine modified silica material, stirring and dispersing to obtain mixed glue solution; and S3, weighing graphite and conductive carbon black, sequentially adding part of graphite, conductive carbon black and residual graphite into a stirring kettle, stirring and mixing, adding the mixed glue solution, adding the residual polyacrylic acid binder and stirring to obtain the negative electrode slurry.
Description
Technical Field
The invention belongs to the technical field of secondary batteries, and particularly relates to negative electrode slurry, a preparation method thereof, a negative electrode plate and a secondary battery.
Background
The lithium ion battery is paid attention to because of the advantages of high energy density, long cycle life, environmental friendliness, no memory effect and the like, and has wide application in the fields of 3C digital codes, automobiles and the like. Graphite is used as a cathode material, the theoretical gram capacity of the graphite is only 372mAh/g, and the graphite is free from occurrenceThe method meets the requirements of people on high-energy-density batteries, and particularly the 5G age comes. The silicon material has the highest theoretical guest capacity (-4200 mAh/g) and low discharge voltage (-0.5 Vvs Li/Li) + ) Is considered to be one of the most promising negative electrode materials to replace graphite. The silicon material itself has poor conductivity, and one major improvement is to add Carbon Nanotubes (CNT) to improve conductivity during the homogenization of graphite and silicon. However, in the preparation method of the prior art, the conductivity of the silicon oxide material by the carbon nano tube is improved only a limited way, and the conductivity and the stability are poor. This is a major obstacle to the widespread use of silicon materials in lithium batteries.
Disclosure of Invention
One of the objects of the present invention is: aiming at the defects of the prior art, the preparation method of the anode slurry is provided, and the conductivity and the stability of the silicon material can be solved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing a negative electrode slurry, comprising the steps of:
step S1, weighing a silica material, dopamine hydrochloride and tris (hydroxymethyl) aminomethane, sequentially adding the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane into a solvent, stirring and dispersing, centrifuging, washing and drying to obtain a dopamine modified silica material;
s2, weighing thickener glue solution, polyacrylic acid binder and carbon nanotubes, adding part of polyacrylic acid binder into the thickener glue solution, stirring, adding the carbon nanotubes, stirring, adding dopamine modified silica material, stirring and dispersing to obtain mixed glue solution;
and S3, weighing graphite and conductive carbon black, sequentially adding part of graphite, conductive carbon black and residual graphite into a stirring kettle, stirring and mixing, adding the mixed glue solution, adding the residual polyacrylic acid binder and stirring to obtain the negative electrode slurry.
In the existing preparation method, when the carbon nano tube, graphite and a silicon oxygen material are used for homogenization, the dispersion of the Carbon Nano Tube (CNT) around silicon oxygen is reduced due to the adsorption effect between the Carbon Nano Tube (CNT) and the graphite; meanwhile, high-speed stirring and shearing during the homogenization process may cause the Carbon Nanotubes (CNTs) to fall off. All of the above cases reduce the effect of Carbon Nanotubes (CNTs) on improving the conductivity of the silicon oxygen material itself. According to the preparation method of the negative electrode slurry, the dopamine hydrochloride is used for modifying the silica material to prepare the dopamine modified silica material, and amino functional groups are arranged on the surface of the dopamine modified silica material, so that the interaction with the binder and the conductive agent can be enhanced, and the conductivity and the stability of the negative electrode slurry are improved; firstly, mixing the dopamine modified silica material with thickener glue solution, polyacrylic acid binder and carbon nanotubes to enable the carbon nanotubes to be fully dispersed on the surface of the dopamine modified silica material, thereby greatly improving the conductivity of the silica material; and finally, sequentially adding part of graphite, conductive carbon black and the residual graphite into the mixed glue solution for stirring, so that the conductive carbon black is dispersed among the graphite, and the slurry is uniformly dispersed. The tris can be deprotonated, making the silicone material susceptible to modification by dopamine hydrochloride.
Preferably, in the step S1, the weight portion ratio of the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 4-20: 0.1 to 2:0.1 to 1. The modified silicon oxide material has conductivity and stability by setting a certain proportion.
Preferably, in the step S1, the stirring and dispersing time is 5-30 min, the drying temperature is 70-90 ℃ and the drying time is 40-50 h. Stirring and dispersing for 5min, 8min, 12min, 18min, 24min, 28min, 29min, and 30min; the drying temperature is 70 ℃, 2 ℃, 78 ℃, 82 ℃, 85 ℃ and 90 ℃; the drying time is 40h, 41h, 42h, 43h, 44h, 45h, 46h, 47h, 48h, 50h.
Preferably, in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nanotubes and the dopamine modified silica material is 1-10:20-35:1-5:20-60. The carbon nanotubes are uniformly distributed on the surface of the dopamine modified silica material in the mixed solution after a certain proportion is set, so that the mixed solution has good conductivity and stability.
Preferably, the particle size of the silicon carbon material is 3-16 μm. The particle size of the silicon carbon material was 3 μm, 4 μm, 4.5 μm, 5.5 μm, 6 μm, 6.5 μm, 7 μm, 7.5 μm, 8 μm, 9 μm, 10 μm, 10.5 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm.
Preferably, the step S3 further comprises adjusting the solid content, secondary stirring and vacuum defoaming after adding the remaining polyacrylic binder.
Preferably, the solid content is 40% -60%, and the secondary stirring time is 60-180 min. Solids content 40%, 42%, 46%, 50%, 53%, 58%, 60%;
the second object of the present invention is: aiming at the defects of the prior art, the negative electrode slurry is provided, and has good conductivity and good cycle performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the negative electrode slurry is prepared by the preparation method of the negative electrode slurry.
The third object of the present invention is to: aiming at the defects of the prior art, the negative plate has good conductivity and better cycle performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the negative electrode plate comprises a negative electrode current collector and a negative electrode coating layer coated on at least one surface of the negative electrode current collector, wherein the negative electrode coating layer comprises the negative electrode slurry.
The fourth object of the invention is that: aiming at the defects of the prior art, the secondary battery has good electrochemical performance and good cycle performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a secondary battery comprises the negative plate.
Compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the negative electrode slurry, the dopamine hydrochloride is used for modifying the silica material to prepare the dopamine modified silica material, and amino functional groups are arranged on the surface of the dopamine modified silica material, so that the interaction with the binder and the conductive agent can be enhanced, and the conductivity and the stability of the negative electrode slurry are improved; firstly, mixing the dopamine modified silica material with thickener glue solution, polyacrylic acid binder and carbon nanotubes to enable the carbon nanotubes to be fully dispersed on the surface of the dopamine modified silica material, thereby greatly improving the conductivity of the silica material; and finally, sequentially adding part of graphite, conductive carbon black and the residual graphite into the mixed glue solution for stirring, so that the conductive carbon black is dispersed among the graphite, and the slurry is uniformly dispersed.
Detailed Description
The present invention will be described in further detail with reference to the following specific embodiments, but the embodiments of the present invention are not limited thereto.
Example 1
A method for preparing a negative electrode slurry, comprising the steps of:
step S1, weighing a silica material, dopamine hydrochloride and tris (hydroxymethyl) aminomethane, sequentially adding the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane into a solvent, stirring and dispersing, centrifuging, washing and drying to obtain a dopamine modified silica material;
s2, weighing thickener glue solution, polyacrylic acid binder and carbon nanotubes, adding part of polyacrylic acid binder into the thickener glue solution, stirring, adding the carbon nanotubes, stirring, adding dopamine modified silica material, stirring and dispersing to obtain mixed glue solution;
and S3, weighing graphite and conductive carbon black, sequentially adding part of graphite, conductive carbon black and residual graphite into a stirring kettle, stirring and mixing, adding the mixed glue solution, adding the residual polyacrylic acid binder and stirring to obtain the negative electrode slurry.
Wherein, in the step S1, the weight part ratio of the silicon oxygen material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 18:0.4:0.25.
wherein, in the step S1, the stirring and dispersing time is 20min, the drying temperature is 80 ℃ and the drying time is 45h.
In the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nanotubes and the dopamine modified silica material is 6:25:3.5:30.
Wherein the particle size of the silicon carbon material is 10 mu m.
Example 2
The difference from example 1 is that: in the step S1, the weight part ratio of the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 20:0.4:0.25.
the remainder is the same as in example 1 and will not be described again here.
Example 3
The difference from example 1 is that: in the step S1, the weight part ratio of the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 18:1.5:0.8.
the remainder is the same as in example 1 and will not be described again here.
Example 4
The difference from example 1 is that: in the step S1, the weight part ratio of the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 18:0.1:0.1.
the remainder is the same as in example 1 and will not be described again here.
Example 5
The difference from example 1 is that: in the step S1, the weight part ratio of the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 12:0.6:0.4.
the remainder is the same as in example 1 and will not be described again here.
Example 6
The difference from example 1 is that: in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nano tube and the dopamine modified silica material is 6:25:3.5:60.
The remainder is the same as in example 1 and will not be described again here.
Example 7
The difference from example 1 is that: in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nano tube and the dopamine modified silica material is 6:25:3.5:20.
The remainder is the same as in example 1 and will not be described again here.
Example 8
The difference from example 1 is that: in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nano tube and the dopamine modified silica material is 6:25:5:30.
The remainder is the same as in example 1 and will not be described again here.
Example 9
The difference from example 1 is that: in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nano tube and the dopamine modified silica material is 6:25:1:30.
The remainder is the same as in example 1 and will not be described again here.
Example 10
The difference from example 1 is that: in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nano tube and the dopamine modified silica material is 8:30:4:45.
The remainder is the same as in example 1 and will not be described again here.
Comparative example 1
The difference from example 1 is that: the preparation method of the cathode slurry comprises the following steps: s1, weighing thickener glue solution, polyacrylic acid binder, carbon nano tubes and silicon oxide materials, adding part of polyacrylic acid binder into the thickener glue solution, stirring, adding the carbon nano tubes, stirring, adding the silicon oxide materials, stirring and dispersing to obtain mixed glue solution;
and S2, weighing graphite and conductive carbon black, sequentially adding part of graphite, conductive carbon black and residual graphite into a stirring kettle, stirring and mixing, adding the mixed glue solution, adding the residual polyacrylic acid binder and stirring to obtain the negative electrode slurry.
The remainder is the same as in example 1 and will not be described again here.
Comparative example 2
The difference from example 1 is that: the preparation method of the cathode slurry comprises the following steps: step S1, weighing a silica material, dopamine hydrochloride and tris (hydroxymethyl) aminomethane, sequentially adding the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane into a solvent, stirring and dispersing, centrifuging, washing and drying to obtain a dopamine modified silica material;
s2, weighing thickener glue solution, polyacrylic acid binder and carbon nanotubes, adding part of polyacrylic acid binder into the thickener glue solution, stirring, adding the carbon nanotubes, stirring, adding part of dopamine modified silica material, stirring and dispersing to obtain mixed glue solution;
and S3, weighing graphite and conductive carbon black, sequentially adding part of graphite, conductive carbon black, residual dopamine modified silica material and residual graphite into a stirring kettle, stirring and mixing, adding the mixed glue solution, adding residual polyacrylic acid binder and stirring to obtain the negative electrode slurry.
The remainder is the same as in example 1 and will not be described again here.
The negative electrode pastes prepared in examples 1 to 10 and comparative examples 1 and 2 were used to prepare a negative electrode sheet and a secondary battery using a lithium ion battery as an example and LiCoO as a positive electrode 2 As an active substance, a JL 7 μm oil-based diaphragm is adopted as the diaphragm; obtaining a bare cell by adopting a full-automatic winding mode; and (3) jacking the bare cell by using an aluminum plastic film outer package with a certain size, injecting a certain amount of electrolyte into the dried semi-packaged cell, and completing packaging. And (5) continuing to perform the working procedures of standing, formation, shaping, capacity division and the like to finish the preparation of the lithium ion soft package battery.
Performance test: the performance of the lithium ion battery prepared above was tested, and the test results were recorded in table 1.
TABLE 1
As can be seen from the above table 1, the negative electrode sheet and the secondary battery prepared by the preparation method of the negative electrode slurry of the present invention have better cycle capacity retention and rate charge capacity retention than the prior art. As shown by comparison of the example 1 and the comparative example 1, the silicon-oxygen material is modified by using dopamine hydrochloride, so that the surface of the silicon-oxygen material is rich in amino functional groups, the silicon-oxygen material can be firmly combined with a binder and a conductive agent, and the interaction is stronger, the stability is better, and the cycle capacity retention rate and the rate charge capacity retention rate are higher. As is evident from the comparison of example 1 and comparative example 2, the prepared negative electrode slurry has better performance when the dopamine-modified silicone material is added to the carbon nanotubes in one step. The method is characterized in that the dopamine-modified silica material is fully contacted with the carbon nano tube, so that the carbon nano tube is uniformly adsorbed on the surface of the dopamine-modified silica material instead of the graphite surface, thereby improving the conductivity of the silica material, reducing the electrical deactivation in the circulation process and reducing the fading problem in the circulation process. As shown by comparison of examples 1-5, when the weight part ratio of the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane in the step S1 is set to be 18:0.4: when the content of the dopamine hydrochloride is 0.25, the prepared secondary battery has better performance, because the modified silica material has more groups on the surface, the interaction and stability are effectively improved, but when the content of the dopamine hydrochloride is excessive, the modified silica material is easily unstable, so that the performance is influenced. As shown by comparison of examples 1 and 6-10, when the weight ratio of the thickener gum solution, the polyacrylic acid binder, the carbon nanotubes and the dopamine-modified silica material in the step S2 is set to be 6:25:3.5:30, the prepared secondary battery has better performance, because the suitable carbon nanotubes can effectively improve the conductivity of the dopamine-modified silica material without causing the problem of poor stability of the negative electrode slurry.
Variations and modifications of the above embodiments will occur to those skilled in the art to which the invention pertains from the foregoing disclosure and teachings. Therefore, the present invention is not limited to the above-described embodiments, but is intended to be capable of modification, substitution or variation in light thereof, which will be apparent to those skilled in the art in light of the present teachings. In addition, although specific terms are used in the present specification, these terms are for convenience of description only and do not limit the present invention in any way.
Claims (7)
1. A method for preparing a negative electrode slurry, comprising the steps of:
step S1, weighing a silica material, dopamine hydrochloride and tris (hydroxymethyl) aminomethane, sequentially adding the silica material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane into a solvent, stirring and dispersing, centrifuging, washing and drying to obtain a dopamine modified silica material;
s2, weighing thickener glue solution, polyacrylic acid binder and carbon nanotubes, adding part of polyacrylic acid binder into the thickener glue solution, stirring, adding the carbon nanotubes, stirring, adding dopamine modified silica material, stirring and dispersing to obtain mixed glue solution;
step S3, weighing graphite and conductive carbon black, sequentially adding part of graphite, conductive carbon black and residual graphite into a stirring kettle, stirring and mixing, adding mixed glue solution, adding residual polyacrylic acid binder and stirring to obtain negative electrode slurry;
wherein, in the step S1, the weight part ratio of the silicon oxygen material, the dopamine hydrochloride and the tris (hydroxymethyl) aminomethane is 4-20: 0.1 to 2:0.1 to 1;
wherein, in the step S1, the stirring and dispersing time is 5-30 min, the drying temperature is 70-90 ℃ and the drying time is 40-50 h;
wherein, in the step S2, the weight part ratio of the thickener glue solution, the polyacrylic acid binder, the carbon nano tube and the dopamine modified silica material is 1-10:20-35:1-5:20-60.
2. The method for producing a negative electrode slurry according to claim 1, wherein the particle size of the silicon oxide material is 3 to 16 μm.
3. The method for preparing a negative electrode slurry according to claim 1, wherein the step S3 further comprises adjusting the solid content, secondary stirring, and vacuum defoaming after adding the remaining polyacrylic binder.
4. The method for producing a negative electrode slurry according to claim 3, wherein the solid content is 40 to 60%, and the time for secondary stirring is 60 to 180 minutes.
5. A negative electrode slurry, characterized by being produced by the method for producing a negative electrode slurry according to any one of claims 1 to 4.
6. A negative electrode sheet comprising a negative electrode current collector and a negative electrode coating layer coated on at least one surface of the negative electrode current collector, the negative electrode coating layer comprising the negative electrode slurry of claim 5.
7. A secondary battery comprising the negative electrode sheet according to claim 6.
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