CN111063875A - Spongy porous structure silicon-based composite material and preparation method thereof - Google Patents
Spongy porous structure silicon-based composite material and preparation method thereof Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H01M4/00—Electrodes
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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Abstract
The invention discloses a spongy porous silicon-based composite material and a preparation method thereof, wherein the spongy porous silicon-based composite material comprises the following raw materials in parts by mass: 10-20 parts of nano silicon, 20-40 parts of expanded graphite, 20-40 parts of metal Li, 10-20 parts of sodium alginate, 2-8 parts of a dispersing agent and 2-8 parts of an organic solvent. The invention has the advantages of high first efficiency, low expansion, long cycle and the like, the spongy carbon conductive network can effectively improve the conductivity of the silicon-based material, and the sponge structure can effectively relieve the volume effect in the charging and discharging process, effectively avoid the pulverization of the material in the cycle process, relieve the volume expansion effect of the silicon-based material, improve the cycle performance and improve the conductivity and the rate capability of the material.
Description
Technical Field
The invention relates to the technical field of new energy lithium ion battery cathode materials, in particular to a spongy porous structure silicon-based composite material and a preparation method thereof.
Background
At present, commercial negative electrode materials are mainly natural graphite, artificial graphite and middle equal graphite materials, but the theoretical capacity of the materials is low (372mAh/g), so that the requirements of the market cannot be met. In recent years, people aim at novel high specific capacity negative electrode materials: lithium storage metals and their oxides (e.g., Sn, Si) and lithium transition metal phosphides. Among a plurality of novel high-specific-capacity negative electrode materials, Si becomes one of the most potential replaceable graphite materials due to high theoretical specific capacity (4200mAh/g), but silicon-based materials have huge volume effect in the charging and discharging process and are easy to break and pulverize, so that the contact with a current collector is lost, and the cycle performance is sharply reduced; in addition, the silicon-based material has low intrinsic conductivity and poor rate capability. Therefore, the volume expansion effect is reduced, and the cycle performance and the rate capability are improved, so that the method has great significance for the application of the silicon-based material in the lithium ion battery.
CN 103367727 a discloses a silicon-carbon negative electrode material for lithium ion batteries. Mixing nano-silicon, a dispersing agent, a binder and granular graphite in a solvent, drying to obtain nano-silicon embedded between gaps of the granular graphite or polymer attached to the surface of the granular graphite, adding the obtained polymer into dispersion liquid of a carbon source precursor, mixing, and drying to obtain the silicon-carbon composite material. The carbon carrier used in the method is granular graphite, so that the conductive network between nano silicon is poor, and the multiplying power performance is not ideal. In addition, the silicon-carbon composite material prepared by the method has local silicon aggregation, so that the cycle performance of the material is poor.
CN 103682287A discloses a silicon-based composite negative electrode material of a lithium ion battery, a preparation method and the battery. The method comprises the steps of mixing nano-silicon, a dispersing agent and a hollow graphite solvent, drying to obtain a precursor, and then combining the precursor with mechanical fusion, isotropic pressurization, carbon coating and mechanical grinding to obtain the silicon-based composite anode material which embeds nano-silicon particles into a graphite inner layer and realizes uniform coating of the surfaces of the graphite particles. The carrier used in the method is hollow graphite, so that a large amount of nano silicon is bound to aggregate, and the cycle performance of the material is not ideal.
Disclosure of Invention
The invention aims to provide a spongy porous silicon-based composite material and a preparation method thereof, the spongy porous silicon-based composite material has the advantages of high first efficiency, low expansion, long cycle and the like, the spongy carbon conductive network can effectively improve the conductivity of the silicon-based material, and the spongy structure can effectively relieve the volume effect in the charge-discharge process, effectively avoid the pulverization of the material in the cycle process, relieve the volume expansion effect of the silicon-based material, improve the cycle performance, and improve the conductivity and the rate capability of the material so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a spongy porous structure silicon-based composite material comprises the following raw materials in parts by weight:
10-20 parts of nano silicon, 20-40 parts of expanded graphite, 20-40 parts of metal Li, 10-20 parts of sodium alginate, 2-8 parts of a dispersing agent and 2-8 parts of an organic solvent.
Further, the material comprises the following raw materials in parts by mass:
10 parts of nano silicon, 40 parts of expanded graphite, 30 parts of metal Li, 10 parts of sodium alginate, 2 parts of a dispersing agent and 8 parts of an organic solvent.
Further, the material comprises the following raw materials in parts by mass:
15 parts of nano silicon, 30 parts of expanded graphite, 30 parts of metal Li, 15 parts of sodium alginate, 5 parts of a dispersing agent and 5 parts of an organic solvent.
Further, the material comprises the following raw materials in parts by mass:
20 parts of nano silicon, 20 parts of expanded graphite, 40 parts of metal Li, 10 parts of sodium alginate, 8 parts of a dispersing agent and 2 parts of an organic solvent.
Further, the material comprises the following raw materials in parts by mass:
20 parts of nano silicon, 28 parts of expanded graphite, 20 parts of metal Li, 20 parts of sodium alginate, 6 parts of a dispersing agent and 6 parts of an organic solvent.
Further, the dispersant is glyceryl tristearate.
Further, the organic solvent is absolute ethyl alcohol.
The other technical scheme to be solved by the invention is as follows: a preparation method of a silicon-based composite material with a spongy porous structure comprises the following steps:
s101: uniformly mixing and dispersing nano-silicon, a dispersing agent and expanded graphite in an organic solvent to obtain a precursor A;
s102: carrying out suction filtration on the precursor A, and enabling nano-silicon to enter gaps of the expanded graphite at a high speed by utilizing negative pressure to obtain a precursor B;
s103: drying the precursor B to obtain a precursor C;
s104: mechanically mixing the precursor C and a carbon source, namely mechanically fusing to obtain a precursor D;
s105: and (4) carrying out high-temperature calcination and screening treatment on the precursor D to obtain the spongy porous silicon-based composite material.
Compared with the prior art, the invention has the beneficial effects that: the invention has the advantages of high first efficiency, low expansion, long cycle and the like, the spongy carbon conductive network can effectively improve the conductivity of the silicon-based material, and the sponge structure can effectively relieve the volume effect in the charging and discharging process, effectively avoid the pulverization of the material in the cycle process, relieve the volume expansion effect of the silicon-based material, improve the cycle performance and improve the conductivity and the rate capability of the material.
Drawings
FIG. 1 is a flow chart of a preparation method of a silicon-based composite material with a spongy porous structure according to the invention;
FIG. 2 is a graph of the cycle performance of the present invention;
FIG. 3 is a second graph of the cycle performance of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A spongy porous structure silicon-based composite material comprises the following raw materials in parts by weight:
10 parts of nano silicon, 40 parts of expanded graphite, 30 parts of metal Li, 10 parts of sodium alginate, 2 parts of glyceryl tristearate and 8 parts of absolute ethyl alcohol.
Based on the above silicon-based composite material with a spongy porous structure, the present embodiment provides a preparation method of a silicon-based composite material with a spongy porous structure, the flow of which is shown in fig. 1, and the method includes the following steps:
step 1: uniformly mixing and dispersing 10 parts of nano silicon, 2 parts of glyceryl tristearate and 40 parts of expanded graphite in 8 parts of absolute ethyl alcohol to obtain a precursor A;
step 2: carrying out suction filtration on the precursor A, and enabling nano-silicon to enter gaps of the expanded graphite at a high speed by utilizing negative pressure to obtain a precursor B;
and step 3: drying the precursor B to obtain a precursor C;
and 4, step 4: mechanically mixing the precursor C and a carbon source, namely mechanically fusing to obtain a precursor D;
and 5: and (4) carrying out high-temperature calcination and screening treatment on the precursor D to obtain the spongy porous silicon-based composite material.
Example 2
A spongy porous structure silicon-based composite material comprises the following raw materials in parts by weight:
15 parts of nano silicon, 30 parts of expanded graphite, 30 parts of metal Li, 15 parts of sodium alginate, 5 parts of a dispersing agent and 5 parts of an organic solvent.
Based on the above silicon-based composite material with a spongy porous structure, the embodiment provides a preparation method of a silicon-based composite material with a spongy porous structure, which includes the following steps:
step 1: uniformly mixing and dispersing 15 parts of nano silicon, 5 parts of glyceryl tristearate and 30 parts of expanded graphite in 5 parts of absolute ethyl alcohol to obtain a precursor A;
step 2: carrying out suction filtration on the precursor A, and enabling nano-silicon to enter gaps of the expanded graphite at a high speed by utilizing negative pressure to obtain a precursor B;
and step 3: drying the precursor B to obtain a precursor C;
and 4, step 4: mechanically mixing the precursor C and a carbon source, namely mechanically fusing to obtain a precursor D;
and 5: and (4) carrying out high-temperature calcination and screening treatment on the precursor D to obtain the spongy porous silicon-based composite material.
Example 3
A spongy porous structure silicon-based composite material comprises the following raw materials in parts by weight:
20 parts of nano silicon, 20 parts of expanded graphite, 40 parts of metal Li, 10 parts of sodium alginate, 8 parts of a dispersing agent and 2 parts of an organic solvent.
Based on the above silicon-based composite material with a spongy porous structure, the embodiment provides a preparation method of a silicon-based composite material with a spongy porous structure, which includes the following steps:
step 1: uniformly mixing and dispersing 20 parts of nano silicon, 8 parts of glyceryl tristearate and 20 parts of expanded graphite in 2 parts of absolute ethyl alcohol to obtain a precursor A;
step 2: carrying out suction filtration on the precursor A, and enabling nano-silicon to enter gaps of the expanded graphite at a high speed by utilizing negative pressure to obtain a precursor B;
and step 3: drying the precursor B to obtain a precursor C;
and 4, step 4: mechanically mixing the precursor C and a carbon source, namely mechanically fusing to obtain a precursor D;
and 5: and (4) carrying out high-temperature calcination and screening treatment on the precursor D to obtain the spongy porous silicon-based composite material.
Example 4
A spongy porous structure silicon-based composite material comprises the following raw materials in parts by weight:
20 parts of nano silicon, 28 parts of expanded graphite, 20 parts of metal Li, 20 parts of sodium alginate, 6 parts of a dispersing agent and 6 parts of an organic solvent.
Based on the above silicon-based composite material with a spongy porous structure, the embodiment provides a preparation method of a silicon-based composite material with a spongy porous structure, which includes the following steps:
step 1: uniformly mixing and dispersing 20 parts of nano silicon, 6 parts of glyceryl tristearate and 28 parts of expanded graphite in 6 parts of absolute ethyl alcohol to obtain a precursor A;
step 2: carrying out suction filtration on the precursor A, and enabling nano-silicon to enter gaps of the expanded graphite at a high speed by utilizing negative pressure to obtain a precursor B;
and step 3: drying the precursor B to obtain a precursor C;
and 4, step 4: mechanically mixing the precursor C and a carbon source, namely mechanically fusing to obtain a precursor D;
and 5: and (4) carrying out high-temperature calcination and screening treatment on the precursor D to obtain the spongy porous silicon-based composite material.
When the charge and discharge tests are performed on the silicon-based composite material with the spongy porous structure in the above 5 embodiments, the reversible capacity can be kept stable with the increase of the cycle number, and the reversible capacity is maintained at 750-820mAh/g (as shown in FIG. 2 and FIG. 3).
The invention has the advantages of high first efficiency, low expansion, long cycle and the like, the spongy carbon conductive network can effectively improve the conductivity of the silicon-based material, and the sponge structure can effectively relieve the volume effect in the charging and discharging process, effectively avoid the pulverization of the material in the cycle process, relieve the volume expansion effect of the silicon-based material, improve the cycle performance and improve the conductivity and the rate capability of the material.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (8)
1. The spongy silicon-based composite material with the porous structure is characterized by comprising the following raw materials in parts by mass:
10-20 parts of nano silicon, 20-40 parts of expanded graphite, 20-40 parts of metal Li, 10-20 parts of sodium alginate, 2-8 parts of a dispersing agent and 2-8 parts of an organic solvent.
2. The silicon-based composite material with the spongy porous structure, as set forth in claim 1, is characterized by comprising the following raw materials in parts by mass:
10 parts of nano silicon, 40 parts of expanded graphite, 30 parts of metal Li, 10 parts of sodium alginate, 2 parts of a dispersing agent and 8 parts of an organic solvent.
3. The silicon-based composite material with the spongy porous structure, as set forth in claim 1, is characterized by comprising the following raw materials in parts by mass:
15 parts of nano silicon, 30 parts of expanded graphite, 30 parts of metal Li, 15 parts of sodium alginate, 5 parts of a dispersing agent and 5 parts of an organic solvent.
4. The silicon-based composite material with the spongy porous structure, as set forth in claim 1, is characterized by comprising the following raw materials in parts by mass:
20 parts of nano silicon, 20 parts of expanded graphite, 40 parts of metal Li, 10 parts of sodium alginate, 8 parts of a dispersing agent and 2 parts of an organic solvent.
5. The silicon-based composite material with the spongy porous structure, as set forth in claim 1, is characterized by comprising the following raw materials in parts by mass:
20 parts of nano silicon, 28 parts of expanded graphite, 20 parts of metal Li, 20 parts of sodium alginate, 6 parts of a dispersing agent and 6 parts of an organic solvent.
6. The silicon-based composite material with a spongy porous structure according to any one of claims 1 to 5, wherein the dispersant is glyceryl tristearate.
7. The silicon-based composite material with a spongy porous structure according to any one of claims 1 to 5, wherein the organic solvent is absolute ethanol.
8. A method for preparing a silicon-based composite material with a spongy porous structure according to claim 1, comprising the following steps:
s101: uniformly mixing and dispersing nano-silicon, a dispersing agent and expanded graphite in an organic solvent to obtain a precursor A;
s102: carrying out suction filtration on the precursor A, and enabling nano-silicon to enter gaps of the expanded graphite at a high speed by utilizing negative pressure to obtain a precursor B;
s103: drying the precursor B to obtain a precursor C;
s104: mechanically mixing the precursor C and a carbon source, namely mechanically fusing to obtain a precursor D;
s105: and (4) carrying out high-temperature calcination and screening treatment on the precursor D to obtain the spongy porous silicon-based composite material.
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Cited By (4)
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| WO2021129125A1 (en) * | 2019-12-25 | 2021-07-01 | 广东凯金新能源科技股份有限公司 | Silicon-carbon composite negative electrode material with hollow core-shell structure, and preparation method therefor |
| CN113241441A (en) * | 2020-12-07 | 2021-08-10 | 广东凯金新能源科技股份有限公司 | Pomegranate-like structure silicon-based composite material, and preparation method and application thereof |
| CN114447313A (en) * | 2022-01-28 | 2022-05-06 | 江苏集芯半导体硅材料研究院有限公司 | Preparation method and production device of silicon-based negative electrode material |
| JP2023509253A (en) * | 2020-12-07 | 2023-03-08 | 広東▲凱▼金新能源科技股▲フン▼有限公司 | Self-filling coated silicon-based composite material, its preparation method and its application |
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| JP7357699B2 (en) | 2020-12-07 | 2023-10-06 | 広東▲凱▼金新能源科技股▲フン▼有限公司 | Self-filling coated silicon-based composite material, its preparation method and its application |
| CN114447313A (en) * | 2022-01-28 | 2022-05-06 | 江苏集芯半导体硅材料研究院有限公司 | Preparation method and production device of silicon-based negative electrode material |
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Application publication date: 20200424 |