CN111584831A - Polymer-coated silicon/sulfur-doped graphene negative electrode material and preparation method thereof - Google Patents
Polymer-coated silicon/sulfur-doped graphene negative electrode material and preparation method thereof Download PDFInfo
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- CN111584831A CN111584831A CN201910118008.0A CN201910118008A CN111584831A CN 111584831 A CN111584831 A CN 111584831A CN 201910118008 A CN201910118008 A CN 201910118008A CN 111584831 A CN111584831 A CN 111584831A
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Abstract
The invention discloses a polymer-coated silicon/sulfur-doped graphene negative electrode material and a preparation method thereof, wherein the negative electrode material consists of a silicon material, sulfur-doped graphene and a polymer coating layer coated outside the silicon material, and the preparation method comprises the following steps of S1: ball-milling the silicon nanoparticles and the sulfur-doped graphene to obtain a silicon/sulfur-doped graphene composite material; s2: dispersing the composite material into deionized water, adding a pyrrole monomer and a dopamine monomer, cooling, and adding ferric chloride hexahydrate for reaction; s3: precipitating, cleaning, drying, and grinding. The core silicon nanoparticles of the material have lithium storage activity, and the silicon nanoparticles are adsorbed on sulfur-doped graphene sulfur (-S) and defect positions, so that the circulation stability can be improved, the formed Si-S has a coordination effect, the electron transfer is accelerated, and the rate capability is improved; the polymer coating layer improves the conductivity of the silicon-based material and buffers the volume expansion of the silicon-based material; meanwhile, the preparation method is simple to operate, simple and environment-friendly in process and wide in application prospect.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to a polymer-coated silicon/sulfur-doped graphene cathode material and a preparation method thereof.
Background
The lithium ion battery is a green high-energy environment-friendly battery, and has the outstanding advantages of high energy density, environmental friendliness, no memory effect, long cycle life, small self-discharge and the like, so the lithium ion battery is widely concerned in the application of mobile phone batteries, mobile power supplies, electric vehicles and the like. When the lithium ion battery is widely applied to new energy automobiles as a power battery, no material can completely meet the requirements of an automobile power system on the lithium ion battery at present because the safety performance, the energy density, the high rate performance and the cycle life of the lithium ion battery are further improved.
In order to develop a lithium ion battery suitable for a new energy automobile, researchers mainly focus on anode and cathode materials at the present stage. At present, graphite is mainly used as a negative electrode material, but the specific capacity and the lithium removal potential of the negative electrode material are low, and the low lithium removal potential (only 0.05V) causes a safety problem, so that the application of the graphite in a large-capacity battery is limited. The appearance of silicon gives great hope to new energy automobiles, has the characteristics of the highest theoretical specific capacity (4200 mAh & g < -1 >), moderate lithium removal potential (< 0.5V vs Li +/Li) and abundant reserve of 27.6 percent and the like, and is greatly valued by researchers. However, silicon has poor conductivity, and when the highest specific capacity is reached, the volume expansion of silicon is as high as more than 300%, which seriously affects the cycle performance of the lithium ion battery, finally results in poor electrochemical performance, and limits the commercial application of the lithium ion battery.
Therefore, the prior art has yet to be improved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a polymer-coated silicon/sulfur-doped graphene negative electrode material and a preparation method thereof, and aims to improve the conductivity of a silicon-based material, buffer the volume expansion of the silicon-based material and improve the cycle performance and rate capability of a lithium ion battery.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a polymer-coated silicon/sulfur-doped graphene negative electrode material is composed of 50wt% -80 wt% of silicon material, 10wt% -20 wt% of graphene and 10wt% -30% of a polymer coating layer coated outside the silicon material.
The silicon material is silicon nanoparticles, and the particle size is 20-100 nm.
The graphene is sulfur-doped graphene.
The polymer is a polypyrrole/polydopamine compound.
A preparation method of a polymer-coated silicon/sulfur-doped graphene negative electrode material comprises the following steps:
s1: preparing a silicon/sulfur-doped graphene composite material: taking silicon nanoparticles and sulfur-doped graphene, and carrying out ball milling to obtain a silicon/sulfur-doped graphene composite material;
s2: preparing a polymer-coated silicon/sulfur-doped graphene negative electrode material: dispersing the silicon/sulfur doped graphene composite material into deionized water, magnetically stirring for 60min, then adding a pyrrole monomer and a dopamine monomer, cooling to 5-10 ℃, adding ferric chloride hexahydrate, and reacting for 8-12 h;
s3: and (3) precipitating the product of S2, washing with deionized water, repeating for a plurality of times, drying, and grinding into powder.
And in the S1, the ball milling time is 1-3 h.
The dopamine monomer accounts for 2% -8% of the pyrrole monomer.
The reaction temperature in the S2 is 5-10 ℃, and the reaction time is 8-12 h.
The invention has the beneficial effects that: the core silicon nanoparticles of the cathode material have lithium storage activity, and the silicon nanoparticles are adsorbed on sulfur-doped graphene sulfur (-S) and defect positions, so that the long-term circulation stability can be improved, the formed Si-S has a coordination effect, the electron transfer is accelerated, and the rate capability is improved; the polypyrrole/polydopamine outer coating can obviously improve the conductivity of the silicon-based material and buffer the volume expansion of the silicon-based material; meanwhile, the preparation method is simple to operate, simple and environment-friendly in process and has wide prospects in commercial application.
Drawings
Fig. 1 is a flow chart of the preparation of the polymer-coated silicon/sulfur-doped graphene anode material of the present invention.
Fig. 2 is a 0.5C cycle performance diagram of a lithium ion battery assembled by the polymer-coated silicon/sulfur-doped graphene negative electrode material in embodiment 1 of the invention.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and the description in this section is only exemplary and explanatory and should not be construed as limiting the scope of the present invention in any way.
A polymer-coated silicon/sulfur-doped graphene negative electrode material is composed of 50wt% -80 wt% of silicon material, 10wt% -20 wt% of graphene and 10wt% -30% of a polymer coating layer coated outside the silicon material.
The silicon material is silicon nanoparticles, and the particle size is 20-100 nm.
The graphene is sulfur-doped graphene.
The polymer is a polypyrrole/polydopamine compound.
A preparation method of a polymer-coated silicon/sulfur-doped graphene negative electrode material comprises the following steps:
s1: preparing a silicon/sulfur-doped graphene composite material: taking silicon nanoparticles and sulfur-doped graphene, and carrying out ball milling to obtain a silicon/sulfur-doped graphene composite material;
s2: preparing a polymer-coated silicon/sulfur-doped graphene negative electrode material: dispersing the silicon/sulfur doped graphene composite material into deionized water, magnetically stirring for 60min, then adding a pyrrole monomer and a dopamine monomer, cooling to 5-10 ℃, adding ferric chloride hexahydrate, and reacting for 8-12 h;
s3: and (3) precipitating the product of S2, washing with deionized water, repeating for a plurality of times, drying, and grinding into powder.
And in the S1, the ball milling time is 1-3 h.
The dopamine monomer accounts for 2% -8% of the pyrrole monomer.
The reaction temperature in the S2 is 5-10 ℃, and the reaction time is 8-12 h.
In the above technical scheme, the preparation method of the polymer-coated silicon/sulfur-doped graphene anode material comprises the following steps:
preferably, the ball milling time of the silicon nanoparticles and the sulfur-doped graphene is 2 hours.
Preferably, the dopamine monomer accounts for 3% -6% of the pyrrole monomer.
Preferably, the reaction temperature is 8 ℃.
Preferably, the reaction time is 8-10 h.
A polymer-coated silicon/sulfur-doped graphene negative electrode material is prepared by the preparation method of the polymer-coated silicon/sulfur-doped graphene negative electrode material.
Example 1:
s1: preparing a silicon/sulfur-doped graphene composite material: taking 50wt% of silicon nanoparticles and 30wt% of sulfur-doped graphene, and carrying out ball milling for 3h to obtain a silicon/sulfur-doped graphene composite material;
s2: preparing a polymer-coated silicon/sulfur-doped graphene negative electrode material: dispersing the silicon/sulfur doped graphene composite material into deionized water, magnetically stirring for 60min, then adding 20wt% of pyrrole monomer and dopamine monomer, cooling to 8 ℃, adding ferric chloride hexahydrate, and reacting for 12 h;
s3: precipitating the product of S2, washing with deionized water, repeating for 5 times, drying, and grinding into powder.
Example 2:
s1: preparing a silicon/sulfur-doped graphene composite material: taking 60wt% of silicon nanoparticles and 25wt% of sulfur-doped graphene, and carrying out ball milling for 2 hours to obtain a silicon/sulfur-doped graphene composite material;
s2: preparing a polymer-coated silicon/sulfur-doped graphene negative electrode material: dispersing the silicon/sulfur doped graphene composite material into deionized water, magnetically stirring for 60min, then adding 15wt% of pyrrole monomer and dopamine monomer, cooling to 8 ℃, adding ferric chloride hexahydrate, and reacting for 10 h;
s3: precipitating the product of S2, washing with deionized water, repeating for 5 times, drying, and grinding into powder.
Example 3:
s1: preparing a silicon/sulfur-doped graphene composite material: taking 65wt% of silicon nanoparticles and 15wt% of sulfur-doped graphene, and carrying out ball milling for 2 hours to obtain a silicon/sulfur-doped graphene composite material;
s2: preparing a polymer-coated silicon/sulfur-doped graphene negative electrode material: dispersing the silicon/sulfur doped graphene composite material into deionized water, magnetically stirring for 60min, then adding 20wt% of pyrrole monomer and dopamine monomer, cooling to 8 ℃, adding ferric chloride hexahydrate, and reacting for 10 h;
s3: precipitating the product of S2, washing with deionized water, repeating for 5 times, drying, and grinding into powder.
Fig. 1 specifically illustrates the entire preparation process of the anode material; fig. 2 shows that after 1500 cycles of the lithium ion battery assembled by the negative electrode material in example 1 of the present invention, 90% of the capacity of the lithium ion battery can be maintained without fading, which indicates that the negative electrode material has excellent cycling stability.
The invention provides a polymer-coated silicon/sulfur-doped graphene negative electrode material and a preparation method thereof, which improve the conductivity of a silicon-based material, buffer the volume expansion of the silicon-based material, and improve the cycle performance and rate capability of a lithium ion battery.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (9)
1. The polymer-coated silicon/sulfur-doped graphene negative electrode material is characterized by consisting of 50-80 wt% of silicon material, 10-20 wt% of graphene and 10-30 wt% of polymer coating layer coated outside the silicon material.
2. The polymer-coated silicon/sulfur-doped graphene anode material as claimed in claim 1, wherein the silicon material is silicon nanoparticles with a particle size of 20-100 nm.
3. The polymer-coated silicon/sulfur-doped graphene anode material as claimed in claim 1, wherein the graphene is sulfur-doped graphene.
4. The polymer-coated silicon/sulfur-doped graphene anode material according to claim 1, wherein the polymer is a polypyrrole/polydopamine composite.
5. The preparation method of the polymer-coated silicon/sulfur-doped graphene anode material according to any one of claims 1 to 4, characterized by comprising the following steps:
s1: preparing a silicon/sulfur-doped graphene composite material: taking silicon nanoparticles and sulfur-doped graphene, and carrying out ball milling to obtain a silicon/sulfur-doped graphene composite material;
s2: preparing a polymer-coated silicon/sulfur-doped graphene negative electrode material: dispersing the silicon/sulfur doped graphene composite material into deionized water, magnetically stirring for 60min, then adding a pyrrole monomer and a dopamine monomer, cooling to 5-10 ℃, adding ferric chloride hexahydrate, and reacting for 8-12 h;
s3: and (3) precipitating the product of S2, washing with deionized water, repeating for a plurality of times, drying, and grinding into powder.
6. The preparation method of the polymer-coated silicon/sulfur-doped graphene anode material according to claim 5, wherein the ball milling time in S1 is 1-3 h.
7. The preparation method of the polymer-coated silicon/sulfur-doped graphene anode material according to claim 5, wherein the dopamine monomer accounts for 2-8% of the pyrrole monomer.
8. The preparation method of the polymer-coated silicon/sulfur-doped graphene anode material according to claim 5, wherein the reaction temperature in S2 is 5-10 ℃, and the reaction time is 8-12 h.
9. The polymer-coated silicon/sulfur-doped graphene anode material and the preparation method thereof according to any one of claims 1 to 8, wherein the polymer-coated silicon/sulfur-doped graphene anode material comprises the polymer-coated silicon/sulfur-doped graphene anode material prepared by the preparation method of any one of claims 5 to 8.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024001153A1 (en) * | 2022-06-28 | 2024-01-04 | 贝特瑞新材料集团股份有限公司 | Negative electrode material and preparation method therefor, and lithium ion battery |
| WO2024044982A1 (en) * | 2022-08-30 | 2024-03-07 | 宁德新能源科技有限公司 | Electrochemical apparatus and electronic device |
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| WO2024001153A1 (en) * | 2022-06-28 | 2024-01-04 | 贝特瑞新材料集团股份有限公司 | Negative electrode material and preparation method therefor, and lithium ion battery |
| WO2024044982A1 (en) * | 2022-08-30 | 2024-03-07 | 宁德新能源科技有限公司 | Electrochemical apparatus and electronic device |
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