Method for preparing sub-nano silicon carbon composite material by liquid phase method

A silicon-carbon composite material and sub-nanometer technology, which is applied in the direction of nano-carbon, silicon compound, nanotechnology, etc., can solve the difficulty of obtaining sub-nanometer-sized silicon-carbon composite materials conveniently, and the growth and deposition of silane gas into silicon particles cannot be precisely controlled , It is difficult to realize the preparation of sub-nano-sized silicon materials, etc., to achieve the effect of improving high energy density, easy scale-up of the method, and stable structure

Active Publication Date: 2022-07-22
YANCHENG INST OF TECH +1
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The current mainstream process for the preparation of small-sized silicon materials is to use CVD or PVD methods to grow and deposit in high-temperature furnaces. This method can ensure continuous production, but the disadvantages are that it consumes a lot of energy and is harmful to the growth and deposition of silane gas. Silicon-forming particles cannot be precisely regulated, especially difficult to achieve the preparation of sub-nano-sized silicon materials
The newspaper Nature Energy, 2021, doi: 10.1038 / s41560-021-00945-z and the patent number CN201710527122.X announced a method for rapidly preparing sub-nanometer spherical silicon powder by arc, but these methods are still cumbersome and difficult to obtain sub-nanometer Dimensions of Silicon Carbon Composites

Method used

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  • Method for preparing sub-nano silicon carbon composite material by liquid phase method
  • Method for preparing sub-nano silicon carbon composite material by liquid phase method

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Effect test

Embodiment 1

[0025] Step (1): HSiCl 3 And ethylenediamine is dissolved in acetonitrile in the range of mass ratio of 5:1, and stirred at room temperature for 10 hours to obtain a yellow solution;

[0026] Step (2): mixing and reacting the yellow solution in step (1) with 0.1 mol of amylmagnesium bromide, stirring at room temperature for 2 hours, and purifying to obtain a mixed solution of silicon clusters modified by organic groups;

[0027] Step (3): the mixed solution in step (2) was vacuumed and drained to obtain a yellow solid, which was placed in a tube furnace, and the yellow solid was heat-treated at a temperature of 500° C. for 2h under the protection of flowing high-purity argon gas. After cooling The sub-nanometer silicon-carbon composite material was prepared.

Embodiment 2

[0029] Step (1): HSiCl 3 Dissolve in tetrahydrofuran with ethylenediamine in a mass ratio of 5:1, and stir at room temperature for 10 hours to obtain a yellow solution;

[0030] Step (2): mixing and reacting the yellow solution in step (1) with 0.1 mol of amylmagnesium bromide, stirring at room temperature for 2 hours, and purifying to obtain a mixed solution of silicon clusters modified by organic groups;

[0031] Step (3): the mixed solution in step (2) was vacuumed and drained to obtain a yellow solid, which was placed in a tube furnace, and the yellow solid was heat-treated at a temperature of 500° C. for 2h under the protection of flowing high-purity argon gas. After cooling The sub-nanometer silicon-carbon composite material was prepared.

Embodiment 3

[0033] Step (1): Put Si 2 Cl 6 And ethylenediamine is dissolved in acetonitrile in the range of mass ratio of 5:1, and stirred at room temperature for 10 hours to obtain a yellow solution;

[0034] Step (2): mixing and reacting the yellow solution in step (1) with 0.1 mol of amylmagnesium bromide, stirring at room temperature for 2 hours, and purifying to obtain a mixed solution of silicon clusters modified by organic groups;

[0035] Step (3): the mixed solution in step (2) was vacuumed and drained to obtain a yellow solid, which was placed in a tube furnace, and the yellow solid was heat-treated at a temperature of 500° C. for 2h under the protection of flowing high-purity argon gas. After cooling The sub-nanometer silicon-carbon composite material was prepared.

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Abstract

The invention discloses a method for preparing a sub-nano silicon carbon composite material by a liquid phase method, comprising the following steps: step (1), dissolving small molecular silane and ethylenediamine in a conventional In an organic solvent, stir at room temperature for 5-10 hours to obtain a yellow solution; step (2), mix the yellow solution in step (1) with Grignard reagent, stir at room temperature for 2 hours, and purify to obtain a silicon group modified by an organic group Cluster mixed solution; in step (3), the mixed solution in step (2) is decompressed and drained to obtain a yellow solid, and placed in a tube furnace, under the protection of flowing high-purity argon, in a temperature range of 500-1000 ° C The yellow solid is heat-treated, and the sub-nanometer silicon-carbon composite material is prepared after cooling. The method of the invention has the advantages of mild reaction conditions, easy amplification and regulation, is expected to be used for industrialized preparation of sub-nanometer silicon-carbon composites, and can be applied in the energy field, especially in the field of lithium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of functional materials, in particular to a method for preparing a sub-nano silicon carbon composite material by a liquid phase method. Background technique [0002] Silicon-carbon composites have attracted great attention in the field of high-energy-density lithium-ion batteries due to their high energy density, relatively suitable working potential, and abundant silicon reserves in the earth's crust. Silicon carbon composites are generally considered to be the most promising alternative to the current mainstream graphite anodes and become a new generation of anode materials with high energy density. In the field of lithium-ion batteries, the biggest obstacle to the application of silicon carbon anodes is the huge volume change during the charging and discharging process, which leads to the shortening of battery cycle life. Therefore, it is particularly important to use small-sized silicon materials (especi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/021C01B32/15B82Y40/00H01M4/36H01M4/38H01M4/62
CPCC01B33/021C01B32/15B82Y40/00H01M4/364H01M4/386H01M4/625Y02E60/10
Inventor 孙林刘宴秀张磊吴俊姜瑞雨
Owner YANCHENG INST OF TECH
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