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

A silicon-carbon composite material and sub-nanometer technology, applied in nano-carbon, silicon compounds, nanotechnology and other directions, can solve the problem that it is difficult to easily obtain a sub-nano-sized silicon-carbon composite material, 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 to enlarge the method, and stable structure

Active Publication Date: 2022-03-29
YANCHENG INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • 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

Examples

Experimental program
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Effect test

Embodiment 1

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

[0026] Step (2): Mix and react the yellow solution in step (1) with 0.1 mol of amylmagnesium bromide, stir at room temperature for 2 hours, and purify to obtain a mixed solution of organic group-modified silicon clusters;

[0027] Step (3): The mixed solution in step (2) was pumped dry under reduced pressure to obtain a yellow solid, which was placed in a tube furnace and heat-treated at 500°C for 2 hours under the protection of flowing high-purity argon. After cooling, The subnano-silicon-carbon composite material was prepared.

Embodiment 2

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

[0030] Step (2): Mix and react the yellow solution in step (1) with 0.1 mol of amylmagnesium bromide, stir at room temperature for 2 hours, and purify to obtain a mixed solution of organic group-modified silicon clusters;

[0031] Step (3): The mixed solution in step (2) was pumped dry under reduced pressure to obtain a yellow solid, which was placed in a tube furnace and heat-treated at 500°C for 2 hours under the protection of flowing high-purity argon. After cooling, The subnano-silicon-carbon composite material was prepared.

Embodiment 3

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

[0034] Step (2): Mix and react the yellow solution in step (1) with 0.1 mol of amylmagnesium bromide, stir at room temperature for 2 hours, and purify to obtain a mixed solution of organic group-modified silicon clusters;

[0035] Step (3): The mixed solution in step (2) was pumped dry under reduced pressure to obtain a yellow solid, which was placed in a tube furnace and heat-treated at 500°C for 2 hours under the protection of flowing high-purity argon. After cooling, The subnano-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, which comprises the following steps: step (1), dissolving micromolecular silane and ethylenediamine in a conventional organic solvent according to a mass ratio of 0.5: 1 to 10: 1, and stirring at room temperature for 5-10 hours to obtain a yellow solution; (2) mixing the yellow solution in the step (1) with a Grignard reagent, stirring at room temperature for 2 hours, and purifying to obtain an organic group modified silicon cluster mixed solution; and (3) carrying out vacuum pumping on the mixed solution in the step (2) to obtain a yellow solid, putting the yellow solid into a tubular furnace, carrying out heat treatment on the yellow solid in a temperature range of 500-1000 DEG C under the protection of flowing high-purity argon, and cooling to obtain the sub-nano silicon-carbon composite material. The method disclosed by the invention has the advantages of mild reaction conditions and easiness in amplification and regulation, is expected to be used for industrially preparing the sub-nano silicon-carbon composite, and is applied to the field of energy sources, especially 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 subnano silicon-carbon composite material by a liquid phase method. Background technique [0002] Silicon-carbon composite materials have received great attention in the field of high-energy-density lithium-ion batteries due to their high energy density, relatively suitable working potential, and abundant reserves of silicon in the earth's crust. Silicon-carbon composite materials are generally considered to be the most promising alternatives to the current mainstream graphite anode, becoming 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 charging and discharging, which leads to shortened battery cycle life. Therefore, it is particularly important to use small-sized silicon materials (especial...

Claims

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Application Information

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Patent Type & Authority Applications(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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