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Method for preparing high-purity nano-silicon

A nano-silicon and nano-silicon dioxide technology, which is applied in the field of preparing high-purity nano-silicon, can solve problems such as many crystal defects, uneven particle distribution, and low product purity, and achieve small nano-silicon size, oversized particle size, and process simple effect

Active Publication Date: 2020-01-17
HUNAN SHINZOOM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the mechanical ball milling method is relatively simple and low in cost, but has disadvantages such as low product purity, many crystal defects, long time consumption, and uneven particle distribution.
The raw material price of the plasma evaporation and condensation method is low and no post-treatment is required, but the quality of the product is greatly affected by the quality of the raw material, and it is difficult to guarantee the yield and product purity
The reaction mechanism of the chemical vapor deposition method is not clear enough, the safety of the reaction needs to be solved, and the shape of the obtained products is mostly amorphous

Method used

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  • Method for preparing high-purity nano-silicon
  • Method for preparing high-purity nano-silicon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix ethyl orthosilicate with ethanol and deionized water in a beaker, the mixing mass ratio is 1:2:3, put it into a water bath for water bath stirring, the water bath temperature is 40°C, and the stirring time is 4h. After dispersing evenly, add ammonia water into the beaker, the mass ratio of ammonia water to tetraethyl orthosilicate is 1:1, continue to stir for 5 hours, finally wash with ethanol ultrasonically, and dry in an oven. The obtained product was mixed evenly with magnesium hydride, and reduced in a box furnace under a nitrogen atmosphere, kept at 300°C for 2 hours, continued to heat up to 800°C, kept at 3h, and the heating rate was 2°C / min. After the reaction is cooled, the residual nano-silica and magnesium oxide are washed away with hydrofluoric acid, then cleaned and filtered with ultra-pure water until neutral, and finally vacuum-dried to obtain nano-silicon. The XRD figure, TEM figure of gained nano-silicon are respectively as follows figure 1 , figu...

Embodiment 2

[0026] Take a certain amount of tetraethyl orthosilicate and mix it with propanol and deionized water in a beaker, the mixing mass ratio is 1:2:2, put it into a water bath for water bath stirring, the water bath temperature is 50°C, and the stirring time is 1h. After dispersing evenly, add ammonia water into the beaker, the mass ratio of ammonia water to tetraethyl orthosilicate is 0.8:1, continue to stir for 3 hours, finally wash with ethanol ultrasonically, and dry in an oven. The obtained product and aluminum hydride were subjected to hydrogen carbonization reduction in a drum furnace, kept at 500°C for 2 hours, and continued to heat up to 1000°C for 4 hours at a heating rate of 10°C / min. After the reaction is cooled, the remaining nano silicon dioxide and aluminum oxide are washed away with hydrofluoric acid, then cleaned and filtered with ultrapure water until neutral, and finally vacuum dried to obtain nano silicon.

Embodiment 3

[0028] Mix tetraethyl orthosilicate, propanol and deionized water at a mass ratio of 1:2:4, put them into a water bath for water bath stirring, the temperature of the water bath is 70°C, and the stirring time is 1h. After dispersing evenly, add ammonia water into the beaker, the mass ratio of ammonia water to tetraethyl orthosilicate is 0.5:1, continue to stir for 2 hours, finally wash with ethanol ultrasonically, and dry in an oven. The obtained product and alkaline earth metal hydrides other than Be were subjected to hydrogen carbonization reduction in a drum furnace, kept at 400°C for 2 hours, continued to heat up to 1300°C, kept at 6 hours, and the heating rate was 6°C / min. After the reaction is cooled, the remaining nano silicon dioxide and metal oxides are washed away with hydrofluoric acid, then cleaned and filtered with ultrapure water until neutral, and finally vacuum dried to obtain nano silicon.

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Abstract

The invention relates to a method for preparing high-purity nano-silicon. The method comprises the following steps: preparing nano-silica by an organosilicon through a sol-gel method, reducing the nano-silica to nano-silicon monoxide by a metal hydride, carrying out a disproportionation reaction of the silicon monoxide at a high temperature to produce nano-silicon and nano-silica, and removing theexcess nano-silica by hydrofluoric acid treatment. The method is simple in process and low in cost, the purity of the obtained nano-silicon is high, and a size of the nano-silicon is small.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion battery electrode material, in particular to a method for preparing high-purity nano-silicon. Background technique [0002] Nano-silica powder is a semiconductor material widely used in the fields of microelectronics, electrode materials and solar cells. It has the advantages of large surface area, high surface activity and low bulk density. At present, the common methods used to prepare nano-silicon powder include mechanical ball milling, plasma evaporation and condensation, and chemical vapor deposition. Among them, the mechanical ball milling method is relatively simple and low in cost, but has disadvantages such as low product purity, many crystal defects, long time consumption, and uneven particle distribution. The raw material price of the plasma evaporation and condensation method is low, and no post-treatment is required, but the quality of the product is greatly affected by the qu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/023H01M4/38H01M10/0525B82Y40/00
CPCB82Y40/00C01B33/023C01P2002/72C01P2004/04C01P2004/64H01M4/386H01M10/0525Y02E60/10
Inventor 李能皮涛王志勇黄越华邵浩明陈松彭杨城李钰余梦泽
Owner HUNAN SHINZOOM TECH
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