Method for preparing silica powder through mechanical chemical method

A technology for silicon powder and powder, which is applied in the field of silicon powder preparation, can solve the problems of low primary utilization rate of raw materials, high requirements for preparation conditions and high cost, and achieves the effects of easy industrialization, simple preparation process and good quality.

Active Publication Date: 2016-01-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These preparation methods are costly, require high preparation conditions, consume a lot of energy in the production proc

Method used

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  • Method for preparing silica powder through mechanical chemical method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under the protection of an argon atmosphere, 0.7 g of lithium hydride and 1.3 g of silicon tetrachloride were uniformly mixed and added into a ball mill jar. Then put the balls into the ball mill jar and seal it. The mass ratio of grinding balls to materials is 20:1. Under the condition of room temperature, the ball mill tank was continuously ball milled at a speed of 500 rpm for 20 hours, and after taking it out, it was washed 3 times with 5% dilute hydrochloric acid, and washed with deionized water until the solution was neutral. The powder obtained by drying and cooling is silicon powder (purity greater than 95%).

Embodiment 2

[0030] Under the protection of a nitrogen atmosphere, 1.12g of magnesium hydride and 0.88g of silicon tetrachloride were uniformly mixed and then added to a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of ball mass to material mass is 60:1. Under the condition of room temperature, the ball mill jar was continuously ball milled at a speed of 450 rpm for 24 hours. After taking it out, it was washed 3 times with 8% dilute hydrochloric acid, and washed with deionized water until the solution was neutral. The powder obtained by drying and cooling is silicon powder (purity greater than 95%).

Embodiment 3

[0032] Under the protection of an argon atmosphere, 1.23g of calcium hydride and 3.47g of silicon tetrabromide were evenly mixed and then added to the ball mill jar. Then put the balls into the ball mill jar and seal it. The mass ratio of grinding balls to materials is 40:1. Under room temperature conditions, the ball mill tank was continuously ball milled at a speed of 550r / min for 15h, and after taking it out, it was washed 3 times with dilute hydrochloric acid with a concentration of 100%, and washed with deionized water until the solution was neutral. The powder obtained by drying and cooling is silicon powder (purity greater than 93%).

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Abstract

The invention discloses a method for preparing silica powder through a mechanical chemical method. The method includes the following steps that 1, silicon halide, metal hydride and grinding balls are added into a ball-milling tank in protecting atmosphere, and then the ball-milling tank is sealed, wherein the molar ratio of the silicon halide to the metal hydride is 1:2-1:6; 2, a ball-milling reaction is carried out on the silicon halide and the metal hydride under the conditions of the room temperature and the 100-rpm-to-500-rpm ball-milling rotating speed in the sealed ball-milling tank, and the ball-milling time is 1 h to 24 h; 3, after the ball-milling reaction is completed, hydrogen in the ball-milling tank is collected, and then powder in the ball-milling tank is taken out; 4, the powder is subjected to acid pickling and then washed till washing liquid is neutral; 5, the washed powder is dried and cooled, and the simple-substance silica powder is obtained. The method for preparing the silica powder has the advantages of being simple in technology, efficient and nontoxic, and facilitating industrialization implementing.

Description

(1) Technical field [0001] The invention relates to a method for preparing silicon powder by mechanochemical method (2) Background technology [0002] Silicon material has become a research hotspot in many fields due to its unique physical and chemical properties. It is a non-toxic, odorless and non-polluting inorganic non-metallic material. Silicon is the most abundant element except oxygen in the earth's crust, but it rarely occurs in nature in the form of simple substance. At present, the silicon preparation methods that have been industrialized mainly include: improved trichlorosilane hydrogen reduction method, that is, high-purity trichlorosilane is reduced with high-purity hydrogen on a high-purity silicon core at about 1100 ° C, and polycrystalline silicon is deposited on the silicon core. Silane method, namely SiH 4 The gas is introduced into the silane decomposition furnace, and high-purity polysilicon is decomposed and deposited on the heating silicon core at 800...

Claims

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Application Information

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IPC IPC(8): C01B33/027
Inventor 许浩辉梁初夏阳陶新永张文魁甘永平黄辉张俊
Owner ZHEJIANG UNIV OF TECH
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